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EP3749499A1 - Extrudeuse, système comprenant une extrudeuse, procédé de production de produits polymères cibles à partir d'un matériau contenant du plastique à partir d'une solution à l'aide d'une telle extrudeuse - Google Patents

Extrudeuse, système comprenant une extrudeuse, procédé de production de produits polymères cibles à partir d'un matériau contenant du plastique à partir d'une solution à l'aide d'une telle extrudeuse

Info

Publication number
EP3749499A1
EP3749499A1 EP19705143.6A EP19705143A EP3749499A1 EP 3749499 A1 EP3749499 A1 EP 3749499A1 EP 19705143 A EP19705143 A EP 19705143A EP 3749499 A1 EP3749499 A1 EP 3749499A1
Authority
EP
European Patent Office
Prior art keywords
solvent
extruder
target polymer
solution
water
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP19705143.6A
Other languages
German (de)
English (en)
Inventor
Hans-Jürgen Gnam
Renè GLOOR
Tamer Balikavlayan
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Domo Engineering Plastics GmbH
Original Assignee
Domo Engineering Plastics GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Domo Engineering Plastics GmbH filed Critical Domo Engineering Plastics GmbH
Publication of EP3749499A1 publication Critical patent/EP3749499A1/fr
Pending legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B17/00—Recovery of plastics or other constituents of waste material containing plastics
    • B29B17/02—Separating plastics from other materials
    • B29B17/0206—Selectively separating reinforcements from matrix material by destroying the interface bound before disintegrating the matrix to particles or powder, e.g. from tires or belts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B17/00—Recovery of plastics or other constituents of waste material containing plastics
    • B29B17/02—Separating plastics from other materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
    • B29B7/58—Component parts, details or accessories; Auxiliary operations
    • B29B7/66—Recycling the material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/74—Mixing; Kneading using other mixers or combinations of mixers, e.g. of dissimilar mixers ; Plant
    • B29B7/7476—Systems, i.e. flow charts or diagrams; Plants
    • B29B7/748—Plants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/80—Component parts, details or accessories; Auxiliary operations
    • B29B7/88—Adding charges, i.e. additives
    • B29B7/885—Adding charges, i.e. additives with means for treating, e.g. milling, the charges
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/80—Component parts, details or accessories; Auxiliary operations
    • B29B7/88—Adding charges, i.e. additives
    • B29B7/90—Fillers or reinforcements, e.g. fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00—Making granules
    • B29B9/02—Making granules by dividing preformed material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/275—Recovery or reuse of energy or materials
    • B29C48/277—Recovery or reuse of energy or materials of materials
    • B29C48/278—Recovery or reuse of energy or materials of materials of additives or processing aids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/50—Details of extruders
    • B29C48/76—Venting, drying means; Degassing means
    • B29C48/762—Vapour stripping
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/50—Details of extruders
    • B29C48/76—Venting, drying means; Degassing means
    • B29C48/763—Vent constructions, e.g. venting means avoiding melt escape
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/50—Details of extruders
    • B29C48/76—Venting, drying means; Degassing means
    • B29C48/765—Venting, drying means; Degassing means in the extruder apparatus
    • B29C48/766—Venting, drying means; Degassing means in the extruder apparatus in screw extruders
    • B29C48/767—Venting, drying means; Degassing means in the extruder apparatus in screw extruders through a degassing opening of a barrel
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F6/00—Post-polymerisation treatments
    • C08F6/06—Treatment of polymer solutions
    • C08F6/10—Removal of volatile materials, e.g. solvents
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/20—Compounding polymers with additives, e.g. colouring
    • C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B13/00—Conditioning or physical treatment of the material to be shaped
    • B29B13/02—Conditioning or physical treatment of the material to be shaped by heating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B13/00—Conditioning or physical treatment of the material to be shaped
    • B29B13/06—Conditioning or physical treatment of the material to be shaped by drying
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B17/00—Recovery of plastics or other constituents of waste material containing plastics
    • B29B17/02—Separating plastics from other materials
    • B29B2017/0213—Specific separating techniques
    • B29B2017/0293—Dissolving the materials in gases or liquids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
    • B29B7/34—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices
    • B29B7/38—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2793/00—Shaping techniques involving a cutting or machining operation
    • B29C2793/0027—Cutting off
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92009—Measured parameter
    • B29C2948/92209—Temperature
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92009—Measured parameter
    • B29C2948/92228—Content, e.g. percentage of humidity, volatiles, contaminants or degassing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/001—Combinations of extrusion moulding with other shaping operations
