JP2020511562A - Method for separating and purifying polymers from recycled products - Google Patents

Abstract

A method for separating and purifying a polymer of recycled product (rP) is disclosed. The rP is contacted with the extraction solvent at elevated temperature and pressure to produce the extracted rP (erP). The first polymer is purified at elevated temperature and pressure by contacting the solvent with erP to form a solution and contacting it with a solid medium under conditions sufficient to solubilize the first polymer. To produce a purified solution of. The purified polymer is then separated from the purification solution and the process steps are repeated until all the polymer has been separated and purified.

Description

  The present invention relates generally to methods of separating and purifying polymers from reclaimed products (rP) using heated and pressurized solvents and solid media. More specifically, the separated and purified polymer is a colorless or transparent, odorless, and virgin-like polymer. Reclaimed film (rF) and reclaimed absorbent hygiene product (rAHP) are examples of rP containing at least two polymers and are products after consumer and / or industrial use. May be The method includes adhesives (adhesives, ADH) from rAHP, thermoplastic elastomers (TPE), polypropylene (polypropylene, PP), polyethylene (polyethylene, PE), polyester, cellulose, and poly (acrylic acid) ( It is especially useful for the separation and purification of poly (acrylic acid), PAA).

Polymers, especially synthetic plastics, are ubiquitous in everyday life due to their relatively low production cost and good material property balance. Synthetic plastics are used in a wide range of applications such as packaging, automobile parts, medical devices, and consumer goods. To meet the high demand for these applications, tens of billions of pounds of synthetic plastics are manufactured each year around the world. The vast majority of synthetic plastics are produced from the increasingly scarce fossil resources (eg oil and natural gas). In addition, the production of synthetic plastics from fossil resources produces CO ₂ , a strong greenhouse gas, as a by-product.

  The ubiquitous use of synthetic plastics produces millions of tons of plastic waste each year. Most plastic waste is landfilled by municipal solid waste programs, but a significant portion of plastic waste is found in the environment as trash, which can be unaesthetic and potentially harmful to the environment. is there. Plastic waste often flows into river systems and eventually into the sea.

  To reduce the problems associated with the widespread use of plastics, plastic recycling has emerged as one solution. By recovering and reusing plastics, waste is prevented from entering landfills, demand for virgin plastics produced from fossil resources is reduced, and as a result, greenhouse gas emissions are reduced. . In developed countries such as the United States and the European Union, increasing awareness of consumers, businesses, and manufacturing has led to an increase in plastic recycling rates. Most of the recycled materials, including plastics, are mixed into a single stream that is collected and processed at a material recovery facility (MRF). In MRF, materials are sorted, washed and packaged for resale. Plastics can be individual materials such as high-density polyethylene (HDPE) or poly (ethylene terephthalate) (PET), or other common plastics such as PP, low density. For mixed flow of polyethylene (low-density polyethylene, LDPE), polyvinyl chloride (poly (vinyl chloride), PVC), polystyrene (polystyrene, PS), polycarbonate (polycarbonate, PC), and polyamide (polyamides, PA) Can be classified. The single stream or mixed stream can then be further classified, washed and reworked into pellets, which are suitable for reuse in plastics processing such as blow molding and injection molding.

  Recycled plastics are mainly sorted into a uniform stream and washed with aqueous and / or caustic solutions, but the final reprocessed pellets contain unwanted waste impurities such as spoiled food residues and residual flavor components. Often remains highly contaminated. In addition, recycled plastic pellets are darkly colored due to the mixture of dyes and pigments commonly used to color plastic articles, except those obtained from recycled beverage containers. . While some applications are less amenable to color and contamination (eg black plastic containers for paint, hidden automotive parts) most applications require colorless pellets. The need for high quality "virgin-like" recycled resins is particularly important in food and pharmaceutical contact applications such as food packaging. In addition to contamination by impurities and mixed colorants, many recycled resin products often have heterogeneous chemical compositions and may contain significant amounts of polymeric impurities, such as PE impurities in recycled PP and reverse impurities. Is also the same.

  Mechanical recycling (also called secondary recycling) is the process of converting recycled plastic waste into a form that can be reused for subsequent manufacturing processes. For a more detailed review of mechanical recycling and other plastic recovery processes, see S.W. M. Al-Salem, P .; Lettieri, and J.M. Baeyens, "Recycling and recovery routes of plastic solid waste (PSW): A review", Waste Management, Volume 29, Issue 10, October 2009, p. 2625-2643, ISSN 0956-053X. Although advances in mechanical recycling technology have improved the quality of recycled polymers to some extent, mechanical decontamination approaches have fundamental limitations, such as the physical entrapment of the pigment within the polymer matrix. Therefore, even with the improvement of mechanical recycling technology, the deep coloring and high level of chemical pollution in the currently available recycled plastic wastes prevent the widespread use of recycled resins by the plastics industry.

  In order to overcome the fundamental limitations of mechanical recycling, a number of chemical approaches (chemical recycling) have been developed to purify contaminated polymers. Many of these methods use a solvent to decontaminate and purify the polymer. The use of a solvent allows the extraction of impurities and the dissolution of the polymer, which in turn allows another separation technique.

  For example, US Pat. No. 7,935,736 describes a method of recycling polyester from polyester-containing waste using a solvent to dissolve the polyester prior to cleaning. The '736 patent further describes the need to recover polyester from solvent using precipitation.

  In another example, US Pat. No. 6,555,588 describes a method of making polypropylene blends from plastic mixtures containing other polymers. The '588 patent describes extracting impurities from a polymer in a selected solvent (e.g., hexane) at a temperature below the dissolution temperature of the polymer for a given residence time. The '588 patent further describes increasing the temperature of the solvent (or second solvent) to dissolve the polymer prior to filtration. The '588 patent further describes the use of shear or flow to precipitate PP from solution. The PP blend described in the '588 patent contained up to 5.6 wt% PE.

  In another example, European Patent Application No. 849,312 (translated from German to English) describes a process for obtaining purified polyolefin from a polyolefin-containing plastic mixture or polyolefin-containing waste. The '312 patent application relates to extracting a polyolefin mixture or waste with a hydrocarbon fraction of gasoline or diesel fuel having a boiling point above 90 ° C. at temperatures between 90 ° C. and the boiling point of the hydrocarbon solvent. It describes. The '312 patent application further describes removing foreign components from the solution by contacting the hot polyolefin solution with bleached clay and / or activated carbon. The '312 patent further claims that the solution is cooled to a temperature below 70 ° C. to crystallize the polyolefin and then the polyolefin is heated to a temperature above the melting point of the polyolefin or the deposition solvent is evaporated in a vacuum. Or removing the adhering solvent by passing a stream of gas through the polyolefin precipitate and / or extracting the solvent with an alcohol or ketone boiling below the melting point of the polyolefin.

  In another example, US Pat. No. 5,198,471 uses a solvent at a first low temperature to separate a polymer from a physically mixed solid mixture containing multiple polymers (eg, waste plastic). And describes the method of forming the first single-phase solution and the remaining solid components. The'471 patent further describes heating the solvent to a higher temperature to dissolve additional polymer that was not solubilized at the first, lower temperature. The '471 patent describes filtering insoluble polymeric components.

  In another example, US Pat. No. 5,233,021 discloses dissolving each component in a supercritical fluid at an appropriate temperature and pressure and then varying the temperature and / or pressure to sequentially cool the particular component. A method for extracting pure polymer components from a multi-component structure (eg, carpet waste) by extraction is described. However, like the '471 patent, the' 021 patent only describes filtration of insoluble components.

  In another example, US Pat. No. 5,739,270 discloses a method and apparatus for the continuous separation of a polymeric component of a plastic from contaminants and other plastic components using cosolvents and working fluids. Is described. The co-solvent at least partially dissolves the polymer and the second fluid (which is liquid and in the critical or supercritical state) solubilizes the components of the polymer and partially dissolves the dissolved polymer. Precipitate from. The '270 patent further describes a process for removing particulate contaminants such as glass particles by filtering a thermoplastic cosolvent (with or without working fluid).

  The known solvent-based methods for purifying contaminated polymers described above do not produce "virgin-like" polymers. In the process, co-dissolution, and thus cross-contamination of other polymers, often occurs. When using an adsorbent, filtration and / or centrifugation steps are often used to remove the spent adsorbent from the solution. In addition, separation processes for solvent removal such as heating, vacuum evaporation, and / or precipitation with precipitating chemistries are used to produce residual solvent free polymers.

  In addition, absorbent hygiene products (AHP), such as baby diapers, feminine protection pads, and adult incontinence pads, and products and packaging films (F) are typically disposed of in landfills. Are not recycled. However, these products contain various polymers such as in the case of AHP, ADH, TPE, PP, PE, PET, cellulose, and PAA that can be recycled as individual streams.

US Patent No. 7,935,736 US Pat. No. 6,555,588 European Patent Application No. 849,312 US Pat. No. 5,198,471 US Pat. No. 5,233,021 US Pat. No. 5,739,270

S. M. Al-Salem, P .; Lettieri, and J.M. Baeyens, "Recycling and recovery routes of plastic solid waste (PSW): A review", Waste Management, Volume 29, Issue 10, October 2009, p. 2625-2643, ISSN 0956-053X

  Thus, it uses a solvent that is easily and economically removed from the polymer, is relatively simple in terms of number of unit operations, produces the polymer without significant polymer cross-contamination, and is essentially colorless. There remains a need for a method of using improved solvents for purifying impure polymers that produces polymers of the present invention and polymers that are essentially odorless. There is also a need to separate and purify the various polymers that make up rAHP and rF so that these separated and purified polymers can be reused in the production of AHP and F or in other applications.

  In one embodiment of the present invention, a method of separating and purifying a polymer from a recycled product (rP), wherein the rP comprises the polymer and impurities, the polymer comprising a base polymer and particulates associated with the polymer. An additive and an extractable material associated with the polymer, wherein the particulate additive associated with each polymer is dispersed in the base polymer at a concentration and the polymer is a soluble polymer, Selected from the group consisting of insoluble polymers, and mixtures thereof, wherein the impurities include particulate matter associated with the impurities and extractable material associated with the impurities, and the extractable material in the rP Material comprises the extractable material associated with the polymer and the extractable material associated with the impurities, and the extractable material in the rP , Present in a concentration that is in the rP, method is provided. The method comprises: (a) obtaining rP, wherein rP is selected from the group consisting of the product after consumer use, the product after industrial use, and combinations thereof; ) Extracting the rP with an extraction solvent at a temperature above about 100 ° C. and a pressure above about 150 psig (1 MPa), wherein the extraction solvent has a normal boiling point of less than about 70 ° C. producing rP (erP), the extractable material having a concentration in the erP that is lower than the concentration of the extractable material in the rP, and (c) a first solubility. By contacting the erP with the dissolution process solvent in a temperature range and pressure range sufficient to solubilize the base polymer in the dissolution process solvent, the first soluble base polymer of the rP. A step of dissolving the particles to form an initial suspension, wherein the initial suspension is in the form of particles associated with the first soluble polymer in the first soluble base polymer solution. Comprising a suspension of additives and domains of all of the remaining polymer, wherein the first soluble base polymer has a solubilization range that is less than the solubilization range of the remaining soluble base polymer; ) A settling collection of particulate additive and domains of all of the remaining polymer, and a step of settling the initial suspension in a temperature range and pressure range sufficient to produce an intermediate suspension, The settled collection of particulate additives comprises particulate additives associated with the first soluble polymer and the intermediate suspension comprises the first soluble base polymer solution in the first soluble base polymer solution. Related to soluble polymers And (e) using a solid medium in a temperature range and pressure range sufficient to produce a final suspension, A step of purifying, wherein the portion of the particulate additive associated with the first soluble polymer is retained by the solid medium and the final suspension is in the first soluble base polymer solution. A step comprising a suspension of unretained particulate additive associated with the first soluble polymer, and (f) a temperature sufficient to produce a separated and purified first soluble polymer. A step of separating the dissolution step solvent from the final suspension in a range and pressure range, wherein the separated and purified first soluble polymer is in the rP and the first soluble base polymer. The first in the first soluble polymer of Of the particulate polymer associated with the first soluble polymer dispersed in the separated and purified first soluble polymer at a concentration lower than the concentration of the particulate additive associated with the soluble polymer of And a step including (g) step b (extraction step), c (dissolution step), d (precipitation step), e (purification step), and f (separation step). Repeated with each collection of settled particulate additive obtained from the previous iteration of and all the domains of the remaining polymer, through the additional soluble polymer at one time and from the second soluble polymer. Producing a separated and purified soluble polymer through extracting, dissolving, precipitating, purifying, and separating the soluble base polymer in a proceeding sequence, the sequence comprising: Profit Minimum solubilization until each individual soluble polymer produced was produced in its separated and purified form and a final collection of precipitated particulate additive and the relevant domain of all insoluble base polymer was produced. Proceeding from a soluble base polymer having a range to a maximum solubilization range.

  In another embodiment of the invention, a method of separating and purifying ADH, TPE, PP, PE, PET, cellulose, and PAA polymers from regenerated absorbent hygiene products (rAHP), wherein the rAHP is The particulate additive containing impurities, each polymer comprising a base polymer, a particulate additive associated with each polymer, and an extractable material associated with each polymer, and associated with each polymer. Dispersed in each of the base polymers at a concentration, each of the polymers being selected from the group consisting of soluble polymers, insoluble polymers, and mixtures thereof, the impurities being associated with the impurities. Comprising particulate matter and extractable material associated with the impurities, the extractable material in the rAHP being associated with the polymer And a extractable material associated with possible materials and the impurities out, the extractable material in the RAHP is present in a concentration that is in the RAHP, method is provided. The method comprises: (a) obtaining rAHP, wherein the rAHP is selected from the group consisting of products after consumer use, products after industrial use, and combinations thereof; and (b) Extracting the rAHP with an extraction solvent at a temperature above about 100 ° C. and a pressure above about 150 psig (1 MPa), wherein the extraction solvent has a normal boiling point below about 70 ° C. Producing (erAHP), the extractable material having a concentration in the erAHP that is lower than the concentration of the extractable material in the rAHP, and (c) the ADH base polymer is a dissolution step solvent. Of the rAHP by contacting the erAHP with the dissolution step solvent in a temperature range and pressure range sufficient to solubilize the rAHP. Dissolving the ADH-based polymer to form an initial suspension, the initial suspension comprising the particulate additive associated with the ADH polymer in an ADH-based polymer solution, as well as TPE, PP. , PE, PET, cellulose, and suspensions with domains of PAA polymer, wherein the ADH-based polymer has a solubilization range less than that of the TPE, PP, PE, and PET-based polymers. And (d) a collection of settled particulate additives and such domains of TPE, PP, PE, PET, cellulose, and PAA polymers, and a temperature range and pressure range sufficient to produce an intermediate suspension. At a step of settling the initial suspension, wherein the settled collection of particulate additives is particles associated with the ADH polymer. An additive, wherein the intermediate suspension comprises a suspension of unprecipitated particulate additive associated with the ADH polymer in the ADH base polymer solution; and (e) a final suspension. Purifying the intermediate suspension with a solid medium in a temperature range and pressure range sufficient to produce a sol., Wherein a portion of the particulate additive associated with the ADH polymer is retained by the solid medium. And (f) the separated and purified ADH polymer, wherein the final suspension comprises a suspension of unretained particulate additive associated with the ADH polymer in the ADH base polymer solution. Separating the dissolution step solvent from the final suspension at a temperature and pressure range sufficient to produce the ADH polymer, wherein the separated and purified ADH polymer is the ADH-based polymer. And the ADH polymer dispersed in the separated and purified ADH polymer at a concentration lower than the concentration of the particulate additive associated with the ADH polymer in the ADH polymer in the rAHP. And a step including (g) step b (extraction step), c (dissolution step), d (sedimentation step), e (purification step), and f (separation step). Repeated once with the TPE, PP, PE, PET, cellulose, and the domain of TPA, PP, PE, cellulose, and PAA polymer, once and with the TPE, each collection of precipitated particulate additives from the previous iteration of bf. The TPE, PP, PE, and, in sequence, from the base polymer to the PP base polymer, then to the PE base polymer, and finally to the PET base polymer. A process for producing a separated and purified soluble polymer through extracting, dissolving, precipitating, purifying, and separating an ET base polymer, the sequence comprising: producing a separated and purified TPE polymer. A separated and purified PP polymer is produced, a separated and purified PE polymer is produced, a separated and purified TPE polymer is produced and a final collection of precipitated particulate additive and cellulose and PAA polymer Proceeding until the domain is generated, once and at a step.