    • B29C48/0022—Combinations of extrusion moulding with other shaping operations combined with cutting
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/05—Filamentary, e.g. strands
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/28—Storing of extruded material, e.g. by winding up or stacking
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
    • B29C48/397—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using a single screw
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/50—Details of extruders
    • B29C48/505—Screws
    • B29C48/57—Screws provided with kneading disc-like elements, e.g. with oval-shaped elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2023/00—Use of polyalkenes or derivatives thereof as moulding material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2023/00—Use of polyalkenes or derivatives thereof as moulding material
    • B29K2023/04—Polymers of ethylene
    • B29K2023/06—PE, i.e. polyethylene
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2077/00—Use of PA, i.e. polyamides, e.g. polyesteramides or derivatives thereof, as moulding material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2507/00—Use of elements other than metals as filler
    • B29K2507/04—Carbon
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2323/04—Homopolymers or copolymers of ethene
    • C08J2323/06—Polyethene
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/10—Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/62—Plastics recycling; Rubber recycling

Definitions

  • Extruder plant with an extruder, process for the preparation of target polymer products from a plastic-containing material from a solution using such an extruder
  • the present invention relates to an extruder as well as to a plant with such an extruder, and to a process for the production of target polymer products from a plastics-containing material, such as e.g. a single-grade target polymer or a composite material containing the target polymer from a solution using such an extruder; and the target polymer products obtainable by this method or equipment.
  • a plastics-containing material such as e.g. a single-grade target polymer or a composite material containing the target polymer from a solution using such an extruder
  • target polymer products obtainable by this method or equipment.
  • it relates to the preparation of these target polymer products from production waste of composite materials.
  • Raw material costs the time required for the production of a product and the costs for plant construction.
  • material recycling processes are becoming increasingly important. Recycling processes in which waste materials or individual constituents thereof are recycled materially have the great advantage that the raw materials used as raw materials are available free of charge or at low cost.
  • recycling processes must be energy-efficient and of great added value, and also the other requirements, such as a simple, rapid processing of large flow rates in the simplest possible apparatus.
  • a first problem is that recycling processes as well as primary production can be energy and material-consuming.
  • a second problem is that polymers differ in their macromolecular structure as thermosets, elastomers and thermoplastics and their chemical composition is usually so different that the workup must be polymer-specific.
  • a third problem is that polymers are being used more extensively in composite materials in which they are firmly bonded to other polymers as well as metals or other solids.
  • a first aspect of the present invention relates to the preparation of target polymer products from recycled target polymers, in particular thermoplastics, which are present as pure-type polymers or are contained as a constituent in a composite material with the solution of the above problems.
  • a second aspect of the present invention relates to the incorporation of large quantities of additives in the isolated target polymer products as part of the process for obtaining additive-containing target polymer products.
  • thermoplastics can be dissolved in organic solvents because of their straight-chain structure.
  • a known method for recycling thermoplastics is therefore to dissolve a thermoplastic in an organic solvent and to recover it in powder form from the solution. Achieving and maintaining the preferred powdered state proves difficult when working at elevated temperatures.
  • a powdered thermoplastic first transitions to the rubber-elastic state at the glass transition temperature, in which the particles stick together.
  • the particles melt, usually resulting in a viscous mass. If the viscous mass is subsequently cooled again, owing to the macromolecular structure of the polymers, rubbery or glassy or even sticky agglomerates often form.
  • target polymer product any product obtained by carrying out any of the processes of the invention.
  • target polymer product includes the target polymer products which are target polymers which may have a residual content of water and / or solvent, furthermore the target polymer products which can be prepared anhydrous and / or solvent-free by complete drying and the target polymer products into which additives such as carbon black or reinforcing fillers have been deliberately introduced. Irrespective of this definition, in the present description, target polymer products are sometimes referred to simply as shortened but also as target polymers.
  • a recycling process in which target polymers are obtained in powder consists of the selective dissolution of a water-insoluble target polymer in an organic solvent and its precipitation from the polymer solution with the aid of water.
  • the polymer solution can be introduced into liquid water.