  In yet another embodiment of the present invention is a method of separating and purifying PP, cellulose and PAA polymers from regenerated absorbent hygiene products (rAHP), wherein the rAHP comprises the polymer and impurities. Comprises a PP-based polymer, a particulate additive associated with the PP polymer, and an extractable material associated with the PP polymer, wherein the particulate additive associated with the PP polymer is present at a certain concentration. Dispersed in a PP base polymer, the PP polymer is a soluble polymer, the cellulose and the PAA polymer are non-soluble polymers, the impurities are particulate matter associated with the impurities, and Extractable material associated with impurities, wherein the extractable material in the rAHP is associated with the polymer. And a said extractable material associated with extractable material and the impurities, the extractable material in the RAHP is present in a concentration that is in the RAHP, method is provided. The method comprises: (a) obtaining the rAHP, wherein the rAH is selected from the group consisting of products after consumer use, products after industrial use, and combinations thereof; b) extracting the rAHP with an extraction solvent at a temperature above about 100 ° C. and a pressure above about 150 psig (1 MPa), wherein the extraction solvent has a normal boiling point of less than about 70 ° C. Producing a rAHP (erAHP), the extractable material having a concentration in the erAHP that is lower than the concentration of the extractable material in the rAHP, and (c) the PP-based polymer is dissolved. By contacting the erAHP with the dissolution process solvent in a temperature range and pressure range sufficient to solubilize the process solvent, the rAHP Dissolving the PP-based polymer to form an initial suspension, the initial suspension comprising the particulate additive and cellulose and PAA associated with the PP polymer in a PP-based polymer solution. A process comprising a suspension of domains of polymer, and (d) a collection of precipitated particulate additives and a domain of the cellulose and PAA polymer, and a temperature range sufficient to produce an intermediate suspension. And a step of settling the initial suspension in a pressure range, wherein the settled collection of particulate additives comprises particulate additives associated with the PP polymer, and the intermediate suspension is A process comprising a suspension of unprecipitated particulate additives associated with the PP polymer in a PP base polymer solution, and (e) a temperature range sufficient to produce a final suspension. And purifying the intermediate suspension with a solid medium in a pressure range, wherein a portion of the particulate additive associated with the PP polymer is retained by the solid medium and the final suspension comprises: A step comprising a suspension of unretained particulate additives associated with the PP polymer in the PP base polymer solution, and (f) a temperature range sufficient to produce a separated and purified PP polymer. And a step of separating the dissolution step solvent from the final suspension in a pressure range, wherein the separated and purified PP polymer is the PP base polymer and the PP polymer in the PP polymer in the rAHP. The particulate additive associated with the PP polymer dispersed in the separated and purified PP polymer at a concentration lower than the concentration of the particulate additive associated with And a step of including an agent.

  In yet another embodiment of the present invention, a method of separating and purifying a polymer from a recycled product (rP), wherein the rP comprises the polymer and impurities, the polymer being associated with a base polymer and the polymer. And a particulate additive associated with the polymer, wherein the particulate additive associated with each polymer is dispersed in the base polymer at a concentration and the polymer is dissolved. Selected from the group consisting of soluble polymers, insoluble polymers, and mixtures thereof, wherein the impurities include particulate matter associated with the impurities and extractable materials associated with the impurities, and The extractable material comprises the extractable material associated with the polymer and the extractable material associated with the impurities, and the extractable material in the rP. Capacity material is present in a concentration that is in the rP, method is provided. The method comprises (a) obtaining an rP selected from the group consisting of a product after consumer use, a product after industrial use, and combinations thereof; and (b) the size of the rP is less than about 10 mm. Reducing the particles to the largest dimension, (c) solid separating each polymer of the rP of interest in the polymer stream and processing each polymer stream containing the soluble polymer separately in a process that includes: (1) extracting the polymer stream containing the soluble polymer with an extraction solvent at a temperature above about 100 ° C. and a pressure above about 150 psig (1 MPa), wherein the extraction solvent is below about 70 ° C. The extraction having a normal boiling point produces an extracted polymer, wherein the extractable material is lower than the concentration of the extractable material in the rP. And (2) contacting the extracted polymer with a dissolution process solvent in a temperature range and pressure range sufficient to solubilize the soluble base polymer in the dissolution process solvent. Thereby dissolving the soluble polymer to form an initial suspension, wherein the initial suspension is a suspension of the particulate additive associated with the first soluble polymer. And (3) allowing the initial suspension to settle in a temperature range and pressure range sufficient to produce a collection of settled particulate additive and an intermediate suspension. , The settled particulate additive collection comprises particulate additive associated with the first soluble polymer, and the intermediate suspension comprises the first soluble base polymer solution in the first soluble base polymer solution. 1 soluble polymer And (4) the intermediate suspension using a solid medium in a temperature range and a pressure range sufficient to produce a final suspension, comprising: A step of purifying the liquid, wherein the portion of the particulate additive associated with the first soluble polymer is retained by the solid medium, and the final suspension is the first soluble base polymer solution. A) comprising a suspension of unretained particulate additive associated with the first soluble polymer in (5) sufficient to produce a separated and purified first soluble polymer A step of separating the dissolution step solvent from the final suspension in an appropriate temperature range and a pressure range, wherein the separated and purified first soluble polymer is the first soluble base polymer, in the first soluble polymer in rP Related to the first soluble polymer dispersed in the separated and purified first soluble polymer at a concentration lower than the concentration of the particulate additive associated with the first soluble polymer And a step of containing the particulate additive.

It is a block flow diagram which shows the main processes of one embodiment of the present invention. It is a block flow diagram which shows the main processes of another embodiment of the present invention.

I DEFINITIONS As used herein, the term “recycled product” (rP) refers to a product that was previously used for some purpose and then recovered for further processing.

  As used herein, the term "recycled film" (rF) refers to a film previously used for a purpose and then recovered for further processing.

  As used herein, the term "regenerated absorbent hygiene product" (rAHP) was previously used for some purpose and then recovered for further processing. , For example, baby diapers, feminine protection products and adult incontinence products).

  As used herein, the term "product after consumer use" refers to product used by the end consumer and disposed of in a waste stream.

  As used herein, the term "post-industrial product" refers to a product that has been manufactured but not yet used by the consumer, and is typically waste product from the manufacturing process.

  As used herein, the term "post-consumer recycled material" (PCR) refers to material produced after it has been used by the end consumer and disposed of in a waste stream.

  As used herein, the term "polymer" refers to a material that includes a base polymer, particulate additives associated with the polymer, and extractable materials associated with the polymer.

  As used herein, the term "base polymer" refers to the polymer prior to the addition of any additive package (either particulate or extractable) (ie, the base polymer is unmodified). .

  As used herein, the term "particulate additive" refers to particles that are added to a base polymer before the polymer or article is commercially sold. Non-limiting examples of such particulate additives that can be used in the case of both soluble and insoluble base polymers include fining agents, flame retardants, fillers, reinforcing agents, antacids, stabilizers. Agents, antioxidants, slid agents, antiblocking agents, lubricants, release agents, nucleating agents, and pigments.

  As used herein, the term "extractable material" refers to a material that can be extracted with an extraction solvent.

As used herein, the term "soluble polymer" refers to a polymer that is soluble in a solvent at the molecular level. Further, the thermodynamic stability of the polymer / solvent solution can be described by Equation 1 below:
ΔG _mix = ΔH _mix −TΔS _mix Equation 1
(Where ΔG _mix is the Gibbs free energy change of the mixing of the soluble polymer and the solvent, ΔH _mix is the enthalpy change of the mixing, T is the absolute temperature, and ΔS _mix is the entropy of the mixing). . The Gibbs free energy must be negative and minimal to maintain a stable solution of the soluble polymer in the solvent. Therefore, any combination of soluble polymer and solvent that minimizes the negative Gibbs free energy at the appropriate temperature and pressure can be used in the present invention.

  As used herein, the term "insoluble polymer" refers to a polymer that is insoluble in a solvent at the molecular level.

  As used herein, the term "impurities" refers to unwanted or unwanted materials that were present in rP and were not part of the polymer used to make the product (eg, impurities. Is the material that adheres to the product during its use, disposal process, or rP regeneration process). These impurities include particulate matter associated with the impurities and extractable materials associated with the impurities.

  As used herein, the terms "extraction solvent" and "dissolution process solvent" refer to substances that can exist in a liquid state under specified temperature and pressure conditions. In some embodiments, the extraction solvent and the dissolution process solvent may have a substantially homogeneous chemical composition of one molecule or isomer, while in other embodiments, the extraction solvent and the dissolution process solvent are: It may be a mixture of several different molecular compositions or isomers. Furthermore, in some embodiments of the invention, the terms "extraction solvent" and "dissolution process solvent" also apply to substances at, near, or above the critical temperature and pressure (critical point) of the substance. obtain. Those of ordinary skill in the art are well aware that a substance beyond its critical point is known as a "supercritical fluid," which does not have the typical physical properties (ie, density) of a liquid. Has been.

  As used herein, the term “normal boiling point” refers to the boiling point established by the International Union of Pure and Applied Chemistry (IUPAC) at exactly 100 kPa (1 bar, 14.5 psia, 0.9869 atm) absolute pressure. ..

  As used herein, the term “standard enthalpy of vaporization change” refers to the enthalpy change required for a given amount of a substance to change from a liquid to a vapor at the normal boiling point of the substance.

  As used herein, the term "polymer solution" refers to a solution of the base polymer dissolved in a solvent.

  As used herein, the term "sedimentation" refers to the process of precipitating suspended particles in response to forces (typically gravity) acting on the particles. For purposes of the present invention, the terms "settling" and "spinning" are used interchangeably.

  As used herein, the term "solid medium" refers to a substance that exists in the solid state under the conditions of use. The solid medium can be crystalline, semi-crystalline, or amorphous. The solid medium may be granular and provided in different shapes (ie spheres, cylinders, pellets, etc.). If the solid medium is granular, its particle size and particle size distribution may be defined by the mesh size used to classify the granular medium. An example of a standard mesh size notation can be found in the American Society for Testing and Materials (ASTM) standard ASTM E11, "Standard Specification for Woven Wire Test Sieve Clost and Test Sieves." The solid medium may also be a non-woven fiber mat or woven fabric.

  As used herein, the term "purified polymer" refers to a polymer in which the particulate additive and the extractable material have a concentration lower than that in the same polymer prior to the extraction, dissolution, precipitation, and purification steps. Point to. For the purposes of the present invention, the terms "purified polymer" and "purer polymer" have the same meaning and are used interchangeably.

  As used herein, the term "separated and purified polymer" refers to a purified polymer separated from other polymers.

  As used herein, the term "extraction" refers to the process of moving a solute species across a phase boundary from a liquid phase (or solid matrix) to another immiscible liquid phase. The driving force for extraction is explained by the theory of distribution.

  As used herein, the term "extracted" refers to a material that has less solute species (ie, extractable material) than the same material before the extraction step.

  As used herein, the term "extracted rAHP" refers to an rAHP that has less solute species (ie, extractable material) than the same rAHP before the extraction step.

  As used herein, the term "virgin-like polymer" refers to a polymer that is essentially free of particulate additives, extractable materials, and impurities, is homogeneous, and has properties similar to its base polymer. Point to. For purposes of the present invention, the terms "virgin-like polymer" and "base polymer" are used interchangeably.

  As used herein, the term "oligomeric acrylic acid" (OAA) is less than 1,000 AA units, as opposed to AA polymer (PAA), which refers to a molecular complex of more than 1,000 AA units. Refers to the molecular complex of.

  As used herein, the terms "poly (acrylic acid)" and "PAA" refer to acrylics used in various applications such as superabsorbent polymers (SAPs), adhesives, coatings, flocculants and the like. Refers to a polymer of acids.

  As used herein, any reference to international units of pressure (eg, MPa) refers to gauge pressure.

II Polymer Separation and Purification Methods Surprisingly, certain solvents exhibiting temperature and pressure dependent polymer solubilities in the preferred embodiment were polymer, especially regenerated or recycled, when used in a relatively simple process. It has been found that the polymer in the product can be separated and purified to near virgin quality. Each of these polymers includes a base polymer, particulate additives, and extractable materials. The process illustrated in FIG. 1 obtains the recycled product (step a in FIG. 1) and can subsequently be extracted from the recycled product using the extraction solvent at the extraction temperature (T _E ) and extraction pressure (P _E ). extract the material (step b in Figure 1), followed by dissolution temperature (T _D) and dissolution pressure (P _D) by dissolving the base polymer to dissolving process solvent in (step c in Figure 1), the base polymer solution of forming a suspension of particulate additives, followed by dissolution temperature (T _D) and dissolution pressure (P _D) of the polymer suspension was allowed to settle in the (step d in Figure 1), of the base polymer solution to form a suspension of particulate additive which has not precipitated in the previous step, followed by it in the dissolution temperature (T _D) and dissolution pressure (P _D) of the suspension by contact with a solid medium Purified (step e in Figure 1), base polymer solution Reducing the concentration of particulate additive therein, followed by separating the polymer from the dissolution process solvent (step f in Figure 1) to produce a separated and purified polymer. The process steps of dissolving, precipitating, purifying and separating are then repeated for each one of the soluble polymers in the recycled product.

  In one embodiment of the invention, the separated and purified polymer, which can be sourced from waste streams after consumer use, is essentially free of particulate additives (eg, free of pigments). It is free of impurities, free of extractable materials (eg odorless), homogeneous and similar in properties to virgin polymers. Further, in a preferred embodiment of the present invention, the physical properties of the dissolution step solvent of the present invention may allow for a more energy efficient method for separating the solvent from the purified polymer.

Recycled Product For the purposes of this invention, recycled product (rP) refers to either the product or the package. A non-limiting example of a product or packaging after consumer use is from a roadside recycling stream where the end consumer puts the used product or packaging in a designated container for collection by a garbage carrier or recycler. The resulting product or packaging, and the product or packaging obtained from the in-store "collection" program in which the consumer brings the waste or packaging to the store and places the waste or packaging in a designated collection container. A non-limiting example of post-industrial waste may be waste polymers produced during the manufacture or transportation of goods or products collected by the manufacturer as unusable materials (ie, cuttings, out-of-specification materials). , Starting waste). Non-limiting examples of waste from special waste streams are electronic waste, also known as e-waste, automobiles, and waste from the recycling of used carpet and textiles.

  In one embodiment of the invention, the rP is selected from the group consisting of post consumer use products, post industrial use products, post commercial use products, specialty waste streams, and combinations thereof. In another embodiment of the invention, the rP is selected from the group consisting of post consumer use products, post industrial use products, and combinations thereof. In yet another embodiment of the invention, a method of separating and purifying a polymer from recycled product (rP) comprises obtaining the rP.

  In yet another embodiment of the present invention, the rP is recycled film. In one embodiment of the invention, the rF comprises at least 2 polymers. In another embodiment of this invention, the rF comprises at least 4 polymers. In yet another embodiment of the invention, the rF comprises a multilayer film. In yet another embodiment of the present invention, the rF comprises a film having at least two layers. These layers in rF may include tie layers known to those skilled in the art. Non-limiting examples of polymers used in the layers of the multilayer film include PE, PP, PET, polystyrene (PS), poly (lactic acid), PLA, ionomers, polyamides (PA), and It is polybutylene succinate (PBS).

  In one embodiment of the invention, the rP is a regenerated absorbent hygiene product (rAHP). In another embodiment of the invention, the rAHP is selected from the group consisting of baby diapers, feminine protection products, and adult incontinence products.

  In one embodiment of the invention, the rP comprises the polymer and impurities. For the purposes of the present invention, the polymer in the recycled product is a homogeneous polymer or a mixture of several different polymer compositions. Non-limiting examples of polymers are PE, PP, PET, ADH, TPE, cellulose, hemicellulose, lignin, PAA, PLA, ionomers, PA, and PBS. Non-limiting examples of PP compositions include homopolymers of propylene, copolymers of propylene and ethylene (including "impact" and "random clarified" copolymers), copolymers of propylene and alpha-olefins. , Polypropylene rubber, as well as other soluble polypropylene compositions that may be apparent to those skilled in the art. In one embodiment of the invention, the polymer is soluble. In another embodiment of the invention, the polymer is insoluble. In yet another embodiment of the present invention, the polymer is selected from the group consisting of soluble polymers, insoluble polymers, and mixtures thereof. In one embodiment of the invention, the soluble polymer is selected from the group consisting of PP, PE, PET, ADH, TPE, and mixtures thereof. In another embodiment of the invention the first soluble polymer is ADH, the second soluble polymer is TPE, the third soluble polymer is PP and the fourth soluble polymer. The soluble polymer is PE and the fifth soluble polymer is PET. In yet another embodiment of the present invention, the insoluble polymer is selected from the group consisting of cellulose, hemicellulose, lignin, and PAA, and mixtures thereof. In yet another embodiment of the present invention, the non-soluble polymer is cellulose and PAA.

  Non-limiting examples of impurities are dust particles, stains, odors from product use, disposal, and reclamation processes, and particles from other products. In another embodiment of the invention, the impurities include particulate matter associated with the impurities and extractable materials associated with the impurities.

  The polymer in the recycled product comprises a base polymer, particulate additives associated with the polymer, and extractable materials associated with the polymer. Particulate additives are added to the base polymer during polymerization of the base polymer or conversion into a product. Non-limiting examples of particulate additives include fining agents, flame retardants, fillers, reinforcing agents, antacids, stabilizers, antioxidants, slip agents, anti-tacking agents, lubricants, mold release agents, cores. Forming agents, pigments, and plasticizers. Non-limiting examples of pigments are organic pigments (eg copper phthalocyanine), inorganic pigments (eg titanium dioxide) and other pigments as may be apparent to those skilled in the art. One non-limiting example of an organic pigment is Basic Yellow 51. A non-limiting example of an antistatic agent is glycerol monostearate and the slip agent is erucamide. A non-limiting example of a stabilizer is octadecyl-3- (3,5-di-tert.butyl-4-hydroxyphenyl) -propionate. Non-limiting examples of fillers are calcium carbonate, talc, and fiberglass.

  In one embodiment of the present invention, the particulate additive is a fining agent, flame retardant, filler, reinforcing agent, antacid, stabilizer, antioxidant, slip agent, anti-sticking agent, lubricant, release agent. Selected from the group consisting of agents, nucleating agents, pigments, and mixtures thereof. In another embodiment of the invention, the particulate additive associated with the polymer is dispersed in the base polymer at a concentration.

  In one embodiment of the invention, the concentration of the particulate additive associated with each soluble polymer dispersed in each soluble base polymer in the rP is less than about 5%. In another embodiment of this invention, the concentration of the particulate additive associated with each soluble polymer dispersed in each soluble base polymer in the rP is about 3%. In yet another embodiment of the invention, the concentration of the particulate additive associated with each soluble polymer dispersed in each soluble base polymer in the rP is less than about 3%. In yet another embodiment of the present invention, the concentration of the particulate additive associated with each soluble polymer dispersed in each soluble base polymer in the rP is less than about 1%. In one embodiment of the invention, the concentration of the particulate additive associated with each soluble polymer dispersed in each soluble base polymer in the rP is less than about 0.1%.