  • the polymer solution may be initially charged and then the liquid water added. In this case, especially at room temperature, a pulverulent target polymer is frequently formed in a large amount of a water / solvent mixture.
  • EP 1 124 908 B1 describes a process for the preparation of dye-containing polymer particles which contain at least one dye in a matrix of a substantially water-insoluble polymer.
  • the polymer particles are precipitated from a solution of the polymer and the dye in a water-miscible organic solvent by adding an aqueous phase.
  • EP 0 644 230 B1 relates to a process for working up or reworking polyolefin granules, films or sheets and polyolefin-containing composite materials for virtually complete recycling of the individual components.
  • a polymer portion is dissolved in a solvent.
  • Olefinic polymers are dissolved, for example, in cycloalkanes and precipitated with an aqueous surfactant solution.
  • EP 1 646 678 B1 discloses a process for recovering at least one polymer dissolved in a solvent by precipitation with water. After dissolving the polymer, an additive can be added to the solution.
  • US 2008/47671 A1 describes a process for the recovery of a polymer dissolved in a solvent. Water is added to the homogeneous medium. From the heterogeneous medium formed, the solvent is removed by heating and evaporation. The homogeneous medium may contain additives.
  • DE 10 2014 114831 A1 and DE 10 2016 106726 A1 describe a process for the production of target polymer products from plastics-containing materials.
  • a solution with the target polymer product is dried successively with the addition of water vapor in a falling film evaporator, a thin film evaporator and in a vacuum screw and brought to the desired residual moisture of the solvent.
  • the object of the present invention is to provide equipment, systems and methods which can effectively extract further moisture, in particular solvent and / or water, from a concentrated target polymer solution.
  • An extruder has a housing, a first material inlet for a mixture of at least one solvent and dissolved agent, a material outlet, a worm drive screw, at least one distillation zone between inlet and outlet, which allows solvent and / or water to exit the mixture , and a derivative for the leaked solvent.
  • a plant for producing the target polymer product has at least one falling-film evaporator and / or a thin-film evaporator and an extruder connected thereto with a distillation zone for discharging solvent and / or water between the inlet and outlet of the extruder.
  • the solution is placed in an extruder having at least one distillation zone where solvent exits the surface of the solution and is removed.
  • a possible application of the invention is a process for producing a solid, preferably granular, crumbly or powdery target polymer product from a target polymer solution comprising the steps of: a) preparing the target polymer solution by dissolving the target polymer in a solvent or dissolving the target polymer with a solvent from a composite material and separating the target polymer solution from the insoluble components, b) concentrating the target polymer solution having a temperature above 100 ° C or at least the boiling temperature of water, preferably by contacting the target polymer solution with water vapor at a temperature of at least the boiling temperature the water, thereby expelling a solvent / water vapor mixture, and further concentrating with the described extruder until the target polymer product is in the form of a tough ductile solid strand, the temperature of the target polymer solution being lower than the boiling temperature when the solvent / water vapor mixture is expelled the target polymer solution remains.
  • the present invention furthermore relates to the additive-containing or additive-free target polymer products obtainable by the above or below-described process and / or with the described extruder and the overall plant.
  • the target polymer product may be in the form of a masterbatch which can serve as a carrier for pigments and in particular comprises a polyolefin, in particular a polyethylene, as a target polymer which contains at least 40% by weight, advantageously at least 50% by weight. and more preferably contains at least 60% by weight of carbon black.
  • the carbon black may be a carbon black as an additive for color pigmentation as well as a special carbon black for obtaining electrical conductivity in plastics.
  • the target polymer product may also be a compound which comprises, in particular, a polyolefin, in particular a polypropylene, as the target polymer, which reinforces talc and / or fibers with particularly long fiber lengths, wherein the fiber lengths may be more than 1 mm, typically 1 to 1, 5 mm, especially 2 mm or more than 3 mm.
  • the present invention furthermore relates to a process in which a solvent-containing polymer, in particular polyolefin, very particularly polyethylene, with or without additive addition, if appropriate with the aid of the described extruder, is dried only to the extent that a target polymer product with a residual solvent content in the range of 1 to 7% by weight, preferably 3 to 5 wt .-%, is present.
  • a solvent-containing polymer in particular polyolefin, very particularly polyethylene
  • polystyrene resin in particular polyethylenes or polypropylenes, may contain from 1 to 7% by weight, preferably from 3 to 5% by weight, of solvent.
  • the target polymer products in particular polyolefins such as polyethylenes and polypropylenes, may contain carbon black (s) and / or talc and / or reinforcing fillers with extra-long fibers greater than 1 mm and may contain from 1 to 7% by weight and preferably from 3 to 5% by weight % Solvent, which improves the material properties of the mixture in dispersing and granulating.
  • Target polymer is understood to mean any polymer which can be converted by the process according to the invention or by means of the described extruder or the overall plant into a solid and possibly granular and / or pulverulent solid and optionally mixed with additives target polymer product.
  • the method can serve for the separation of composites and / or the incorporation of additives into a polymer. It is first prepared in a step a) a target polymer solution.
  • the target polymer solution can be prepared by dissolving a single-grade target polymer to be worked up by a recycling process.
  • the target polymer can also be part of a too be recycled composite material.
  • the target polymer is selectively dissolved out of the composite by the solvent, while the other constituents of the composite form a solid residue which is separated, for example, by filtering or centrifuging.
  • step b) in other parts of the system then the expulsion of the solvent from the solution, including a distillation of the solvent from the solution takes place.
  • the extruder mentioned is used in a rather late process step.
  • polymer waste can be efficiently recycled and at the same time target polymer products can be obtained. It can be production and consumer waste.
  • the production waste comes from primary molding processes, such as polymer processing for the production of molded parts, semi-finished products, fibers or films by injection molding, extrusion, calendering, rotational molding, foaming, blow molding or the like.
  • the polymer wastes arising in these production processes are dissolved in step a) in a suitable organic solvent.
  • the layer structure of the film material can be destroyed by pregranulation before being dissolved. Pre-granulation ensures that all polymer layers of the multilayer film come into contact with the solvent.
  • non-polar target polymers are polyolefins, such as polyethylenes (PE) and polypropylenes (PP).
  • the polyethylene may be a high density polyethylene (HDPE), a low density polyethylene (LDPE), a linear low density polyethylene (LLDPE), a high molecular weight polyethylene (PE-HMW) or an ultra high molecular weight polyethylene (PE-UHMW)
  • polar target polymers are exemplified polyvinyl chloride (PVC), polyvinylidene chloride (PVDC), polystyrenes (PS), modified polystyrenes, styrene copolymers, polyacrylates, polymethacrylates, poly esters, such as polyethylene terephthalate (PET) or polybutylene terephthalate (PBT), polyamides and polycarbonates. This list is not intended to be limiting or conclusive.
  • the process according to the invention can be
  • the process is preferably used as a process for the recycling of single-grade polyolefins or polyolefins contained in a composite material and at the same time as a production process for polymer products.
  • Polymer products to be understood in this context are, in particular, polymers with additives which, compared to the polymers, are intended as virgin material and have intentionally changed properties.
  • a first example of such a composite material is a multilayer film containing at least one layer of polyethylene as the target polymer and at least one layer of polyamide.
  • the polyethylene can be dissolved out of the composite material with the aid of a non-polar solvent, for example at a temperature of about 100 ° C., the polyamide remaining as a solid.
  • multilayer films are PP / PA multilayer films, such as filter mats, PP / PET multilayer films, PP / PE multilayer films.
  • An example of composite material that is not a multilayer film is PVB glass composite, such as in automotive windshields, PE / aluminum, or PVC / aluminum, such as in medical packaging.
  • the target polymer can be dissolved in the solvent even at room temperature. However, for faster dissolution it is advantageous to prepare the target polymer solution by heating, stirring and pumping, the temperature remaining below the boiling temperature of the solvent. In addition, at higher temperatures, larger amounts of polymer can be solubilized to yield highly saturated or supersaturated target polymer solutions and can be used in the same way. less solvent is needed in a timely manner.
  • the dissolution process can be carried out, for example, at 50 to 150 ° C., such as at 100 ° C., with higher and lower temperatures being typical, depending on the type of polymer and the type of solvent, in particular as a function of the boiling temperature of the solvent Upper temperature limit for the dissolution of the target polymer, are also possible.
  • the solubility of the target polymers in a solvent also depends on the polar or non-polar character of the solvent and the target polymer.
  • Polar solvents preferably dissolve polar polymers, non-polar solvents preferably nonpolar polymers.