  In one embodiment of the invention, the concentration of the particulate additive associated with each soluble polymer dispersed in each soluble base polymer in the rAHP is less than about 5%. In another embodiment of this invention, the concentration of the particulate additive associated with each soluble polymer dispersed in each soluble base polymer in the rAHP is about 3%. In yet another embodiment of the invention, the concentration of the particulate additive associated with each soluble polymer dispersed in each soluble base polymer in the rAHP is less than about 3%. In yet another embodiment of the present invention, the concentration of the particulate additive associated with each soluble polymer dispersed in each soluble base polymer in the rAHP is less than about 1%. In one embodiment of the invention, the concentration of the particulate additive associated with each soluble polymer dispersed in each soluble base polymer in the rAHP is less than about 0.1%.

  In one embodiment of the invention, the concentration of the particulate additive associated with the PP polymer dispersed in the PP base polymer in the rP is less than about 5%. In another embodiment of this invention, the concentration of the particulate additive associated with the PP polymer dispersed in the PP base polymer in the rP is about 3%. In yet another embodiment of the invention, the concentration of the particulate additive associated with the PP polymer dispersed in the PP base polymer in the rP is less than about 3%. In yet another embodiment of the invention, the concentration of the particulate additive associated with the PP polymer dispersed in the PP base polymer in the rP is less than about 1%. In one embodiment of the invention, the concentration of the particulate additive associated with the PP polymer dispersed in the PP base polymer in the rP is less than about 0.1%.

  In one embodiment of the invention, the concentration of the particulate additive associated with PP polymer dispersed in the PP base polymer in the rAHP is less than about 5%. In another embodiment of this invention, the concentration of the particulate additive associated with the PP polymer dispersed in the PP base polymer in the rAHP is about 3%. In yet another embodiment of the invention, the concentration of the particulate additive associated with the PP polymer dispersed in the PP base polymer in the rAHP is less than about 3%. In yet another embodiment of the invention, the concentration of the particulate additive associated with the PP polymer dispersed in the PP base polymer in the rAHP is less than about 1%. In one embodiment of the invention, the concentration of the particulate additive associated with the PP polymer dispersed in the PP base polymer in the rAHP is less than about 0.1%.

  In one embodiment of the invention, the extractable material in the rP comprises the extractable material associated with the polymer and the extractable material associated with the impurity. In another embodiment of the invention, the extractable material in the rP is present at a concentration in the rP. Non-limiting examples of extractable materials associated with either polymers or impurities are dyes, fragrances, flavors, and mixtures thereof. Extractable materials associated with either the polymer or the impurities include residual processing aids added to the polymer, residual product formulations that come into contact with the polymer during use of the product, and other materials such as during and after waste collection. It can be any other extractable material that may have been intentionally added to the polymer or unintentionally incorporated into the polymer during its accumulation with the waste.

  In one embodiment of the invention, the method further comprises sterilizing the rP after the obtaining step. In another embodiment of the invention, the method further comprises the step of sterilizing the rAHP after the obtaining step. Since AHP is considered a biohazardous product after use, sterilization is required to eliminate the microbial load on rP, and more specifically on rAHP. Sterilization processes and conditions are well known to those of skill in the art and can be performed in autoclaves, Parr reactors, and similar equipment.

  In one embodiment of the invention, the method further comprises reducing the size of the rAHP after the obtaining step and before the extracting step. In another embodiment of the invention, the reducing step comprises milling, cutting, shearing, or a combination thereof.

  In one embodiment of the invention, the method comprises the steps of obtaining the rP, extracting the rP with an extraction solvent, and dissolving the first soluble base polymer in a dissolution step solvent to initially suspend. A step of producing a liquid, a step of settling the initial suspension to produce an intermediate suspension, a step of purifying the intermediate suspension with a solid medium to produce a final suspension, and a step of dissolving the solution. A step of separating a process solvent from the final suspension to produce a separated and purified first soluble polymer, and the dissolution step, the precipitation step, the purification step using all remaining soluble polymer And a step of repeating the separation step.

Extraction Step In one embodiment of the invention, a method of separating and purifying a polymer from a recycled product (rP) comprises extracting the rP with an extraction solvent at a temperature above about 100 ° C. and a pressure above about 150 psig (1 MPa). Wherein the extraction solvent has a normal boiling point of less than about 70 ° C. to produce extracted rP (erP) and the extractable material is the extractable material of the rP. Having a concentration of erP that is lower than the concentration. In another embodiment of the invention, the extraction step is a step of extracting the rAHP with an extraction solvent at a temperature above about 100 ° C. and a pressure above about 150 psig (1 MPa), wherein the extraction solvent is about 70 Having a normal boiling point of less than 0 ° C. produces extracted rAHP (erAHP) such that the extractable material has a concentration in the erAHP that is lower than the concentration of the extractable material in the rAHP. Having, including steps. In yet another embodiment of the invention, the extraction step is a step of extracting the rF with an extraction solvent at a temperature above about 100 ° C. and a pressure above about 150 psig (1 MPa), wherein the extraction solvent comprises about A concentration in the erF that produces an extracted rF (erF) by having a normal boiling point of less than 70 ° C. and the extractable material is lower than the concentration of the extractable material in the rF. Including a step.

  The extraction solvent of the present invention has a normal boiling point of less than about 70 ° C. Pressurization keeps the extraction solvent having a normal boiling point below the operating temperature range of the present invention with little or no solvent vapor present. In one embodiment of the invention, the extraction solvent having a normal boiling point of less than about 70 ° C. is selected from the group consisting of carbon dioxide, ketones, alcohols, ethers, esters, alkenes, alkanes, and mixtures thereof. In another embodiment of the invention, the extraction solvent is selected from the group consisting of olefinic hydrocarbons, aliphatic hydrocarbons, and mixtures thereof. Non-limiting examples of extraction solvents having a normal boiling point of less than about 70 ° C. are carbon dioxide, acetone, methanol, dimethyl ether, diethyl ether, ethyl methyl ether, tetrahydrofuran, methyl acetate, ethylene, propylene, 1-butene, 2- Butene, isobutylene, 1-pentene, 2-pentene, branched isomers of pentene, 1-hexene, 2-hexene, methane, ethane, propane, n-butane, isobutane, n-pentane, isopentane, neopentane, n- Hexane, isomers of isohexane, and other materials as may be apparent to one of ordinary skill in the art. In one embodiment of the invention, the extraction solvent in n-butane. In another embodiment of the invention, the extraction solvent in propane. In yet another embodiment of the invention, the extraction solvent in pentane. In yet another embodiment of the present invention, the extraction solvent in hexane.

  The choice of extraction solvent and dissolution process solvent used will determine the temperature and pressure ranges used to carry out the process of the invention. A review of the behavior of polymer phases in solvents of the type described in this invention is provided in the following references: Kirby and McHugh. (1999) Chem. Rev. 99: 565-602.

  In one embodiment of the invention, a method of separating and purifying a polymer from recycled product (rP) comprises contacting the rP with the extraction solvent at a temperature and pressure at which the polymer is essentially insoluble in the extraction solvent. including. Without wishing to be bound by theory, applicants can control the temperature and pressure dependent solubilities to prevent the extraction solvent from completely solubilizing the polymer, but the extraction solvent is We believe that any extractable material that diffuses inside can be extracted.

  In one embodiment of the invention, the extraction may be accomplished by fixing the temperature of the polymer / extraction solvent system and then controlling the pressure below the pressure or pressure range at which the polymer dissolves in the extraction solvent. In another embodiment of the present invention, extraction may be accomplished by fixing the pressure of the polymer / extraction solvent system and then controlling the temperature below the temperature or temperature range at which the polymer dissolves in the extraction solvent. The temperature and pressure controlled extraction of the polymer with the extraction solvent may be arranged to allow continuous extraction of the polymer with the extraction solvent using a suitable pressure vessel. In one embodiment of the invention, the pressure vessel is a continuous liquid-liquid extraction column in which the molten polymer is pumped to one end of the extraction column and the extraction solvent is the same or opposite of the extraction column. It may be a column pumped to the side end. In another embodiment of the invention, the fluid containing the extracted impurities is removed from the process. In another embodiment of the invention, the fluid containing the extracted material is purified, recovered and recycled for use in the extraction step or different steps of the process.

  In one embodiment of the present invention, the extraction step may be carried out in a batch process in which the regenerated product is fixed in a pressure vessel and the extraction solvent is continuously pumped through the fixed product phase. The extraction time or amount of extraction solvent used depends on the desired purity of the separated and purified polymer and the amount of extractable material in the starting recycled product.

  In one embodiment of the invention, the extraction process is in batch mode. In another embodiment of the invention the extraction process is in continuous mode.

  In another embodiment of the present invention, erP is contacted with a solid medium in a separation step, as described in the "Purification Step" section below. In yet another embodiment of the invention, the extracting step comprises using an adsorbent to extract a portion of the extractable material. Non-limiting examples of adsorbents include silicon oxide (silica), silica gel, aluminum oxide (alumina), iron oxide, aluminum silicate, magnesium silicate, amorphous volcanic glass, recycled glass, sand, quartz, diatomaceous earth, Zeolite, perlite, clay, fuller's earth, bentonite clay, metal organic framework (MOF), covalent organic framework (COF), zeolite imidazolate framework (ZIF) , Anthracite, carbon black, coke, and activated carbon. In yet another embodiment of the present invention, the adsorbent is selected from the group consisting of activated carbon, zeolite, MOF, COF, (ZIF), and mixtures thereof.

  In one embodiment of the invention, the method comprises contacting the rP with an extraction solvent at a temperature and pressure at which the polymer melts and is in a liquid state. In another embodiment of the invention, the rP is contacted with the extraction solvent at a temperature and pressure where the polymer is in the solid state.

  In one embodiment of the invention, the method of separating and purifying PP from rP comprises contacting PP with an extraction solvent at a temperature and pressure at which PP remains essentially undissolved. In another embodiment of the invention, the method of separating and purifying PP from rP comprises contacting the PP with n-butane at a temperature of about 80 ° C to about 220 ° C. In yet another embodiment of the invention, the method of separating and purifying PP from rP comprises contacting the PP with n-butane at a temperature of about 100 ° C to about 200 ° C. In yet another embodiment of the present invention, the method of separating and purifying PP from rP comprises contacting the PP with n-butane at a temperature of about 130 ° C to about 180 ° C. In one embodiment of the invention, the method of separating and purifying PP from rP comprises contacting the PP with n-butane at a temperature of about 110 ° C to about 170 ° C.

  In one embodiment of the present invention, a method of separating and purifying PP from rP comprises contacting the PP with n-butane at a pressure of about 150 psig (1 MPa) to about 3,000 psig (20.7 MPa). In another embodiment of the invention, a method of separating and purifying PP from rP comprises contacting the PP with n-butane at a pressure of about 1,000 psig (6.9 MPa) to about 2,750 psig (19 MPa). including. In yet another embodiment of the present invention, a method of separating and purifying PP from rP comprises converting the PP to n-butane at a pressure of about 1,500 psig (10.3 MPa) to about 2,500 psig (17.2 MPa). Including contact. In one embodiment of the invention, a method of separating and purifying PP from rP involves contacting the PP with n-butane at a pressure of about 1,100 psig (7.6 MPa) to about 2,100 psig (14.5 MPa). Including that.

  In one embodiment of the invention, the method of separating and purifying PP from rP comprises contacting the PP with propane at a temperature of about 80 ° C to about 220 ° C. In another embodiment of the invention, the method of separating and purifying PP from rP comprises contacting the PP with propane at a temperature of about 100 ° C to about 200 ° C. In yet another embodiment of the present invention, the method of separating and purifying PP from rP comprises contacting the PP with propane at a temperature of about 130 ° C to about 180 ° C.

  In one embodiment of the present invention, a method of separating and purifying PP from rP comprises contacting the PP with propane at a pressure of about 200 psig (1.4 MPa) to about 8,000 psig (55.2 MPa). In another embodiment of the invention, a method of separating and purifying PP from rP comprises contacting the PP with propane at a pressure of about 1,000 psig (6.9 MPa) to about 6,000 psig (41.4 MPa). including. In yet another embodiment of the present invention, a method of separating and purifying PP from rP comprises contacting the PP with propane at a pressure of about 2,000 psig (13.8 MPa) to about 4,000 psig (27.6 MPa). Including that.

  In one embodiment of the invention, the concentration of the extractable material in the erP is less than about 90% of the concentration of the extractable material in the rP. In another embodiment of the invention, the concentration of the extractable material in the erP is less than about 75% of the concentration of the extractable material in the rP. In yet another embodiment of the invention, the concentration of the extractable material in the erP is less than about 50% of the concentration of the extractable material in the rP. In yet another embodiment of the invention, the concentration of the extractable material in the erP is about half the concentration of the extractable material in the rP.

  In one embodiment of the invention, the concentration of the extractable material in the erAHP is less than about 90% of the concentration of the extractable material in the rAHP. In another embodiment of the invention, the concentration of the extractable material in the erAHP is less than about 75% of the concentration of the extractable material in the rAHP. In yet another embodiment of the invention, the concentration of the extractable material in the erAHP is less than about 50% of the concentration of the extractable material in the rAHP. In yet another embodiment of the invention, the concentration of the extractable material in the erAHP is about half the concentration of the extractable material in the rAHP.

  In one embodiment of the invention, the erP is essentially free of the extractable material. In another embodiment of the invention, the erAHP is essentially free of the extractable material. In yet another embodiment of the invention, the concentration of the extractable material in the erP is further reduced during the purification step. In yet another embodiment of the invention, the concentration of the extractable material in the erAHP is further reduced during the purification step.

  In one embodiment of the invention, a method for separating and purifying a PP polymer from rAHP, wherein the temperature range in the extraction step is about 110 ° C to about 170 ° C and the pressure range in the extraction step is about 1 ° C. , 100 psig (7.6 MPa) to about 2,100 psig (14.5 MPa).

  In one embodiment of the present invention, a method for separating and purifying a polymer from rP, wherein the extraction solvent is propane, the temperature in the extraction step is greater than about 100 ° C, and the pressure in the extraction step is A method is provided that is greater than about 150 psig (1 MPa) and less than about 1,500 psig (10.3 MPa). Another embodiment of the invention is a method of separating and purifying a polymer from rP, wherein the extraction solvent is n-butane, the temperature in the extraction step is greater than about 100 ° C, and the extraction step is in the extraction step. A method is provided wherein the pressure is greater than about 150 psig (1 MPa) and less than about 900 psig (6.2 MPa). In yet another embodiment of the invention, a method of separating and purifying a polymer from rP, wherein the extraction solvent is pentane, the temperature in the extraction step is greater than about 100 ° C, and the extraction step is A method is provided wherein the pressure is greater than about 150 psig (1 MPa) and less than about 500 psig (3.4 MPa). In yet another embodiment of the present invention, a method of separating and purifying a polymer from rP, wherein the extraction solvent is hexane, the temperature in the extraction step is greater than about 100 ° C, and the extraction step in the extraction step is A method is provided wherein the pressure is about 150 psig (1 MPa).

Dissolution Step In one embodiment of the present invention, a method of separating and purifying a polymer from a recycled product (rP) is performed in a temperature range and a pressure range sufficient to solubilize a first soluble base polymer in a dissolution step solvent. A step of generating an initial suspension by contacting the erP with the dissolution step solvent to dissolve the first soluble base polymer of the rP, the initial suspension comprising: Comprising a suspension of the particulate additive associated with the first soluble polymer and the domains of all remaining polymer in a first soluble base polymer solution, the first soluble base polymer comprising: Comprising a solubilization range that is less than the solubilization range of the remaining soluble base polymer. In another embodiment of the invention, a method of separating and purifying a polymer from a regenerated absorbent hygiene product (rAHP) comprises a temperature range sufficient to solubilize a first soluble base polymer in a dissolution process solvent and Generating an initial suspension by dissolving the first soluble base polymer of the rAHP by contacting the erAHP with the dissolution step solvent in a pressure range, the initial suspension A liquid comprises a suspension of the particulate additive associated with the first soluble polymer and the domains of all remaining polymer in a first soluble base polymer solution, the first soluble base The polymer has a solubilization range that is less than the solubilization range of the remaining soluble base polymer. In yet another embodiment of the present invention, a method of separating and purifying a polymer from recycled film (rF) is performed in a temperature range and pressure range sufficient to solubilize a first soluble base polymer in a dissolution process solvent. A step of producing an initial suspension by the step of dissolving the first soluble base polymer of the rF by contacting the erF with the dissolution step solvent, the initial suspension comprising: Comprising a suspension of the particulate additive associated with the first soluble polymer and the domains of all remaining polymer in a first soluble base polymer solution, the first soluble base polymer comprising: Comprising a solubilization range that is less than the solubilization range of the remaining soluble base polymer. In yet another embodiment of the present invention, a method of separating and purifying ADH polymer from regenerated absorbent hygiene product (rAHP) comprises a temperature range and pressure sufficient to solubilize ADH base polymer in a dissolution process solvent. In a range, the erAHP is contacted with the dissolution step solvent to dissolve the ADH base polymer of the rAHP to produce an initial suspension, the initial suspension being ADH-based. A suspension of the particulate additive associated with the ADH polymer in a polymer solution and domains of TPE, PP, PE, PET, cellulose, and PAA polymer, wherein the ADH base polymer is the TPE, PP , PE, and PET-based polymers having a solubilization range less than that of the dissolution process domain. The containing TPE, PP, PE, PET, cellulose, and the PAA polymer, comprising the step. In one embodiment of the invention, a method of separating and purifying a PP polymer from a regenerated absorbent hygiene product (rAHP) comprises a temperature range and pressure range sufficient to solubilize the PP base polymer in a dissolution process solvent. A step of generating an initial suspension by the step of dissolving the PP base polymer of the rAHP by contacting the erAHP with the dissolution step solvent, wherein the initial suspension is a PP base polymer solution. Comprising a suspension of the particulate additive associated with the PP polymer and a domain of cellulose and PAA polymer therein.