  • the solubility parameter of the target polymer must be similar to the solubility parameter of the solvent.
  • solubility parameter reference is made to the following specialist literature: "Properties of Polymers", DW van Krevelen, 1990, pp. 200-202, "Polymer Flandbook”, J. Brandrup and EH Immergut, ed. 2nd edition p IV-337 to IV-359. Suitable solvents can also be found in the Plastics Handbook (Kunststoff-Handbuch, Bd.
  • the other constituents of the composite material should be insoluble or only very slightly soluble in the solvent.
  • the excipients may be soluble in the solvent or included in the target polymer solution if they can be readily removed in a further process step or if they can remain in the solid target polymer without adverse effects.
  • An example of ingredients that may remain in the target polymer is levels of color pigments or dyes when the process according to the invention is used for producing a soot-containing masterbatch in which the carbon black covers the coloration of the target polymer.
  • An example of the selective dissolution of a polymer from a composite material is the above-mentioned dissolving out of polyethylene with a non-polar solvent from a PE-PA multilayer film in which the polyamide remains as an insoluble solid. It is a particular advantage of the process according to the invention that constituents from the starting polymer, such as color pigments or dyes, can remain completely, partially or in low concentration in the target polymer product if the target polymer product is so strongly colored by a newly introduced additive that a staining caused by residues is sufficiently covered. In this way, a complex cleaning step to completely remove originally contained components can be avoided.
  • Suitable solvents are organic aromatic or non-aromatic solvents, non-aromatic solvents being preferred for their lower toxicity.
  • Halogen-free polar solvents are preferred for the polar polymers, such as alcohols, ketones, ethers and esters. Particularly advantageous is the use of methanol, ethanol, propanol, isopropanol, acetone, methyl ethyl ketone, tetrahydrofuran and methyl acetate.
  • Fatty acid esters and fatty acid ester mixtures fractions from petroleum distillation, in particular gasoline fractions or diesel fuels, aliphatic hydrocarbons, alicyclic hydrocarbons, aromatic hydrocarbons, can be used for the dissolution of nonpolar target polymers, in particular the polyolefins preferably used, such as polyethylenes or polypropylenes , individually or in mixture.
  • nonpolar target polymers in particular the polyolefins preferably used, such as polyethylenes or polypropylenes , individually or in mixture.
  • fatty acid ester mixtures Biodiesel with a boiling range of 300 to 570 ° C and rapeseed oil are considered.
  • Suitable petroleum fractions include fuel oil and diesel fuel with a boiling range of 170 to 390 ° C.
  • Benzine fractions which are suitable as solvents for non-polar polymers are: the type 1 (boiling range 130-185 ° C) benzene, type 2 (boiling range 140-200 ° C), type 3 (150-190 ° C), Type 4 (boiling range from 180-220 ° C) and Type 5 (boiling range 130-220 ° C), which are also referred to as turpentine substitute, "white spirit" or mineral spirit, the Siebenzennenzine type 2 (boiling range 80-110 ° C) and Type 3 (boiling range 100-140 ° C), benzine (boiling range 80-110 ° C), Aliphatin (boiling range 100-160 ° C), Ligroin (bp 150-180 ° C) and kerosene (boiling range 180- 270 ° C).
  • n-alkanes n-alkanes, z. C8-C17 alkane fractions, as well as isoalkanes such as C10-C25 fractions and isoparaffins.
  • Alicyclic hydrocarbons such as cycloalkanes, e.g. As cycloheptane, and aromatic hydrocarbons such as toluene or xylenes, are also suitable as solvents for non-polar target polymers.
  • the solvent may comprise the above substances individually or as a mixture of two or more of said substances.
  • the solvent may have added additives which may be up to 2 or 5 or 10 or 20% by weight.
  • the process according to the invention is carried out in step b) with a target polymer solution which has a temperature of at least the boiling point or above the boiling point of water.
  • the target polymer solution should preferably remain liquid when the hot steam is introduced and should not boil. Therefore, solvents with a relatively high boiling temperature are preferred.
  • the solvents used according to the invention or its components therefore have a boiling point above 100 ° C., preferably above 110 ° C., for example in the range from 140 to 180 ° C., at atmospheric pressure. Although higher-boiling solvents are preferred, the problem with particularly high-boiling solvents is that the solvents are only expelled with difficulty or only with very hot steam. that can.