  Without wishing to be bound by theory, Applicants believe that the temperature and pressure can be controlled to achieve thermodynamically favorable dissolution of the polymer in the dissolution process solvent. Furthermore, the temperature and pressure can be controlled in such a way that it is capable of dissolving a particular polymer or mixture of polymers and at the same time does not dissolve another polymer or mixture of polymers. This controllable dissolution allows the polymer to be separated from the polymer mixture or recycled product.

  In one embodiment of the present invention, a method for separating and purifying polymers is such that reclaimed products containing these polymers dissolve one of the polymers under the same temperature and pressure conditions, while the other polymer does not. And the step of dissolving in a solvent that remains as a domain in the suspension. The above process is then repeated for the other polymer.

  In one embodiment of the present invention, a method of separating and purifying a PP polymer from a regenerated absorbent hygiene product (rAHP), the PP polymer comprising a PP base polymer and a particulate additive associated with the PP polymer. And a extractable material associated with the PP polymer, the rAHP of the rAHP by contacting the rAHP with the dissolution process solvent at a temperature and conditions at which the PP base polymer dissolves in the dissolution process solvent. The step of dissolving the PP base polymer is included. Another embodiment of the invention is a method of separating and purifying a PP polymer from rAHP, the PP polymer comprising a PP base polymer, a particulate additive associated with the PP polymer, and the PP polymer. The extractable material comprises a step of dissolving the PP base polymer in n-butane at a temperature of about 90 ° C to about 220 ° C. In yet another embodiment of the present invention, a method of separating and purifying a PP polymer from rAHP, the PP polymer comprising a PP base polymer, a particulate additive associated with the PP polymer, and the PP polymer. The method, including associated extractable materials, comprises dissolving the PP-based polymer in n-butane at a temperature of about 100 ° C to about 200 ° C. In yet another embodiment of the present invention, a method for separating and purifying a PP polymer from rAHP, the PP polymer comprising a PP base polymer, a particulate additive associated with the PP polymer, and the PP polymer. And an extractable material related to the method, comprising dissolving the PP-based polymer in n-butane at a temperature of about 130 ° C to about 180 ° C.

  In one embodiment of the present invention, a method of separating and purifying a PP polymer from rAHP, the PP polymer being associated with the PP base polymer, a particulate additive associated with the PP polymer, and the PP polymer. The method, including extractable materials, comprises dissolving the PP base polymer in n-butane at a pressure of about 350 psig (2.4 MPa) to about 20,000 psig (137.9 MPa). Another embodiment of the invention is a method of separating and purifying a PP polymer from rAHP, the PP polymer comprising a PP base polymer, a particulate additive associated with the PP polymer, and the PP polymer. Of the PP-based polymer in n-butane at a pressure of about 350 psig (2.4 MPa) to about 4,000 psig (27.6 MPa). In yet another embodiment of the invention, a method of separating and purifying a PP polymer from rAHP, the PP polymer comprising a PP base polymer, a particulate additive associated with the PP polymer, and the PP polymer. The method, including the relevant extractable materials, comprises dissolving the PP base polymer in n-butane at a pressure of about 1,000 psig (6.9 MPa) to about 3,500 psig (24.1 MPa). In yet another embodiment of the present invention, a method of separating and purifying a PP polymer from rAHP, the PP polymer comprising a PP base polymer, a particulate additive associated with the PP polymer, and the PP polymer. And an extractable material associated with the method, comprising dissolving the PP base polymer in n-butane at a pressure of about 2,000 psig (13.8 MPa) to about 3,000 psig (20.7 MPa). ..

  In one embodiment of the present invention, a method for separating and purifying a PP polymer from rAHP, wherein the temperature range in the dissolution step is about 90 ° C to about 220 ° C and the pressure range in the dissolution step is about 350 psig. A method is provided that is between (2.4 MPa) and about 20,000 psig (137.9 MPa).

  In one embodiment of the present invention, a method for separating and purifying a PP polymer from a regenerated absorbent hygiene product (rAHP), the PP polymer comprising a PP base polymer and a particulate additive associated with the PP polymer. And a extractable material associated with the PP polymer, thereby dissolving the PP base polymer of the rAHP by contacting the rAHP with n-butane at a weight concentration of at least about 0.5%. Including the step of Another embodiment of the invention is a method of separating and purifying a PP polymer from rAHP, the PP polymer comprising a PP base polymer, a particulate additive associated with the PP polymer, and the PP polymer. And extracting the PP-based polymer in n-butane at a weight concentration of at least about 1%. In yet another embodiment of the invention, a method of separating and purifying a PP polymer from rAHP, the PP polymer comprising a PP base polymer, a particulate additive associated with the PP polymer, and the PP polymer. The method, including associated extractable materials, comprises dissolving the PP-based polymer in n-butane at a weight concentration of at least about 2%. In yet another embodiment of the present invention, a method of separating and purifying a PP polymer from rAHP, the PP polymer comprising a PP base polymer, a particulate additive associated with the PP polymer, and the PP polymer. And an extractable material associated with the method of claim 1, comprising dissolving the PP-based polymer in n-butane at a weight concentration of at least about 3%. In one embodiment of the present invention, a method for separating and purifying a PP polymer from a regenerated absorbent hygiene product (rAHP), the PP polymer comprising a PP base polymer and a particulate additive associated with the PP polymer. And a extractable material associated with the PP polymer to dissolve the PP base polymer of the rAHP by contacting the rAHP with n-butane at a weight concentration of at least about 4%. including. Another embodiment of the invention is a method of separating and purifying a PP polymer from rAHP, the PP polymer comprising a PP base polymer, a particulate additive associated with the PP polymer, and the PP polymer. And extracting the PP-based polymer in n-butane at a weight concentration of at least about 5%.

  In one embodiment of the present invention, a method for separating and purifying a PP polymer from a regenerated absorbent hygiene product (rAHP), the PP polymer comprising a PP base polymer and a particulate additive associated with the PP polymer. And a extractable material associated with the PP polymer, the method comprising dissolving the PP base polymer of the rAHP by contacting the rAHP with a dissolution process solvent at a weight concentration of about 20% or less. including. Another embodiment of the invention is a method of separating and purifying a PP polymer from rAHP, the PP polymer comprising a PP base polymer, a particulate additive associated with the PP polymer, and the PP polymer. The extractable material comprises a step of dissolving the PP base polymer in n-butane at a weight concentration of about 18% or less. In yet another embodiment of the invention, a method of separating and purifying a PP polymer from rAHP, the PP polymer comprising a PP base polymer, a particulate additive associated with the PP polymer, and the PP polymer. The method, including associated extractable materials, comprises dissolving the PP-based polymer in n-butane at a weight concentration of about 16% or less. In yet another embodiment of the present invention, a method of separating and purifying a PP polymer from rAHP, the PP polymer comprising a PP base polymer, a particulate additive associated with the PP polymer, and the PP polymer. And a extractable material related to the method of claim 1, comprising dissolving the PP-based polymer in n-butane at a weight concentration of about 14% or less. In one embodiment of the present invention, a method for separating and purifying a PP polymer from a regenerated absorbent hygiene product (rAHP), the PP polymer comprising a PP base polymer and a particulate additive associated with the PP polymer. And a extractable material associated with the PP polymer, the method comprising dissolving the PP base polymer of the rAHP by contacting the rAHP with a dissolution process solvent at a weight concentration of about 12% or less. including.

  In one embodiment of the present invention, a method of separating and purifying a PP polymer from a regenerated absorbent hygiene product (rAHP), the PP polymer comprising a PP base polymer and a particulate additive associated with the PP polymer. And an extractable material associated with the PP polymer, the PP of the rAHP by contacting the rAHP with propane at a temperature and conditions at which the PP base polymer dissolves in a dissolution process solvent. The step of dissolving the base polymer is included. Another embodiment of the invention is a method of separating and purifying a PP polymer from rAHP, the PP polymer comprising a PP base polymer, a particulate additive associated with the PP polymer, and the PP polymer. The extractable material comprises a step of dissolving the PP base polymer in propane at a temperature of about 90 ° C to about 220 ° C. In yet another embodiment of the present invention, a method of separating and purifying a PP polymer from rAHP, the PP polymer comprising a PP base polymer, a particulate additive associated with the PP polymer, and the PP polymer. The method, including associated extractable materials, comprises dissolving the PP-based polymer in propane at a temperature of about 100 ° C to about 200 ° C. In yet another embodiment of the present invention, a method for separating and purifying a PP polymer from rAHP, the PP polymer comprising a PP base polymer, a particulate additive associated with the PP polymer, and the PP polymer. And an extractable material related to the method, comprising the step of dissolving the PP base polymer in propane at a temperature of about 130 ° C to about 180 ° C.

  In one embodiment of the invention, a method of separating and purifying a PP polymer from rAHP, the PP polymer being associated with the PP base polymer, a particulate additive associated with the PP polymer, and the PP polymer. The method, including extractable materials, comprises dissolving the PP base polymer in propane at a pressure of about 2,000 psig (13.8 MPa) to about 8,000 psig (55.2 MPa). Another embodiment of the invention is a method of separating and purifying a PP polymer from rAHP, the PP polymer comprising a PP base polymer, a particulate additive associated with the PP polymer, and the PP polymer. The extractable material comprises a step of dissolving the PP base polymer in propane at a pressure of about 3,000 psig (20.7 MPa) to about 6,000 psig (41.4 MPa). In yet another embodiment of the present invention, a method of separating and purifying a PP polymer from rAHP, the PP polymer comprising a PP base polymer, a particulate additive associated with the PP polymer, and the PP polymer. The method, including associated extractable materials, comprises dissolving the PP-based polymer in propane at a pressure of about 3,500 psig (24.1 MPa) to about 5,000 psig (34.5 MPa).

  In one embodiment of the present invention, a method for separating and purifying a PP polymer from a regenerated absorbent hygiene product (rAHP), the PP polymer comprising a PP base polymer and a particulate additive associated with the PP polymer. And a extractable material associated with the PP polymer, the method comprising dissolving the PP base polymer of the rAHP by contacting the rAHP with propane at a weight concentration of at least about 0.5%. including. Another embodiment of the invention is a method of separating and purifying a PP polymer from rAHP, the PP polymer comprising a PP base polymer, a particulate additive associated with the PP polymer, and the PP polymer. And extracting the PP-based polymer in propane at a weight concentration of at least about 1%. In yet another embodiment of the invention, a method of separating and purifying a PP polymer from rAHP, the PP polymer comprising a PP base polymer, a particulate additive associated with the PP polymer, and the PP polymer. The method, including associated extractable materials, comprises dissolving the PP-based polymer in propane at a weight concentration of at least about 2%. In yet another embodiment of the present invention, a method of separating and purifying a PP polymer from rAHP, the PP polymer comprising a PP base polymer, a particulate additive associated with the PP polymer, and the PP polymer. And an extractable material related to the method, comprising dissolving the PP-based polymer in propane at a weight concentration of at least about 3%. In one embodiment of the present invention, a method for separating and purifying a PP polymer from a regenerated absorbent hygiene product (rAHP), the PP polymer comprising a PP base polymer and a particulate additive associated with the PP polymer. And an extractable material associated with the PP polymer, the method comprising dissolving the PP base polymer of the rAHP by contacting the rAHP with propane at a weight concentration of at least about 4%. . Another embodiment of the invention is a method of separating and purifying a PP polymer from rAHP, the PP polymer comprising a PP base polymer, a particulate additive associated with the PP polymer, and the PP polymer. And extracting the PP-based polymer in propane at a weight concentration of at least about 5%.

  In one embodiment of the present invention, a method for separating and purifying a PP polymer from a regenerated absorbent hygiene product (rAHP), the PP polymer comprising a PP base polymer and a particulate additive associated with the PP polymer. And a extractable material associated with the PP polymer, the method comprising dissolving the PP base polymer of the rAHP by contacting the rAHP with propane at a weight concentration of about 20% or less. . Another embodiment of the invention is a method of separating and purifying a PP polymer from rAHP, the PP polymer comprising a PP base polymer, a particulate additive associated with the PP polymer, and the PP polymer. The extractable material comprises a step of dissolving the PP base polymer in propane at a weight concentration of about 18% or less. In yet another embodiment of the invention, a method of separating and purifying a PP polymer from rAHP, the PP polymer comprising a PP base polymer, a particulate additive associated with the PP polymer, and the PP polymer. The method, including associated extractable materials, comprises dissolving the PP-based polymer in propane at a weight concentration of about 16% or less. In yet another embodiment of the present invention, a method of separating and purifying a PP polymer from rAHP, the PP polymer comprising a PP base polymer, a particulate additive associated with the PP polymer, and the PP polymer. And a extractable material related to ## STR3 ## comprises dissolving the PP base polymer in propane at a weight concentration of about 14% or less. In one embodiment of the present invention, a method for separating and purifying a PP polymer from a regenerated absorbent hygiene product (rAHP), the PP polymer comprising a PP base polymer and a particulate additive associated with the PP polymer. And a extractable material associated with the PP polymer, the method comprising dissolving the PP base polymer of the rAHP by contacting the rAHP with propane at a weight concentration of about 12% or less. .

  In one embodiment of the invention, the dissolution process solvent is selected from the group consisting of olefinic hydrocarbons, aliphatic hydrocarbons, and mixtures thereof. In another embodiment of the invention, the extraction solvent is the same as the dissolution process solvent.

  In one embodiment of the invention the dissolution step is in batch mode. In another embodiment of the invention, the lysing step is in continuous mode.

  In the dissolution process, an initial suspension is produced. The initial suspension comprises a suspension of particulate additives associated with the soluble polymer in the soluble base polymer solution and domains of all remaining polymer.

  In one embodiment of the invention, the domains of all the remaining polymers include cellulose and PAA polymers. In another embodiment of the invention, the domains of all of the remaining polymer are separated into the PAA polymer and the cellulosic polymer. One of the purposes of separating PAA and cellulose polymers is to reuse them in AHP in the future. In one embodiment of the invention, the PAA polymer separated from the dissolution step domain comprises a concentration of water in excess of 30 g water / g PAA polymer. In another embodiment of the present invention, the PAA polymer is further dehydrated via a dehydration process to less than 1 g water / g PAA polymer. A non-limiting example of a dehydration process is contacting a PAA polymer with a salt solution, an acidic solution, a basic solution, and a solvent that forms an azeotrope with water, pressurizing, and centrifuging. In yet another embodiment of the invention, the dehydration process comprises contacting the PAA polymer with a salt solution, an acidic solution, a basic solution, and a solvent that forms an azeotrope with water, pressurizing, centrifugation. And a combination of these. Non-limiting examples of solvents that form an azeotrope with water are methanol, ethanol, n-propanol, isopropyl alcohol, n-butanol, isobutanol, and 2-butanol. In still yet another embodiment of the present invention, the solvent is an alcohol selected from the group consisting of methanol, ethanol, n-propanol, isopropyl alcohol, n-butanol, isobutanol, 2-butanol, and mixtures thereof. is there.

In one embodiment of the invention, the dehydrated PAA polymer is used to produce new AHP. In another embodiment of the invention, the PAA polymer is subjected to depolymerization to produce monomeric acrylic acid (AA) or oligomeric acrylic acid (OAA). In yet another embodiment of the invention, the AA or OAA is further polymerized to a virgin PAA polymer and used to produce new AHP. Non-limiting examples of depolymerization of PAA polymers include depolymerization in the presence of dissolved CO ₂ , depolymerization using ultrasonic and solar radiation, thermal decomposition, and mechanochemistry (eg, depolymerization is achieved. For applying mechanical force).

  In one embodiment of the present invention, a method for separating and purifying ADH polymer from rP, wherein the dissolution step solvent is propane and the temperature range in the dissolution step begins at about 100 ° C. A method is provided wherein the pressure range begins at about 1,500 psig (10.3 MPa). In another embodiment of the present invention, a method of separating and purifying ADH polymer from rP, wherein the dissolution step solvent is n-butane and the temperature range in the dissolution step begins at about 100 ° C. A method is provided wherein the pressure range of interest in the process begins at about 900 psig (6.2 MPa). In yet another embodiment of the present invention, a method for separating and purifying ADH polymer from rP, wherein the dissolution step solvent is pentane and the temperature range in the dissolution step begins at about 100 ° C. A method is provided in which the pressure range at starts at about 500 psig (3.4 MPa). In yet another embodiment of the present invention, a method of separating and purifying ADH polymer from rP, wherein the dissolution step solvent is hexane and the temperature range in the dissolution step begins at about 100 ° C. A method is provided wherein the pressure range of interest in the process begins at about 150 psig (1 MPa).

  In one embodiment of the present invention, a method for separating and purifying a TPE polymer from rP, wherein the dissolution step solvent is propane and the temperature range in the dissolution step begins at about 100 ° C. A method is provided wherein the pressure range begins at about 3,000 psig (20.7 MPa). In another embodiment of the invention, a method of separating and purifying a TPE polymer from rP, wherein the dissolution step solvent is n-butane and the temperature range in the dissolution step begins at about 100 ° C. A method is provided wherein the pressure range of interest in the process begins at about 1200 psig (8.3 MPa). In yet another embodiment of the present invention, a method of separating and purifying a TPE polymer from rP, wherein the dissolution step solvent is pentane, wherein the temperature range in the dissolution step begins at about 100 ° C. A method is provided in which the pressure range at starts at about 700 psig (4.8 MPa). In yet another embodiment of the present invention, a method of separating and purifying a TPE polymer from rP, wherein the dissolution step solvent is hexane and the temperature range in the dissolution step begins at about 100 ° C. A method is provided in which the pressure range in the process begins at about 200 psig (1.4 MPa).