  • An upper limit for the boiling temperature is therefore 570 ° C, as it can be found in biodiesel, because of the easier vaporizability better below 300 ° C, preferably below 250 ° C or below 220 ° C.
  • the rate at which the solvent vaporizes can be controlled by the temperature of the hot water vapor and the temperature of the target polymer solution, taking care that the solvent in the apparatus used is preferably non-boiling.
  • Solvents such as hexane or cyclohexane, which boil below 100 ° C, are less suitable because they evaporate too quickly on contact with hot water vapor, resulting in sticky and viscous, unsuitable for further processing target polymer masses within the apparatus and not the desired solid, possibly granular , would lead to powdery material.
  • the abovementioned high-boiling solvents have particularly good dissolving properties for the target polymers, in particular polyolefins.
  • target polymers in particular polyolefins.
  • the good solution properties and the low vapor pressure of the solvent fundamentally involve the problem of effectively removing the dissolved target polymer from the solvent to a defined residual content.
  • One of the very essential advantages of the process according to the invention is that the high-boiling solvents, despite their low vapor pressure with the aid of a suitably hot water vapor at a suitably high selected process temperature of the solvent can be removed again up to a desired residual content as an additive from the target polymer but the solubilizer / target polymer solution is in liquid form until the end, before the target polymer product changes into a solid and finally possibly granular or powdery form.
  • This avoids the problems associated with the use of low-boiling and therefore explosive evaporating solvents such as acetone, hexane or methyl ethyl ketone.
  • the solvent or its components may be miscible or immiscible with water.
  • the solvent is not miscible with water, since in this case after the expulsion of the mixture of water vapor and solvent and its condensation, a biphasic liquid is obtained, which can be easily separated into water and solvent. Water and solvents can thus easily be recycled as separate phases in the process.
  • the target polymer solution prepared in step a) of the process according to the invention has a target polymer to solvent ratio preferably in the range from 1: 5 to 1:20 parts by weight, more preferably in the range from 1: 6 to 1:15 parts by weight, and most preferably in the range from 1: 7 to 1: 10 parts by weight.
  • the optionally prepared at room temperature or present Zielpoly merlets can be heated advantageously for step b) to a temperature of more than 100 ° C or at elevated pressure of at least the boiling temperature of water.
  • the thus heated target polymer solution is brought into contact with water vapor at a temperature of at least the boiling point of water.
  • the target polymer solution is typically low viscosity prior to the start of solvent evaporation in step b), which is advantageous for its flowability in devices while facilitating the penetration of water vapor into the target polymer solution.
  • the hot steam with a temperature of at least 100 ° C or with a temperature of at least the boiling point of water at elevated pressure ensures the evaporation of the solvent, whereby the speed can be influenced by the height of the steam temperature the solvent is expelled together with water vapor.
  • the steam can be generated in a steam boiler plant. With the superheater, the water vapor can be further heated above its evaporation temperature, producing superheated steam or superheated steam.
  • Water is either a vapor or a liquid, depending on the pressure, between the triple point at 0 ° C and the critical point at approx. 375 ° C, so that a suitable pressure / temperature combination must be selected in order to obtain water vapor Increasing the pressure, the boiling point of the water and thus the water vapor temperature can be increased.
  • a pressure of 6 bar water boils at 156 ° C
  • a pressure of 10 bar boiling water at about 180 ° C, so that steam temperatures of 180 ° C or even above can be easily generated by a superheater at a operated according to high pressure and the water vapor escapes under expansion and pressure drop from the superheater.
  • the pressure required for a given steam temperature results from the pressure-temperature diagram ((p, T) -diagram) of water, which is attached as FIG. According to the diagram, it is also possible to produce hot steam in the apparatus with an overpressure above atmospheric pressure.
  • Fig. 1 also shows the dependence of the boiling point of the water on the prevailing pressure.
  • the temperature data in this description relate to ambient pressure. If other pressures prevail, correspondingly shifted values may apply.
  • the expulsion of the solvent mixed with steam according to step b) of the invention can be further accelerated by additionally heating the target polymer solution by an external heating device in contact with the target polymer solution.
  • the target polymer solution is heated by both the hot water vapor and the external heater, which can accelerate the evaporation of the solvent below its boiling point, especially in the case of very high boiling solvents.