  In one embodiment of the present invention, a method for separating and purifying a PP polymer from rP, wherein the dissolution step solvent is propane and the temperature range in the dissolution step begins at about 100 ° C. A method is provided wherein the pressure range begins at about 7,000 psig (48.3 MPa). In another embodiment of the invention is a method of separating and purifying a PP polymer from rP, wherein the dissolution step solvent is n-butane and the temperature range in the dissolution step begins at about 100 ° C. A method is provided in which the pressure range of interest in the process begins at about 1800 psig (12.4 MPa). In yet another embodiment of the present invention, a method for separating and purifying a PP polymer from rP, wherein the dissolution step solvent is pentane and the temperature range in the dissolution step begins at about 100 ° C. A method is provided in which the pressure range at starts at about 1,400 psig (9.7 MPa). In yet another embodiment of the invention, a method of separating and purifying a PP polymer from rP, wherein the dissolution step solvent is hexane and the temperature range in the dissolution step begins at about 100 ° C. A method is provided wherein the pressure range of interest in the process begins at about 350 psig (2.4 MPa).

  In one embodiment of the present invention, a method for separating and purifying a PE polymer from rP, wherein the dissolution step solvent is propane and the temperature range in the dissolution step begins at about 100 ° C. A method is provided wherein the pressure range begins at about 10,000 psig (68.9 MPa). In another embodiment of the invention, a method of separating and purifying a PE polymer from rP, wherein the dissolution step solvent is n-butane and the temperature range in the dissolution step begins at about 100 ° C. A method is provided wherein the pressure range in the process begins at about 4,500 psig (31 MPa). In yet another embodiment of the invention, a method of separating and purifying a PE polymer from rP, wherein the dissolution step solvent is pentane and the temperature range in the dissolution step begins at about 100 ° C. A method is provided in which the pressure range at starts at about 2,900 psig (20 MPa). In yet another embodiment of the present invention, a method of separating and purifying a TPE polymer from rP, wherein the dissolution step solvent is hexane and the temperature range in the dissolution step begins at about 100 ° C. A method is provided in which the pressure range in the process begins at about 1,000 psig (6.9 MPa).

  In one embodiment of the present invention, a method of separating and purifying a PET polymer from rP, wherein the dissolution step solvent is propane and the temperature range in the dissolution step begins at about 100 ° C. A method is provided wherein the pressure range begins at about 34,000 psig (234.4 MPa). In another embodiment of the invention, a method of separating and purifying a PET polymer from rP, wherein the dissolution step solvent is n-butane and the temperature range in the dissolution step begins at about 100 ° C. A method is provided wherein the pressure range of interest in the process begins at about 15,000 psig (103.4 MPa). In yet another embodiment of the present invention, a method for separating and purifying a PET polymer from rP, wherein the dissolution step solvent is pentane and the temperature range in the dissolution step begins at about 100 ° C. A method is provided in which the pressure range at starts at about 10,000 psig (68.9 MPa). In yet another embodiment of the present invention, a method for separating and purifying a PET polymer from rP, wherein the dissolution step solvent is hexane and the temperature range in the dissolution step begins at about 100 ° C. A method is provided wherein the pressure range in the process begins at about 3,500 psig (24.1 MPa).

Sedimentation Step In one embodiment of the present invention, a method of separating and purifying a polymer from a regenerated product (rP) provides a collection of sedimented particulate additive and domains of the remaining polymer, as well as an intermediate suspension. Sedimenting the initial suspension in a temperature range and pressure range sufficient to provide the precipitated particulate additive collection to a particulate additive associated with the first soluble polymer. And the intermediate suspension comprises a suspension of unprecipitated particulate additive associated with the first soluble polymer in the first soluble base polymer solution. . In another embodiment of the invention, a method of separating and purifying a polymer from a regenerated absorbent hygiene product (rAHP) comprises a collection of precipitated particulate additives and domains of all of the remaining polymer, and an intermediate suspension. Sedimenting the initial suspension in a temperature and pressure range sufficient to produce a liquid, wherein the settled collection of particulate additives comprises particles associated with the first soluble polymer. A particulate additive, the intermediate suspension comprising a suspension of unprecipitated particulate additive associated with the first soluble polymer in the first soluble base polymer solution. ,including. In yet another embodiment of the present invention, a method of separating and purifying a polymer from reclaimed film (rF) provides a collection of precipitated particulate additive and domains of all the remaining polymer, as well as an intermediate suspension. Sedimenting the initial suspension in a temperature range and pressure range sufficient to provide the precipitated particulate additive collection to a particulate additive associated with the first soluble polymer. And the intermediate suspension comprises a suspension of unprecipitated particulate additive associated with the first soluble polymer in the first soluble base polymer solution. . In yet another embodiment of the present invention, a method of separating and purifying ADH polymer from regenerated absorbent hygiene products (rAHP) comprises a collection of precipitated particulate additives and TPE, PP, PE, PET, cellulose. , And the domain of PAA polymer, and the step of settling the initial suspension at a temperature range and pressure range sufficient to produce an intermediate suspension, wherein the collection of settled particulate additive is , Including a particulate additive associated with the ADH polymer, the intermediate suspension comprising a suspension of non-precipitated particulate additive associated with the ADH polymer in the ADH base polymer solution. ,including. In one embodiment of the present invention, a method of separating and purifying PP polymer from regenerated absorbent hygiene product (rAHP) comprises a collection of precipitated particulate additives and domains of cellulose and PAA polymer, and intermediate suspensions. Sedimenting the initial suspension in a temperature range and pressure range sufficient to produce a liquid, wherein the collected settled particulate additive collects particulate additive associated with the PP polymer. And the intermediate suspension comprises a suspension of the unprecipitated particulate additive associated with the PP polymer in the PP base polymer solution.

The settling step subject the undissolved particulate additive associated with the polymer and the particulate matter associated with the impurities to a force that causes the additive and the agent to move uniformly in the direction of force. Typically, the applied settling force is gravity, but may be centrifugal force, centripetal force, or some other force. The amount of force applied and the duration of the settling time are determined by the particle size and particle density of the particulate additive and particulate matter, and the density and viscosity of the base polymer solution (i.e., the solution of the base polymer dissolved in the dissolution step solvent). ), But not limited thereto, depending on some parameters. Equation 2 below is the relationship between the above parameters and the sedimentation velocity, which is a measure of the sedimentation velocity:
V = (ρ _p −ρ _f ) gd ² / 18η Equation 2
Where V is the sedimentation velocity, ρ _p is the density of the particulate additive and material, ρ _f is the density of the base polymer solution, and g is the applied force (typically gravity). Acceleration, d is the diameter of the particles in the particulate additive and material, and η is the dynamic viscosity of the base polymer solution). Some of the important parameters that determine solution viscosity are the chemical composition of the base polymer solution, the molecular weight and concentration of the base polymer dissolved in the base polymer solution, and the temperature and pressure of the base polymer solution.

  In one embodiment of the invention, the method of separating and purifying PP polymer from rAHP includes n-butane as the dissolution process solvent and the temperature range in the precipitation process is from about 90 ° C to about 220 ° C. In another embodiment of the invention, the method of separating and purifying PP polymer from rAHP comprises n-butane as the dissolution process solvent and the temperature range in the precipitation process is from about 100 ° C to about 200 ° C. In yet another embodiment of the invention, the method of separating and purifying PP polymer from rAHP includes n-butane as the dissolution process solvent and the temperature range in the precipitation process is from about 130 ° C to about 180 ° C.

  In one embodiment of the invention, the method of separating and purifying PP polymer from rAHP includes n-butane as the dissolution process solvent and the pressure range in the precipitation process is from about 350 psig (2.4 MPa) to about 4,000 psig (27 MPa). .6 MPa). In another embodiment of the present invention, a method of separating and purifying PP polymer from rAHP comprises n-butane as the dissolution process solvent and the pressure range in the precipitation process is from about 1,000 psig (6.9 MPa) to about 3, It is 500 psig (24.1 MPa). In yet another embodiment of the present invention, a method of separating and purifying PP polymer from rAHP includes n-butane as a dissolution process solvent and the pressure range in the precipitation process is from about 2,000 psig (13.8 MPa) to about 3 MPa. 1,000 psig (20.7 MPa).

  In yet another embodiment of the present invention, a method for separating and purifying PP polymer from rAHP, wherein the temperature range in the precipitation step is from about 90 ° C to about 220 ° C, and the pressure range in the precipitation step is. Is provided from about 350 psig (2.4 MPa) to about 20,000 psig (137.9 MPa).

  In one embodiment of the present invention, a method for separating and purifying PP polymer from rAHP comprises n-butane as a dissolution step solvent, wherein the weight concentration of the PP base polymer in the PP base polymer solution in the precipitation step is at least. It is about 0.5%. In another embodiment of the present invention, a method for separating and purifying PP polymer from rAHP comprises n-butane as a dissolution step solvent, wherein the weight concentration of the PP base polymer in the PP base polymer solution in the precipitation step is At least about 1%. In yet another embodiment of the present invention, a method for separating and purifying a PP polymer from rAHP comprises n-butane as a dissolution step solvent and the weight concentration of the PP base polymer in the PP base polymer solution in the precipitation step. Is at least about 2%. In yet another embodiment of the present invention, a method of separating and purifying PP polymer from rAHP comprises n-butane as a dissolution step solvent, wherein the weight of the PP base polymer in the PP base polymer solution in the precipitation step. The concentration is at least about 3%. In one embodiment of the present invention, a method for separating and purifying PP polymer from rAHP comprises n-butane as a dissolution step solvent, wherein the weight concentration of the PP base polymer in the PP base polymer solution in the precipitation step is at least. It is about 4%. In another embodiment of the present invention, a method for separating and purifying PP polymer from rAHP comprises n-butane as a dissolution step solvent, wherein the weight concentration of the PP base polymer in the PP base polymer solution in the precipitation step is At least about 5%.

  In one embodiment of the present invention, a method for separating and purifying PP polymer from rAHP comprises n-butane as a dissolution step solvent, and the weight concentration of the PP base polymer in the PP base polymer solution in the precipitation step is about. It is 20% or less. In another embodiment of the present invention, a method for separating and purifying PP polymer from rAHP comprises n-butane as a dissolution step solvent, wherein the weight concentration of the PP base polymer in the PP base polymer solution in the precipitation step is It is about 18% or less. In yet another embodiment of the present invention, a method for separating and purifying a PP polymer from rAHP comprises n-butane as a dissolution step solvent, wherein the weight concentration of the PP base polymer in the PP base polymer solution in the precipitation step. Is about 16% or less. In yet another embodiment of the present invention, a method of separating and purifying PP polymer from rAHP comprises n-butane as a dissolution step solvent, wherein the weight of the PP base polymer in the PP base polymer solution in the precipitation step. The concentration is about 14% or less. In one embodiment of the present invention, a method for separating and purifying PP polymer from rAHP comprises n-butane as a dissolution step solvent, and the weight concentration of the PP base polymer in the PP base polymer solution in the precipitation step is about. It is 12% or less.

  In one embodiment of the invention, the method of separating and purifying PP polymer from rAHP includes propane as the dissolution process solvent and the temperature range in the precipitation process is from about 90 ° C to about 220 ° C. In another embodiment of the invention, the method of separating and purifying PP polymer from rAHP includes propane as the dissolution process solvent and the temperature range in the precipitation process is from about 100 ° C to about 200 ° C. In yet another embodiment of the present invention, the method of separating and purifying PP polymer from rAHP comprises propane as the dissolution process solvent and the temperature range in the precipitation process is from about 130 ° C to about 180 ° C.

  In one embodiment of the invention, the method of separating and purifying PP polymer from rAHP includes propane as the dissolution process solvent and the pressure range in the precipitation process is from about 2,000 psig (13.8 MPa) to about 8,000 psig (55). 0.2 MPa). In another embodiment of the invention, the method of separating and purifying PP polymer from rAHP includes propane as the dissolution process solvent and the pressure range in the precipitation process is from about 3,000 psig (20.7 MPa) to about 6,000 psig ( 41.4 MPa). In yet another embodiment of the present invention, a method of separating and purifying PP polymer from rAHP comprises propane as the dissolution process solvent and the pressure range in the precipitation process is from about 3,500 psig (24.1 MPa) to about 5,000 psig. (34.5 MPa).

  In one embodiment of the invention, the method of separating and purifying PP polymer from rAHP comprises propane as the dissolution step solvent and the weight concentration of the PP base polymer in the PP base polymer solution in the precipitation step is at least about 0. It is 0.5%. In another embodiment of the present invention, a method for separating and purifying PP polymer from rAHP comprises propane as a dissolution step solvent, and the weight concentration of the PP base polymer in the PP base polymer solution in the precipitation step is at least about. 1%. In yet another embodiment of the present invention, a method of separating and purifying PP polymer from rAHP comprises propane as a dissolution step solvent, wherein the weight concentration of the PP base polymer in the PP base polymer solution in the precipitation step is at least. It is about 2%. In yet another embodiment of the present invention, a method of separating and purifying PP polymer from rAHP comprises propane as a dissolution step solvent, wherein the weight concentration of the PP base polymer in the PP base polymer solution in the precipitation step is At least about 3%. In one embodiment of the invention, the method for separating and purifying PP polymer from rAHP comprises propane as the dissolution step solvent and the weight concentration of the PP base polymer in the PP base polymer solution in the precipitation step is at least about 4%. %. In another embodiment of the present invention, a method for separating and purifying PP polymer from rAHP comprises propane as a dissolution step solvent, and the weight concentration of the PP base polymer in the PP base polymer solution in the precipitation step is at least about. 5%.

  In one embodiment of the present invention, a method of separating and purifying PP polymer from rAHP comprises propane as a dissolution step solvent and the PP base polymer solution has a weight concentration of about 20% in the PP base polymer solution in the precipitation step. It is the following. In another embodiment of the present invention, a method for separating and purifying PP polymer from rAHP comprises propane as a dissolution step solvent and the PP base polymer solution has a weight concentration of about 18 in the PP base polymer solution in the precipitation step. % Or less. In yet another embodiment of the present invention, a method for separating and purifying PP polymer from rAHP comprises propane as a dissolution step solvent, and the weight concentration of the PP base polymer in the PP base polymer solution in the precipitation step is about. It is 16% or less. In yet another embodiment of the present invention, a method for separating and purifying PP polymer from rAHP comprises propane as a dissolution step solvent, wherein the weight concentration of the PP base polymer in the PP base polymer solution in the precipitation step is It is about 14% or less. In one embodiment of the invention, the method for separating and purifying PP polymer from rAHP comprises propane as the dissolution process solvent and the PP base polymer solution in the precipitation step has a weight concentration of about 12% of the PP base polymer. It is the following.

  In one embodiment of the invention, the settling process is in batch mode.

  The settling process produces a collection of settled particulate additive and all remaining polymer domains, as well as an intermediate suspension, which lasts for the settling time. The collection of settled particulate additives comprises particulate additives associated with the soluble polymer, and the intermediate suspension comprises unprecipitated particulate additives associated with the soluble polymer in the soluble base polymer solution. Including a suspension of the agent. In one embodiment of the invention, the precipitated collection of particulate additives comprises particulate additives associated with the soluble polymer and particulates associated with the impurities. In another embodiment of the invention, the intermediate suspension comprises a suspension of unprecipitated particulate additive associated with the soluble polymer in a soluble base polymer solution and a suspension associated with the impurities. Not include particulate matter.

  In one embodiment of the invention, the settled collection of particulate additives comprises particles having a diameter greater than about 1 mm. In another embodiment of the invention, the settled particulate additive collection comprises particles having a diameter greater than about 0.75 mm. In yet another embodiment of the present invention, the settled particulate additive collection comprises particles having a diameter greater than about 0.5 mm. In yet another embodiment of the present invention, the collection of precipitated particulate additives comprises particles having a diameter greater than about 300 μm. In one embodiment of the invention, the settled collection of particulate additives comprises particles having a diameter greater than about 100 μm. In another embodiment of the invention, the collection of precipitated particulate additives comprises particles having a diameter greater than about 50 μm. In yet another embodiment of the invention, the settled particulate additive collection comprises particles having a diameter greater than about 20 μm.

  In one embodiment of the invention, the settling time is greater than about 24 hours. In another embodiment of the invention, the precipitation time is greater than about 12 hours. In yet another embodiment of the invention, the settling time is greater than about 6 hours. In yet another embodiment of the invention, the precipitation time is greater than about 3 hours. In one embodiment of the invention, the settling time is greater than about 1 hour. In yet another embodiment of the invention, the settling time is greater than about 0.5 hours.

  In one embodiment of the invention, the precipitation time is about 24 hours to 0.1 hours. In another embodiment of the invention, the precipitation time is about 18 hours to about 0.25 hours. In yet another embodiment of the invention, the precipitation time is about 12 hours to about 0.5 hours. In yet another embodiment of the present invention, the settling time is from about 12 hours to about 1 hour. In one embodiment of the invention, the precipitation time is about 6 hours to about 2 hours. In yet another embodiment of the invention, the precipitation time is about 4 hours.

  In one embodiment of the invention, the density of particulate additive and particulate matter is greater than about 9 g / mL. In another embodiment of the invention, the density of particulate additive and particulate matter is about 1 g / mL to about 9 g / mL. In yet another embodiment of the invention, the density of particulate additive and particulate matter is from about 1 g / mL to about 4 g / mL. In yet another embodiment of the present invention, the density of particulate additive and particulate matter is about 2 g / mL to about 3.5 g / mL.

  In one embodiment of the invention, the density of base polymer solution is greater than about 0.8 g / mL. In another embodiment of the invention, the density of the base polymer solution is about 0.8 g / mL to about 3 g / mL. In yet another embodiment of the present invention, the density of the base polymer solution is about 0.9 g / mL to about 2 g / mL. In yet another embodiment of the present invention, the density of the base polymer solution is about 1 g / mL to about 1.5 g / mL.

  In one embodiment of the invention, the dynamic viscosity of the base polymer solution is higher than about 0.5 mPa · s. In another embodiment of the invention, the dynamic viscosity of the base polymer solution is about 0.6 mPa · s to about 100 mPa · s. In yet another embodiment of the present invention, the base polymer solution has a dynamic viscosity of from about 1 mPa · s to about 20 mPa · s. In yet another embodiment of the present invention, the dynamic viscosity of the base polymer solution is about 2 mPa · s to about 10 mPa · s.

Purification Step In one embodiment of the present invention, a method of separating and purifying a polymer from a recycled product (rP) comprises using a solid medium in a temperature range and pressure range sufficient to produce a final suspension. A step of purifying a suspension, wherein a portion of the particulate additive associated with the first soluble polymer is retained by the solid medium and the final suspension is the first soluble base polymer. Comprising a suspension of unretained particulate additive associated with the first soluble polymer in solution. In another embodiment of the invention, a method of separating and purifying a polymer from regenerated absorbent hygiene product (rAHP) uses a solid medium in a temperature range and pressure range sufficient to produce a final suspension. A step of purifying the intermediate suspension, wherein a portion of the particulate additive associated with the first soluble polymer is retained by the solid medium and the final suspension is the first dissolved polymer. Comprising a suspension of unretained particulate additive associated with the first soluble polymer in a soluble base polymer solution. In yet another embodiment of the present invention, a method of separating and purifying a polymer from reclaimed film (rF) comprises using a solid medium in a temperature range and pressure range sufficient to produce a final suspension. A step of purifying a suspension, wherein a portion of the particulate additive associated with the first soluble polymer is retained by the solid medium and the final suspension is the first soluble base polymer. Comprising a suspension of unretained particulate additive associated with the first soluble polymer in solution. In yet another embodiment of the present invention, a method of separating and purifying ADH polymer from regenerated absorbent hygiene product (rAHP) comprises the solids in a temperature range and pressure range sufficient to produce a final suspension. Purifying the intermediate suspension with a medium, wherein a portion of the particulate additive associated with the ADH polymer is retained by the solid medium, and the final suspension is the ADH base polymer solution. Comprising a suspension of unretained particulate additive associated with the ADH polymer therein. In one embodiment of the invention, a method for separating and purifying PP polymer from regenerated absorbent hygiene product (rAHP) uses the solid medium in a temperature range and pressure range sufficient to produce a final suspension. Purifying the intermediate suspension with a portion of the particulate additive associated with the PP polymer retained by the solid medium, and the final suspension of the particulate suspension in the PP base polymer solution. A process comprising a suspension of unretained particulate additive associated with the PP polymer.

  The solid medium of the present invention is any solid material that retains that portion of the particulate additive from the final suspension. The solid medium can also retain a portion of the particulate matter associated with the impurities and a portion of the extractable material in the rP that was not removed in the extraction process.

  Without wishing to be bound by theory, Applicants believe that the solid medium removes the particulate additive and particulate matter by various mechanisms. Non-limiting examples of possible mechanisms include adsorption, absorption, size exclusion, ion exclusion, ion exchange, and other mechanisms that may be apparent to those of ordinary skill in the art. In addition, pigments and other materials commonly found in recycled products may be polar compounds and may preferentially interact with solid media, which may also be at least slightly polar. Polar-polar interactions are particularly preferred when a non-polar solvent such as an alkane is used as the dissolution process solvent.

  In one embodiment of the invention, the solid medium is selected from the group consisting of inorganic materials, carbonaceous materials, and mixtures thereof. Non-limiting examples of inorganic materials include silicon oxide (silica), silica gel, aluminum oxide (alumina), iron oxide, aluminum silicate, magnesium silicate, amorphous volcanic glass, recycled glass, sand, quartz, diatomaceous earth, Zeolite, perlite, clay, fuller's earth, bentonite clay, metal organic structure (MOF), covalent organic structure (COF), and zeolite imidazolate structure (ZIF). Non-limiting examples of carbonaceous materials are anthracite, carbon black, coke, and activated carbon. In one embodiment of the present invention, the inorganic substance is silicon oxide (silica), silica gel, aluminum oxide (alumina), iron oxide, aluminum silicate, magnesium silicate, amorphous volcanic glass, recycled glass, sand, quartz. , Diatomaceous earth, zeolite, perlite, clay, fuller's earth, bentonite clay, metal organic structure (MOF), covalent organic structure (COF), zeolite imidazolate structure (ZIF), and mixtures thereof. To be selected. In another embodiment of the present invention, the inorganic substance is silicon oxide (silica), silica gel, aluminum oxide (alumina), amorphous volcanic glass, recycled glass, sand, quartz, diatomaceous earth, zeolite, clay, fuller's earth, It is selected from the group consisting of bentonite clay and mixtures thereof. In yet another embodiment of the present invention, the carbonaceous material is selected from the group consisting of anthracite, carbon black, coke, activated carbon, and mixtures thereof. In yet another embodiment of the present invention, the solid medium is recycled glass.

  In one embodiment of the invention, the solid medium is contacted with the intermediate suspension in a container for a specified time while stirring the solid medium. In another embodiment of the invention, the solid medium is removed from the final suspension via a solid-liquid separation step. Non-limiting examples of solid-liquid separation steps include filtration, decantation, centrifugation, and sedimentation. In yet another embodiment of the invention, the intermediate suspension is passed through a stationary bed of solid medium. In yet another embodiment of the present invention, the solid medium is arranged in a fixed bed configuration. This fixed bed configuration includes axial filters, radial filters, or a combination of both. In one embodiment of the invention, the fixed bed configuration comprises at least two fixed beds connected in series. In another embodiment of the invention, the fixed bed height or length of the solid medium is greater than about 5 cm. In yet another embodiment of the present invention, the fixed bed height or length of the solid medium is greater than about 10 cm. In yet another embodiment of the present invention, the fixed bed height or length of the solid medium is greater than about 20 cm. In one embodiment of the invention, the fixed bed diameter of the solid medium is greater than about 1 cm. In another embodiment of the invention, the fixed bed of the solid medium has a diameter of greater than about 2 cm. In yet another embodiment of the invention, the fixed bed of solid medium has a diameter of greater than about 5 cm. In one embodiment of the invention, the ratio of the length of the solid medium to the diameter of the fixed bed is greater than about 1. In another embodiment of the invention, the ratio of the length of the solid medium to the diameter of the fixed bed is greater than about 5. In yet another embodiment of the invention, the ratio of the length of the solid medium to the diameter of the fixed bed is greater than about 10. In yet another embodiment of the invention, the ratio of the length of the fixed bed to the diameter of the solid medium is greater than about 20.

As used herein, the term "solid medium median particle size" refers to the diameter of a solid medium below or above which 50% of the total volume of particles resides _{, and as Dv, 0.50} . It is written. Further, the term "solid media particle span" is a statistical representation of a given solid media particle sample and can be calculated as follows. First, the median particle size is calculated as described above. Then, by the same method, a particle diameter D _{v, 0.10} of the solid medium for separating the particle sample at a volume fraction of 10% is determined, and then a particle diameter D _{v, 0} for separating the particle sample at a volume fraction of 90%. _Ask for _.90 . The solid medium particle span is then equal to ( _{Dv, 0.90-} Dv _{, 0.10} ) _/Dv,0.50 . In one embodiment of the invention, the solid media particle span is less than about 2. In another embodiment of the invention, the solid media particle span is less than about 1.5. In yet another embodiment of the invention, the solid media particle span is less than about 1.5. In still yet another embodiment of the present invention, the solid media particle span is less than about 1.3. In one embodiment of the invention, the solid media particle span is from about 1.1 to about 2. In another embodiment of the invention, the solid medium particle span is about 1.3 to about 1.5.

  In one embodiment of the invention, the solid medium is replaced as needed to maintain the desired composition of the final suspension. In another embodiment of the invention, the solid medium is regenerated and reused in the purification process. In yet another embodiment of the present invention, the solid medium is regenerated by fluidizing the solid medium during the rewashing step.

  In one embodiment of the invention, the purification process is in continuous mode. In another embodiment of the invention, the purification process is in batch mode.

  In one embodiment of the invention, the method of separating and purifying PP polymer from rAHP includes n-butane as the dissolution process solvent and the temperature range in the purification process is from about 90 ° C to about 220 ° C. In another embodiment of the invention, the method of separating and purifying PP polymer from rAHP includes n-butane as the dissolution step solvent and the temperature range in the purification step is from about 100 ° C to about 200 ° C. In yet another embodiment of the present invention, the method for separating and purifying PP polymer from rAHP includes n-butane as the dissolution step solvent and the temperature range in the purification step is about 130 ° C to about 180 ° C.

  In one embodiment of the present invention, the method of separating and purifying PP polymer from rAHP includes n-butane as the dissolution process solvent and the pressure range in the purification process is from about 350 psig (2.4 MPa) to about 4,000 (27). .6 MPa). In another embodiment of the present invention, a method of separating and purifying PP polymer from rAHP comprises n-butane as the dissolution process solvent and the pressure range in the purification process is from about 1,000 psig (6.9 MPa) to about 3, It is 500 (24.1 MPa). In yet another embodiment of the present invention, a method for separating and purifying PP polymer from rAHP comprises n-butane as a dissolution step solvent and the pressure range in the purification step is from about 2,000 psig (13.8 MPa) to about 3, 000 (20.7 MPa).

  In one embodiment of the invention, a method of separating and purifying PP polymer from rAHP is provided, wherein the temperature range in the purification step is from about 90 ° C to about 220 ° C, and the pressure range in the purification step is about 350 psig. (2.4 MPa) to about 20,000 psig (137.9 MPa).

  In one embodiment of the present invention, a method for separating and purifying a PP polymer from rAHP comprises n-butane as a dissolution step solvent, the weight concentration of the PP base polymer in the PP base polymer solution in the intermediate suspension. Is at least about 0.5%. In another embodiment of the invention, a method of separating and purifying a PP polymer from rAHP comprises n-butane as a dissolution step solvent, wherein the weight of the PP base polymer in the PP base polymer solution in the intermediate suspension. The concentration is at least about 1%. In yet another embodiment of the present invention, a method for separating and purifying a PP polymer from rAHP comprises n-butane as a dissolution step solvent, wherein the PP base polymer in the PP base polymer solution in the intermediate suspension is The weight concentration is at least about 2%. In yet another embodiment of the present invention, a method for separating and purifying PP polymer from rAHP comprises n-butane as a dissolution step solvent, wherein the PP base polymer in the PP base polymer solution in the intermediate suspension is used. Has a weight concentration of at least about 3%. In one embodiment of the present invention, a method for separating and purifying a PP polymer from rAHP comprises n-butane as a dissolution step solvent, the weight concentration of the PP base polymer in the PP base polymer solution in the intermediate suspension. Is at least about 4%. In another embodiment of the invention, a method of separating and purifying a PP polymer from rAHP comprises n-butane as a dissolution step solvent, wherein the weight of the PP base polymer in the PP base polymer solution in the intermediate suspension. The concentration is at least about 5%.

  In one embodiment of the present invention, a method for separating and purifying a PP polymer from rAHP comprises n-butane as a dissolution step solvent, the weight concentration of the PP base polymer in the PP base polymer solution in the intermediate suspension. Is about 20% or less. In another embodiment of the invention, a method of separating and purifying a PP polymer from rAHP comprises n-butane as a dissolution step solvent, wherein the weight of the PP base polymer in the PP base polymer solution in the intermediate suspension. The concentration is about 18% or less. In yet another embodiment of the present invention, a method for separating and purifying a PP polymer from rAHP comprises n-butane as a dissolution step solvent, wherein the PP base polymer in the PP base polymer solution in the intermediate suspension is The weight concentration is about 16% or less. In yet another embodiment of the present invention, a method for separating and purifying PP polymer from rAHP comprises n-butane as a dissolution step solvent, wherein the PP base polymer in the PP base polymer solution in the intermediate suspension is used. Has a weight concentration of about 14% or less. In one embodiment of the present invention, a method for separating and purifying a PP polymer from rAHP comprises n-butane as a dissolution step solvent, the weight concentration of the PP base polymer in the PP base polymer solution in the intermediate suspension. Is about 12% or less.

  In one embodiment of the invention, the method of separating and purifying PP polymer from rAHP includes propane as the dissolution process solvent and the temperature range in the purification process is from about 90 ° C to about 220 ° C. In another embodiment of the invention, the method of separating and purifying PP polymer from rAHP includes propane as the dissolution process solvent and the temperature range in the purification process is from about 100 ° C to about 200 ° C. In yet another embodiment of the present invention, the method for separating and purifying PP polymer from rAHP includes propane as the dissolution process solvent and the temperature range in the purification process is from about 130 ° C to about 180 ° C.

  In one embodiment of the invention, the method of separating and purifying PP polymer from rAHP includes propane as the dissolution process solvent and the pressure range in the purification process is from about 2,000 psig (13.8 MPa) to about 8,000 (55). 0.2 MPa). In another embodiment of the present invention, a method of separating and purifying PP polymer from rAHP includes propane as a dissolution process solvent and the pressure range in the purification process is from about 3,000 psig (20.7 MPa) to about 6,000 ( 41.4 MPa). In yet another embodiment of the present invention, a method for separating and purifying PP polymer from rAHP comprises propane as the dissolution process solvent and the pressure range in the purification process is from about 3,500 psig (24.1 MPa) to about 5,000. (34.5 MPa).

  In one embodiment of the present invention, a method of separating and purifying PP polymer from rAHP comprises propane as a dissolution step solvent, wherein the weight concentration of the PP base polymer in the PP base polymer solution in the intermediate suspension is at least. It is about 0.5%. In another embodiment of the present invention, a method for separating and purifying PP polymer from rAHP comprises propane as a dissolution step solvent, wherein the weight concentration of the PP base polymer in the PP base polymer solution in the intermediate suspension is At least about 1%. In yet another embodiment of the present invention, a method for separating and purifying PP polymer from rAHP comprises propane as a dissolution step solvent, wherein the PP base polymer in the intermediate suspension has a weight concentration of the PP base polymer in the PP base polymer solution. Is at least about 2%. In yet another embodiment of the present invention, a method for separating and purifying PP polymer from rAHP comprises propane as a dissolution step solvent, wherein the weight of the PP base polymer in the PP base polymer solution in the intermediate suspension. The concentration is at least about 3%. In one embodiment of the present invention, a method of separating and purifying PP polymer from rAHP comprises propane as a dissolution step solvent, wherein the weight concentration of the PP base polymer in the PP base polymer solution in the intermediate suspension is at least. It is about 4%. In another embodiment of the present invention, a method for separating and purifying PP polymer from rAHP comprises propane as a dissolution step solvent, wherein the weight concentration of the PP base polymer in the PP base polymer solution in the intermediate suspension is At least about 5%.

  In one embodiment of the present invention, a method of separating and purifying PP polymer from rAHP comprises propane as a dissolution step solvent and the weight concentration of the PP base polymer in the PP base polymer solution in the intermediate suspension is about. It is 20% or less. In another embodiment of the present invention, a method for separating and purifying PP polymer from rAHP comprises propane as a dissolution step solvent, wherein the weight concentration of the PP base polymer in the PP base polymer solution in the intermediate suspension is It is about 18% or less. In yet another embodiment of the present invention, a method for separating and purifying PP polymer from rAHP comprises propane as a dissolution step solvent, wherein the PP base polymer in the intermediate suspension has a weight concentration of the PP base polymer in the PP base polymer solution. Is about 16% or less. In yet another embodiment of the present invention, a method for separating and purifying PP polymer from rAHP comprises propane as a dissolution step solvent, wherein the weight of the PP base polymer in the PP base polymer solution in the intermediate suspension. The concentration is about 14% or less. In one embodiment of the present invention, a method of separating and purifying PP polymer from rAHP comprises propane as a dissolution step solvent and the weight concentration of the PP base polymer in the PP base polymer solution in the intermediate suspension is about. It is 12% or less.

Separation Step In one embodiment of the present invention, a method of separating and purifying a polymer from recycled product (rP) is performed at a temperature range and pressure range sufficient to produce a separated and purified first soluble polymer. Dissolving step A step of separating a solvent from the final suspension, wherein the separated and purified first soluble polymer is the first soluble base polymer and the first soluble polymer in the rP. Dissolved in the separated and purified first soluble polymer at a concentration lower than the concentration of the particulate additive associated with the first soluble polymer in the soluble polymer. With the particulate additive associated with the active polymer. In another embodiment of the invention, a method of separating and purifying a polymer from a regenerated absorbent hygiene product (rAHP) comprises a temperature range and pressure sufficient to produce a separated and purified first soluble polymer. A step of separating the dissolution step solvent from the final suspension, wherein the separated and purified first soluble polymer comprises the first soluble base polymer and the first soluble base polymer in the rAHP. A first soluble polymer dispersed in the separated and purified first soluble polymer at a concentration lower than the concentration of the particulate additive associated with the first soluble polymer in the first soluble polymer. And the particulate additive associated with one soluble polymer. In yet another embodiment of the present invention, a method of separating and purifying a polymer from recycled film (rF) comprises applying a temperature and pressure range sufficient to produce a separated and purified first soluble polymer. Dissolving step A step of separating the solvent from the final suspension, wherein the separated and purified first soluble polymer is the first soluble base polymer and the first soluble polymer in the rF. Dissolved in the separated and purified first soluble polymer at a concentration lower than the concentration of the particulate additive associated with the first soluble polymer in the soluble polymer. With the particulate additive associated with the active polymer. In yet another embodiment of the present invention, a method of separating and purifying ADH polymer from regenerated absorbent hygiene product (rAHP) comprises a temperature range and pressure range sufficient to produce separated and purified ADH polymer. A step of separating the dissolution step solvent from the final suspension, wherein the separated and purified ADH polymer is associated with the ADH base polymer and the ADH polymer in the ADH polymer in the rAHP. And the particulate additive associated with the ADH polymer dispersed in the separated and purified ADH polymer at a concentration lower than the concentration of the particulate additive. In one embodiment of the present invention, a method of separating and purifying PP polymer from regenerated absorbent hygiene product (rAHP) comprises dissolving the PP polymer in a temperature range and pressure range sufficient to produce the separated and purified PP polymer. Separating a process solvent from the final suspension, wherein the separated and purified PP polymer is associated with the first PP base polymer and the PP polymer in the PP polymer in the rAHP. Comprising the particulate additive associated with the PP polymer dispersed in the separated and purified PP polymer at a concentration lower than the concentration of the particulate additive.

  In one embodiment of the invention, the separating step is performed at a temperature and pressure at which the polymer precipitates from the solution and is no longer dissolved in the dissolving step solvent. In another embodiment of the invention, the separating step is accomplished by reducing the pressure at a fixed temperature. In yet another embodiment of the invention, the separating step is accomplished by reducing the temperature at a fixed pressure. In yet another embodiment of the present invention, the separating step is accomplished by raising the temperature at a fixed pressure. In one embodiment of the invention, the separating step is accomplished by reducing both temperature and pressure. The dissolution process solvent can be partially or completely converted from the liquid to the vapor phase by controlling the temperature and pressure.

  In another embodiment of the invention, by controlling the temperature and pressure of the dissolution process solvent during the separation process, the precipitated polymer is removed from the dissolution process solvent without completely converting the dissolution process solvent to 100% vapor phase. To be separated. Separation of the precipitated polymer is accomplished by any method of liquid-liquid or liquid-solid separation. Non-limiting examples of liquid-liquid or liquid-solid separations include filtration, decantation, centrifugation, and sedimentation.

  In one embodiment of the invention, the method of separating and purifying PP polymer from rAHP includes n-butane as the dissolution process solvent and the temperature range in the separation process is from about 0 ° C to about 220 ° C. In another embodiment of the invention, the method of separating and purifying PP polymer from rAHP includes n-butane as the dissolution process solvent and the temperature range in the separation process is from about 100 ° C to about 220 ° C. In yet another embodiment of the present invention, the method for separating and purifying PP polymer from rAHP includes n-butane as the dissolution process solvent and the temperature range in the separation process is from about 130 ° C to about 180 ° C.

  In one embodiment of the present invention, a method of separating and purifying a PP polymer from rAHP includes n-butane as a dissolution process solvent and the pressure range in the separation process is from about 0 psig (0 MPa) to about 2,000 psig (13.8 MPa). ). In another embodiment of the present invention, a method of separating and purifying PP polymer from rAHP includes n-butane as a dissolution process solvent and the pressure range in the separation process is from about 50 (0.34 MPa) to about 1,500 psig ( 10.3 MPa). In yet another embodiment of the present invention, a method for separating and purifying PP polymer from rAHP includes n-butane as a dissolution process solvent and the pressure range in the separation process is from about 75 psig (0.52 MPa) to about 1,000 psig. (6.9 MPa).

  In one embodiment of the invention, the method of separating and purifying PP polymer from rAHP includes propane as the dissolution process solvent and the temperature range in the separation process is from about -42 ° C to about 220 ° C. In another embodiment of the invention, the method of separating and purifying PP polymer from rAHP includes propane as the dissolution process solvent and the temperature range in the separation process is from about 0 ° C to about 150 ° C. In yet another embodiment of the invention, the method of separating and purifying PP polymer from rAHP comprises propane as the dissolution process solvent and the temperature range in the separation process is from about 50 ° C to about 130 ° C.

  In one embodiment of the present invention, a method of separating and purifying PP polymer from rAHP includes propane as a dissolution process solvent and the pressure range in the separation process is from about 0 psig (0 MPa) to about 6,000 psig (41.4 MPa). is there. In another embodiment of the present invention, a method of separating and purifying PP polymer from rAHP includes propane as the dissolution process solvent and the pressure range in the separation process is from about 50 (0.34 MPa) to about 3,000 psig (20. 7 MPa). In yet another embodiment of the invention, the method of separating and purifying PP polymer from rAHP comprises propane as the dissolution process solvent and the pressure range in the separation process is from about 75 psig (0.52 MPa) to about 1,000 psig (6). 1.9 MPa).

  In one embodiment of the present invention, a method for separating and purifying a PP polymer from rAHP, wherein the temperature range in the separation step is about 0 ° C to about 220 ° C and the pressure range is about 0 psig (0 MPa) to. A method is provided that is about 2,000 psig (13.8 MPa).

  In one embodiment of the invention, the separated and purified polymer produced from the separation step is lower than the concentration of particulate additive associated with the base polymer and the polymer dispersed in the base polymer in rP. A particulate additive associated with the polymer dispersed in the polymer separated and purified in concentration. In another embodiment of the present invention, the separated and purified polymer produced from the separation step is more concentrated than the concentration of the particulate additive associated with the base polymer and the polymer dispersed in the base polymer in the rAHP. Particulate additives associated with the polymer dispersed in the polymer separated and purified at low concentrations. In yet another embodiment of the present invention, the separated and purified polymer produced from the separation step is more concentrated than the concentration of the particulate additive associated with the base polymer and the polymer dispersed in the base polymer in rF. And a particulate additive associated with the polymer dispersed in the separated and purified polymer at a low concentration.

  In one embodiment of the invention, the concentration of particulate additive associated with each soluble polymer dispersed in the soluble base polymer in the separated and purified soluble polymer is in the base polymer in rAHP. Lower than the concentration of particulate additive associated with the polymer being dispersed. In another embodiment of the invention, the concentration of the particulate additive associated with each soluble polymer dispersed in each soluble base polymer in the separated and purified soluble polymer is about 3 It is less than wt%. In yet another embodiment of the present invention, the concentration of the particulate additive associated with each soluble polymer dispersed in each soluble base polymer in the separated and purified soluble polymer is about It is less than 1% by weight. In yet another embodiment of the present invention, the concentration of the particulate additive associated with each soluble polymer dispersed in each soluble base polymer in the separated and purified soluble polymer is: It is less than about 0.1% by weight. In one embodiment of the invention, each soluble polymer is essentially free of the particulate additive associated with each soluble base polymer in the separated and purified soluble polymer.

  In one embodiment of the invention, the separation process is in batch mode. In another embodiment of the invention, the separation process is in continuous mode.

  The dissolution process solvent separated in the separation process can be recycled back to the dissolution process either directly or after purification using methods well known to those skilled in the art.

Repeating Step In one embodiment of the present invention, a method for separating and purifying a polymer from a recycled product (rP) includes a step of extracting, a dissolving step, a sedimenting step, a purifying step, and a separating step, and repeating steps b to f. Repeating with each collection of precipitated particulate additives obtained from and all the domains of the rest of the polymer, one time and a sequence proceeding from the second soluble polymer through the further soluble polymer, A step of producing a separated and purified soluble polymer through extraction, dissolution, precipitation, purification, and separation of the soluble base polymer, wherein the sequence comprises each individual obtained from the rP. A final collection of particulate additives in which the soluble polymer was produced and precipitated in its isolated and purified form and all domains of the insoluble base polymer From the soluble base polymer having the lowest solubilization range to the highest solubilization range. In another embodiment of the present invention, a method of separating and purifying a polymer from a regenerated absorbent hygiene product (rAHP) comprises a delivery step, a dissolution step, a precipitation step, a purification step, and a separation step in steps b-f. Repeat with each collection of settled particulate additive obtained from the previous iteration and the domains of all of the remaining polymer, in one go and from the second soluble polymer through the additional soluble polymer. Producing a separated and purified soluble polymer through extracting, dissolving, precipitating, purifying, and separating the soluble base polymer in a sequence that comprises obtaining the soluble base polymer from the rAHP. Each of the individual soluble polymers produced was produced in its separated and purified form and precipitated into a final collection of particulate additives and of all insoluble base polymer. Until the domain is generated, traveling from soluble base polymer having the lowest solubilization range up solubilization range, comprising the step. In another embodiment of the present invention, a method of separating and purifying a polymer from recycled film (rF) comprises extracting, dissolving, precipitating, purifying, and separating steps from a previous iteration of these steps. Dissolution with each dissolution step collection of precipitated sedimentary particulate additive and domains of all of the remaining polymer, dissolving once, and in a sequence proceeding from the second soluble polymer through the additional soluble polymer. Producing a separated and purified soluble polymer through extracting, dissolving, precipitating, purifying, and separating the soluble base polymer, wherein the sequence comprises each individual dissolution obtained from the rF. The final collection of particulate additives in which the soluble polymer was produced in its isolated and purified form and precipitated and the domains of all insoluble base polymer were Until done, proceeding from soluble base polymer having the lowest solubilization range up solubilization range, comprising the step.

  In another embodiment of the present invention, a method of separating and purifying ADH, TPE, PP, PE, PET, cellulose, and PAA polymers from regenerated absorbent hygiene products (rAHP) includes extraction, dissolution, and precipitation steps. , Purification step, and separation step using each dissolution step collection of precipitated particulate additive and TPE, PP, PE, PET, cellulose, and PAA polymer domains obtained from a previous iteration of these steps. Extracting the TPE, PP, PE, and PET base polymers in a repeating sequence, one at a time, from the TPE base polymer to the PP base polymer, then to the PE base polymer, and finally to the PET base polymer, Produces a separated and purified soluble polymer via dissolution, precipitation, purification, and separation A step of producing a separated and purified TEP polymer, a separated and purified PP polymer, a separated and purified PE polymer, and a separated and purified PET polymer. Proceeding until a final collection of produced and precipitated particulate additive and the domains of cellulose and PAA polymer is produced.

  In one embodiment of the invention, the final collection of domains comprises cellulose and PAA polymer. In another embodiment of the invention, the final collection of domains is separated into the PAA polymer and the cellulosic polymer. One of the purposes of separating PAA and cellulose polymers is to reuse them in AHP in the future. In one embodiment of the invention, the PAA polymer separated from the final collection of domains comprises a concentration of water in excess of 30 g water / g PAA polymer. In another embodiment of the present invention, the PAA polymer is further dehydrated via a dehydration process to less than 1 g water / g PAA polymer. A non-limiting example of a dehydration process is contacting a PAA polymer with a salt solution, an acidic solution, a basic solution, and a solvent that forms an azeotrope with water, pressurizing, and centrifuging. In yet another embodiment of the invention, the dehydration process comprises contacting the PAA polymer with a salt solution, an acidic solution, a basic solution, and a solvent that forms an azeotrope with water, pressurizing, centrifugation. And a combination of these. Non-limiting examples of solvents that form an azeotrope with water are methanol, ethanol, n-propanol, isopropyl alcohol, n-butanol, isobutanol, and 2-butanol. In still yet another embodiment of the present invention, the solvent is an alcohol selected from the group consisting of methanol, ethanol, n-propanol, isopropyl alcohol, n-butanol, isobutanol, 2-butanol, and mixtures thereof. is there.

In one embodiment of the invention, the dehydrated PAA polymer is used to produce new AHP. In another embodiment of the invention, the PAA polymer is subjected to depolymerization to produce monomeric acrylic acid (AA) or oligomeric acrylic acid (OAA). In yet another embodiment of the invention, the AA or OAA is further polymerized to a virgin PAA polymer and used to produce new AHP. Non-limiting examples of depolymerization of PAA polymers include depolymerization in the presence of dissolved CO ₂ , depolymerization using ultrasonic and solar radiation, thermal decomposition, and mechanochemistry (eg, depolymerization is achieved. For applying mechanical force).

  FIG. 1 shows (a) acquisition step, (b) extraction step, (c) dissolution step, (d) sedimentation step, (e) purification step, (f) separation step, and steps (b) to (f). 3 is a schematic diagram of a process according to iterations.

Size Reduction Step In one embodiment of the invention, a method of separating and purifying a polymer from recycled product (rP), wherein the rP comprises the polymer and impurities, the polymer being associated with a base polymer and the polymer. And a particulate additive associated with the polymer, wherein the particulate additive associated with each polymer is dispersed in the base polymer at a concentration and the polymer is dissolved. Selected from the group consisting of soluble polymers, insoluble polymers, and mixtures thereof, wherein the impurities include particulate matter associated with the impurities and extractable materials associated with the impurities, and The extractable material comprises the extractable material associated with the polymer and the extractable material associated with the impurity, and the extractable material in the rP Methods are provided wherein the extractable material is present in the rP at a concentration. The method comprises: (a) obtaining rP, wherein the rP is selected from the group consisting of products after consumer use, products after industrial use, and combinations thereof; and (b) Reducing the size of the rP to particles having a maximum dimension of less than about 10 mm, and (c) solid separating each polymer of the rP in the polymer stream, each containing separately soluble polymer in a process that includes: Processing the polymer stream, comprising: (1) extracting the polymer stream containing the soluble polymer at a temperature above about 100 ° C. and a pressure above about 150 psig (1 MPa), the extraction solvent comprising: Has a normal boiling point of less than about 70 ° C. to produce extracted polymer, and the extractable material is above the concentration of the extractable material in the rP. And (2) dissolving the extracted polymer in a temperature range and pressure range sufficient to solubilize the soluble base polymer in the dissolution process solvent. A step of producing an initial suspension by dissolving the soluble polymer by contacting with a step solvent, the initial suspension comprising the particulate matter associated with the first soluble polymer. A step comprising a suspension of additive, and (3) allowing the initial suspension to settle in a temperature range and pressure range sufficient to produce a collection of settled particulate additive and an intermediate suspension. Wherein the settled collection of particulate additives comprises particulate additives associated with the first soluble polymer, the intermediate suspension being the first soluble base polymer solution. The first in A step comprising a suspension of unprecipitated particulate additive associated with a soluble polymer, and (4) using a solid medium in a temperature range and pressure range sufficient to produce a final suspension. A step of purifying the intermediate suspension, wherein the portion of the particulate additive associated with the first soluble polymer is retained by the solid medium, and the final suspension has the first solubility. A step comprising a suspension of unretained particulate additive associated with the first soluble polymer in a base polymer solution, and (5) producing a separated and purified first soluble polymer. A step of separating the dissolution step solvent from the final suspension in a temperature range and a pressure range sufficient for, wherein the separated and purified first soluble polymer is the first soluble base polymer. And the first dissolution in the rP Dissolved in the separated and purified first soluble polymer at a concentration lower than the concentration of the particulate additive associated with the first soluble polymer in the soluble polymer. A particulate polymer associated with the hydrophilic polymer, and
including.

  The size reduction step can be performed on various device components, as is well known to those skilled in the art. Non-limiting examples of equipment parts for this process are shredders, crushers, grinders, pulsarizers, choppers, shear slits and the like.

  In one embodiment of the invention, the particles have a maximum dimension of less than about 50 mm. In another embodiment of the invention, the particles have a maximum dimension of less than about 25 mm. In yet another embodiment of the invention, the particles have a maximum dimension of less than about 10 mm. In still yet another embodiment of the present invention, the particles have a maximum dimension of less than about 5 mm. In one embodiment of the invention, the particles have a maximum dimension of less than about 1 mm.

Solid Separation Step In one embodiment of the invention, the solid separation step comprises separating the rP particles into the polymer using a gravimetric technique. In another embodiment of the invention, the gravimetric technique comprises a series of liquids each filled with a liquid having a density between the density of the polymer fed into the tank and the density of the polymer separated at the outlet of the tank. Includes float / think tank. For example, to separate PP from PET, a stream containing PP and PET particles is fed to a tank containing water (density 1 g / mL), where PP with a density of about 0.905 g / mL floats. PET having a density of about 1.38 g / mL sinks. Similarly, to separate PP from PE, a stream containing PP and PE particles is fed to a tank containing 40 wt% isopropyl alcohol in water (density 0.926 g / mL), where the density is about 0. PP of 0.905 g / mL floats and PE of density about 0.95 g / mL sinks.

  In another embodiment of the invention, the solid separation step comprises separating the rP particles into the polymer using optical techniques.

  FIG. 2 shows (a) acquisition step, (b) size reduction step, (c) solid separation step, (1) extraction step, (2) dissolution step, (3) sedimentation step, (4) purification step, and ( 5) is a schematic diagram of a process according to the steps of 5) separating each polymer stream containing soluble polymer.

III. Test Methods The test methods described herein are used to measure the effectiveness of various methods for purifying polymers. Specifically, the methods described improve color and translucency / clarity (ie, bring the color and opacity of the reclaimed polymer closer to the unpigmented virgin polymer), reduce or eliminate elemental contamination. (Ie, removal of heavy metals), reduction or removal of non-combustible impurities (ie, inorganic fillers), reduction or removal of volatile compounds, especially volatile compounds that cause offensive odors in recycled products, and polymers. It demonstrates the effectiveness of a given purification method for reducing or removing impurities, such as polyethylene impurities in polypropylene.

Color and opacity measurements:
Polymer color and opacity / translucency are important parameters that determine whether a polymer can achieve the desired visual aesthetics of articles made from the polymer. For example, recycled polypropylene, especially recycled polypropylene obtained after consumer use, is typically deep in color and opaque due to residual pigments, fillers, and other impurities. Therefore, color and opacity measurements are important parameters that determine the effectiveness of polymer purification methods.

  Prior to measuring color, samples of either polymer powder or pellets are compression molded into square test specimens of 30 mm width x 30 mm length x 1 mm thickness (corners are rounded). The powder sample was prepared by first cold pressing the powder between stainless steel platens using a clean, unused aluminum foil foil as the contact release layer to form a sheet at room temperature (about 20-23 ° C). ) To increase the density. Then, using a stainless steel shim equipped with an aluminum platen, an unused aluminum foil foil release layer, and a cavity corresponding to a square test specimen of the above dimensions, approximately 0.85 g of cold pressed powder or Either of the pellets is compressed into test specimens with a Carver Press Model C (Carver, Inc., Wabash, IN 46992-0554 USA) preheated to 200 ° C. Heat the sample for 5 minutes before applying pressure. Then, after 5 minutes, compress with a press for at least 5 seconds with a hydraulic pressure of at least 2 tons (1.81 metric tons) and release. The molded laminate is then removed and placed between two thick flat metal heat sinks for cooling. The aluminum foil contact release layer is then peeled from the sample and discarded. The flash around at least one side of the sample is stripped to the edge of the mold, then the sample is extruded from the mold. Each test specimen is visually evaluated for void / bubble defects and only samples that are free of color measurement areas (minimum diameter 0.7 "(17.78 mm)) are used for color measurement.

The color of each sample is characterized using the International Commission on Illumination (CIE) three-dimensional color space of L ^* , a ^* , b ^* . The L ^* dimension is a measure of the lightness of the sample, L ^* = 0 corresponds to the darkest black sample and L ^* = 100 corresponds to the brightest white sample. The a ^* dimension is the red or green measurement of the sample, with positive values a ^* corresponding to red and negative values a ^* corresponding to green. The b ^* dimension is a measure of the blue or yellow color of a sample, with positive values of b ^* corresponding to blue and negative values of b ^* corresponding to yellow. The L ^* a ^* b ^* values of a square test specimen sample having a width of 30 mm, a length of 30 mm, and a thickness of 1 mm were measured using a HunterLab model LabScan XE spectrophotometer (Hunter Associates Laboratory, Inc., Reston, VA 20190-5280, USA). ). This spectrophotometer is equipped with D65 as a standard light source, and has an observation angle of 10 °, a field-of-view area diameter of 1.75 ″ (44.45 mm), and a port diameter of 0.7 ″ (17.78 mm).

The opacity of each sample is a measure of how much light passes through the sample (ie, a measure of the translucency of the sample), which is the HunterLab spectrophotometer described above, using the contrast ratio opacity mode. Will be decided. Two measurements are made to determine the opacity of each sample. One measures the lightness value Y white background of the sample on a _{white background} and the other measures the lightness value Y black background of the sample on a _{black background} . The opacity is then calculated from the lightness value using Equation 3 below.

Elemental analysis:
Much of the recycled polymer resources have unacceptably high levels of heavy metal contamination. The presence of heavy metals such as lead, mercury, cadmium, and chromium can prevent the use of reclaimed polymers in certain applications such as food or drug contact applications or medical device applications. Therefore, measuring the concentration of heavy metals is important in determining the effectiveness of polymer purification methods.

Elemental analysis is carried out using Inductively Coupled Plasma Mass Spectrometry (ICP-MS). The test solution was prepared by combining approximately 0.25 g of sample with 4 mL of concentrated nitric acid and 1 mL of concentrated hydrofluoric acid (HF), with n = 2 to n = 6, depending on sample availability. Prepared. Samples are degraded using the Ultrawave Microwave Digestion protocol consisting of 20 minutes to 125 ° C., 10 minutes to 250 ° C., 20 minutes at 250 ° C. The decomposed sample is cooled to room temperature. After adding 0.25 mL of 100 ppm Ge and Rh as an internal standard, the decomposed sample is diluted to 50 mL. To assess the accuracy of the measurements, pre-degradation spikes are prepared by spiking the virgin polymer. Virgin polymer spike samples were weighed using the same procedure as above, and each single sample of interest containing the appropriate amount of: Na, Al, Ca, Ti, Cr, Fe, Ni, Cu, Zn, Cd, and Pb. Spike with one element standard. The spikes are prepared at two different levels: "low spike" and "high spike". Each spike is prepared in triplicate. In addition to the virgin polymer spike, the blank is also spiked to ensure that there are no errors during pipetting and to track recovery throughout the process. The blank spiked sample is also prepared in triplicate at two different concentrations and treated in the same manner as the spiked virgin polymer and the test sample. 0.05, 0.1, 0.5, 1, 5, 10, 50, 100, and 500 ppb solutions containing Na, Al, Ca, Ti, Cr, Fe, Ni, Cu, Zn, Cd, and Pb. A 9-point calibration curve is created by creating All calibration standards are prepared by diluting undiluted standard reference solution with 0.25 mL of 100 ppm Ge and Rh as internal standards in 4 mL of concentrated nitric acid and 1 mL of concentrated HF. Prepared standards, test samples, and spiked test samples are analyzed using an Agilent 8800 ICP-QQQMS optimized according to manufacturer's recommendations. The m / z monitored for each sample and the collision cell gas used for the analysis are as follows: 23 m / z, H ₂ ; Al, 27 m / z, H ₂ ; Ca, 40 m / z, H ₂ ; Ti, 48 m / z, H ₂ ; Cr, 52 m / z, He; Fe, 56 m / z, H ₂ ; Ni, 60 m / z; no gas; Cu, 65 m / z, no gas; Zn, 64 m / z, He; Cd, 112 m / z; H ₂ ; Pb, total of 206 ≧ 206, 207 ≧ 207, 208 ≧ 208 m / z, no gas; Ge, 72 m / z, all modes; Rh, 103 m / z, all modes. Ge is used as an internal standard for all elements <103 m / z and Rh is used as an internal standard for all elements> 103 m / z.

Residual ash content:
Much of the recycled polymer resources include various fillers such as calcium carbonate, talcum, and fiberglass. While useful in the original application of the reclaimed polymer, these fillers alter the physical properties of the polymer such that it may be undesirable for subsequent uses of the reclaimed polymer. Therefore, measuring the amount of filler is important in determining the effectiveness of the polymer purification method.

  Thermogravimetric analysis (TGA) is performed to quantify the amount of non-combustible material (sometimes also referred to as ash) in the sample. Approximately 5-15 mg of sample is placed on a platinum sample pan and heated to 700 ° C at a rate of 20 ° C / min under air atmosphere in a TA Instruments model Q500 TGA instrument. The sample is held isothermally at 700 ° C for 10 minutes. After the isothermal holding, the residual mass ratio is measured at 700 ° C.

Odor analysis:
Odor sensation analysis is performed by placing approximately 3 g of each sample in a 20 mL glass vial and equilibrating at room temperature for at least 30 minutes. After equilibration, each vial is opened and a trained grader sniffs the headspace (snacks like a rabbit) and determines the odor intensity and descriptor profile. The odor intensity is evaluated according to the following scale: 5 = very strong, 4 = strong, 3 = moderate, 2 = weak to moderate, 1 = weak, 0 = no odor.

Polymer contamination analysis:
Many of the recycled polymer resources, especially those derived from mixed stream resources, may contain undesirable polymeric impurities. Without wishing to be bound by theory, polymer impurities (eg, polyethylene incorporation in polypropylene) can affect the physical properties of the polymer through the presence of heterogeneous phases and the resulting weak interactions. In addition, polymer impurities can also increase the opacity of the polymer and can affect color. Therefore, measurement of the amount of polymer impurities is important in determining the effectiveness of polymer purification methods.

  Quasicrystalline polymer impurities are evaluated using Differential Scanning Calorimetry (DSC). To measure the amount of PE impurities in PP, 2, 4, 6, 8, and 10 wt% of Formolene® HB5502F HDPE in Pro-fax 6331 polypropylene (Lyondell Basell Industries Holdings, BV). Prepare a set of 5 PP / PE blends containing (Formosa Plastics Corporation, USA). Approximately 5-15 mg of each sample is sealed in an aluminum DSC dish and analyzed on a TA Instruments model Q2000 DSC using the following method: equilibrate at 30.00 ° C, 200.00 at 20.00 ° C / min. ° C, mark the end of cycle 0, mark 20.00 ° C / min to 30.00 ° C, mark the end of cycle 1, mark 20.00 ° C / min to 200.00 ° C, Mark end of cycle 2 to 30.00 ° C at 20.00 ° C / min, mark end of cycle 3 to 200.00 ° C at 5.00 ° C / min, and cycle 4 Mark the end.

  The 5.00 ° C./min DSC thermogram is used to calculate the melting enthalpy of the HDPE peak around 128 ° C. for each sample of known HDPE content. A linear calibration curve is established by plotting the enthalpy of fusion against the known HDPE concentration (wt%).

  Samples with unknown PE content are analyzed using the same DSC apparatus and method described above. PE content is calculated using the calibration curve described above. The particular HDPE used to generate the calibration curve is very likely to have a different degree of crystallinity as compared to the polyethylene (or polyethylene blend) contamination that may be present in the recovered polypropylene sample. . Crystallinity can independently affect the measured enthalpies of fusion of polyethylene and thus also the calculation of the resulting polyethylene content. However, the DSC test described herein is intended to be used as a relative indicator to compare the effectiveness of various methods of purifying polymers, and to determine the exact polyethylene content in polymer blends. It is not intended to be quantified. Although the above method describes the measurement of PE incorporation in PP, the method is also applicable to the measurement of other quasicrystalline polymers using different temperature ranges and peaks in the DSC thermogram. In addition, other methods such as nuclear magnetic resonance (NMR) spectroscopy can be used to determine the amount of impurities in both quasicrystalline and amorphous polymers in a sample.

  All documents cited herein, including any patents or patent applications that are cross-referenced or related, are hereby incorporated by reference in their entirety, unless expressly excluded or otherwise limited. Be done. Citation of any reference to such invention, whether it is prior art relating to any invention disclosed and claimed herein, or whether it is alone or in any combination with any other reference No admission is made to teach, suggest, or disclose. Furthermore, if any meaning or definition of a term in this document conflicts with the meaning or definition of the same term in the document incorporated by reference, the meaning or definition given to that term in this document shall apply. Shall be.

  While particular embodiments of the present invention have been illustrated and described, it would be obvious to those skilled in the art that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this patent.

Claims (15)

A method of separating and purifying a polymer from a recycled product (rP), wherein the rP comprises a polymer and impurities, the polymer comprising a base polymer, a particulate additive associated with the polymer, and an extraction associated with the polymer. The particulate additive, which comprises possible materials and is associated with each polymer, is dispersed in the base polymer at a concentration, and the method comprises
a. Obtaining the rP, wherein the rP is selected from the group consisting of post consumer use products, post industrial use products, and combinations thereof,
b. Extracting the rP with an extraction solvent at a temperature above about 100 ° C. and a pressure above about 150 psig (1 MPa), wherein the extraction solvent has a normal boiling point of less than about 70 ° C. Producing (erP), the extractable material having a concentration in the erP that is lower than the concentration of the extractable material in the rP.
c. The first soluble base polymer of the rP by contacting the erP with the dissolution process solvent in a temperature range and pressure range sufficient to solubilize the first solubility base polymer in the dissolution process solvent. Producing an initial suspension by dissolving the particulate additive, wherein the initial suspension is associated with the first soluble polymer in a first soluble base polymer solution. And a suspension of domains of all of the remaining polymer, wherein the first soluble base polymer has a solubilization range less than that of the remaining soluble base polymer,
d. Collecting the settled collection of particulate additives and domains of all of the remaining polymer, and the initial suspension in a temperature range and pressure range sufficient to produce an intermediate suspension, the method comprising: A collection of settled particulate additives comprises particulate additives associated with the first soluble polymer, and the intermediate suspension comprises the first soluble base polymer solution in the first soluble base polymer solution. A step comprising a suspension of unprecipitated particulate additive associated with a soluble polymer;
e. Purifying the intermediate suspension using a solid medium in a temperature range and pressure range sufficient to produce a final suspension, the particulate additive associated with the first soluble polymer. A portion of the solid medium is retained by the solid medium and the final suspension is a suspension of unretained particulate additive associated with the first soluble polymer in the first soluble base polymer solution. Including a process, and
f. Separating the dissolution step solvent from the final suspension in a temperature range and pressure range sufficient to produce a separated and purified first soluble polymer, wherein the separated and purified first Of the soluble polymer is less than the concentration of the first soluble base polymer and the particulate additive associated with the first soluble polymer in the first soluble polymer in the rP. A concentration of the particulate additive associated with the first soluble polymer dispersed in the separated and purified first soluble polymer;
g. Step b (extraction step), c (dissolution step), d (sedimentation step), e (purification step), and f (separation step) are added to the sedimented particulate form obtained from the previous repetition of steps b to f. Extracting and dissolving the soluble base polymer, repeating with each collection of agents and domains of all of the remaining polymer, in one go and in a sequence that proceeds from the second soluble polymer through the additional soluble polymer. Producing a separated and purified soluble polymer through precipitation, purification, and separation, wherein the sequence comprises separating and purifying each individual soluble polymer obtained from the rP. The soluble base having the lowest solubilization range until the final collection of particulate additives produced in the formed form and the domains of all insoluble base polymer are produced. It proceeds from Rimmer to a maximum of solubilization range, and the process,
Including,
The polymer is selected from the group consisting of soluble polymers, insoluble polymers, and mixtures thereof, and the impurities include particulate matter associated with the impurities and extractable material associated with the impurities. The extractable material in the rP comprises the extractable material in association with the polymer and the extractable material in association with the impurities, the extractable material in the rP being in the rP The method is present in a concentration at.   The method of claim 1, wherein the rP is recycled film (rF).   The method of claim 2, wherein the rF comprises at least two polymers.   The method of claim 1, wherein the rP is a regenerated absorbent hygiene product (rAHP). The method is
a. obtaining rAHP, wherein the rAHP is selected from the group consisting of products after consumer use, products after industrial use, and combinations thereof,
b. Extracting the rAHP with an extraction solvent at a temperature above about 100 ° C. and a pressure above about 150 psig (1 MPa), wherein the extraction solvent has a normal boiling point below about 70 ° C. Producing (erAHP), the extractable material having a concentration in the erAHP that is lower than the concentration of the extractable material in the rAHP.
c. The first soluble base polymer of the rAHP by contacting the erAHP with the dissolution process solvent in a temperature range and pressure range sufficient to solubilize the first solubility base polymer in the dissolution process solvent. Producing an initial suspension by dissolving the particulate additive, wherein the initial suspension is associated with the first soluble polymer in a first soluble base polymer solution. And a suspension of domains of all of the remaining polymer, wherein the first soluble base polymer has a solubilization range less than that of the remaining soluble base polymer,
d. Collecting the settled collection of particulate additives and domains of all of the remaining polymer, and the initial suspension in a temperature range and pressure range sufficient to produce an intermediate suspension, the method comprising: A collection of settled particulate additives comprises particulate additives associated with the first soluble polymer, and the intermediate suspension comprises the first soluble base polymer solution in the first soluble base polymer solution. A step comprising a suspension of unprecipitated particulate additive associated with a soluble polymer;
e. Purifying the intermediate suspension using a solid medium in a temperature range and pressure range sufficient to produce a final suspension, the particulate additive associated with the first soluble polymer. A portion of the solid medium is retained by the solid medium and the final suspension is a suspension of unretained particulate additive associated with the first soluble polymer in the first soluble base polymer solution. Including a process, and
f. Separating the dissolution step solvent from the final suspension in a temperature range and pressure range sufficient to produce a separated and purified first soluble polymer, wherein the separated and purified first Of the soluble polymer is lower than the first soluble base polymer and the concentration of the particulate additive associated with the first soluble polymer in the first soluble polymer in the rAHP. A concentration of the particulate additive associated with the first soluble polymer dispersed in the separated and purified first soluble polymer;
g. Step b (extraction step), c (dissolution step), d (sedimentation step), e (purification step), and f (separation step) are the precipitated particles obtained from the previous repetition of steps b to f. Extracting the soluble base polymer, repeating with each collection of additives and the domains of all of the remaining polymer, in one step and in sequence, proceeding from the second soluble polymer through the additional soluble polymer, Producing a separated and purified soluble polymer via lysing, settling, purifying, and separating, said sequence wherein each individual soluble polymer obtained from said rAHP The dissolution with a minimum solubilization range until a final collection of particulate additive produced in a purified form and precipitated and the domains of all insoluble base polymer are produced. Travels from the base polymer to a maximum solubilization range, the steps,
The method of claim 4, comprising:   6. The method of claim 5, wherein the rAHP is selected from the group consisting of baby diapers, feminine protection products, adult incontinence products, and mixtures thereof.   6. The method of claim 5, wherein the method further comprises sterilizing the rAHP after the obtaining step.   6. The method of claim 5, wherein the method further comprises reducing the size of the rAHP after the obtaining step and before the extracting step.   9. The method of claim 8, wherein the reducing step comprises milling, cutting, shearing, or a combination thereof.   6. The method of claim 5, wherein the erAHP is essentially free of the extractable material.   The soluble polymer is selected from the group consisting of polypropylene (PP), polyethylene (PE), poly (ethylene terephthalate) (PET), adhesive (ADH), thermoplastic elastomer (TPE), and mixtures thereof. The method according to claim 5.   The first soluble polymer is ADH, the second soluble polymer is TPE, the third soluble polymer is PP, the fourth soluble polymer is PE, and the fifth soluble polymer is The method according to claim 11, wherein the functional polymer is PET.   The particulate additive associated with each soluble polymer is a fining agent, flame retardant, filler, reinforcing agent, antacid, stabilizer, antioxidant, slip agent, anti-tacking agent, lubricant, release agent. The method of claim 5, wherein the method is selected from the group consisting of :, a nucleating agent, a pigment, and mixtures thereof.   The method of claim 5, wherein the insoluble polymer is selected from the group consisting of cellulose, hemicellulose, lignin, poly (acrylic acid) (PAA), and mixtures thereof.   15. The method of claim 14, wherein the insoluble polymers are cellulose and PAA.

Images