  • the external heater By the external heater, the temperature of the target polymer solution can be increased even further than with the water vapor.
  • the external heating the use of less hot water vapor to heat the target polymer solution to the same temperature.
  • a temperature above the boiling point of water prevails in the evaporation device (s) at the pressure prevailing in the device. This prevents condensation of the water in the apparatus, which is therefore always gaseous.
  • An exception is the water, which, in a dynamic equilibrium, increasingly penetrates into the target polymer solution and is incorporated into the target polymer.
  • the temperature of the hot steam is at least 100 ° C or above 100 ° C and at most at the boiling temperature of the target polymer solution.
  • the temperature of the water vapor is within this interval, the solvent is expelled without steam as vapor mixture with steam and at the same time water is stored in the solution.
  • the temperature of the hot water vapor is preferably about 10 to about 100 ° C lower than the boiling temperature of the solvent or the target polymer solution.
  • the rate at which the solvent evaporates can be controlled by means of this temperature difference between the boiling temperature of the target polymer solution and the steam temperature.
  • the person skilled in the art can readily choose the type and the desired boiling point of the solvent, the temperature of the target polymer solution when introducing the steam and the temperature of the hot steam so that from the target polymer solution a solid, possibly granular or pulverulent target polymer product with defined residual solvent content in the desired process time with the desired evaporation rate of the solvent is obtained.
  • the hot water vapor may be introduced into the target polymer solution and optionally further added to the target polymer solution to flow over the surface of the target polymer solution.
  • the hot water vapor is preferably introduced directly into the target polymer liquid or injected under elevated pressure. The water vapor then has atmospheric pressure or a slight overpressure of, for example, 2 bar in the target polymer solution.
  • the introduction of the hot steam and the evaporation of the solvent-water vapor mixture is preferably carried out in one or more falling-film evaporators and / or in one or more thin film evaporators.
  • Falling film evaporators are particularly well suited for concentrating the target polymer solution, the target polymer still being present as a solution after concentration. Due to their construction, thin film evaporators can be used for the further concentration of the target polymer solution, whereby the target polymer can be obtained after concentration as a viscous or granular or pulverulent product.
  • step b) of the method according to the invention it is therefore particularly preferred to use one or more falling-film evaporators and subsequently one or more thin-layer evaporators or exclusively a plurality of thin-layer evaporators for carrying out step b) of the method according to the invention.
  • the quantitative ratio of target polymer to solvent is in the range from 1: 0.5 to 1: 4 parts by weight, and so much solvent is expelled in the thin film evaporator (s) that the target polymer solution contains from 7% to 20% by weight of solvent, based on the total weight of the target polymer and solvent.
  • a construction of one or more suitably attached nozzles can be used.
  • High pressure can prevail upstream of the nozzle and water (just barely) is liquid.
  • Downstream relaxation takes place on the pressure in the solution tank or tube or evaporator (atmospheric pressure or above), the conditions in each case being such that water is applied or applied as vapor.
  • the target polymer solution is a thin flowing liquid film, such as in a large-scale plant in a falling film evaporator
  • the hot water vapor may be cocurrently or countercurrently flowed onto the thin film.
  • the hot steam has several functions in the process according to the invention: a first function is to heat the target polymer solution, whereby a mixture of solvent and water vapor is expelled and the target polymer solution is concentrated. This heating function can advantageously be supplemented by heating the target polymer solution with an external heating device; a second function is to keep the target polymer solution in the liquid state to a high degree of saturation without accumulating the target polymer as a solid, which facilitates processing; a third function of the water vapor is to vigorously stir the target polymer solution when it is introduced or pressed into the target polymer solution.
  • this stirring function partially replaces the use of stirring devices in an industrial plant; -
  • a fourth invention very essential function
  • the water vapor that is introduced or injected into the target polymer solution is to drastically increase the surface from which the solvent of the target polymer solution can evaporate into the gas phase.
  • the evaporation surface in evaporators usually consists of the surfaces that the evaporator, such as a falling film evaporator, provides even for the formation of a liquid film.
  • the introduction or injection of hot steam into the target polymer solution results in the formation of a large number of fine water vapor bubbles in the target polymer solution, the surfaces of which form a very large additional evaporation surface into which the solvent can evaporate.
  • the rate of evaporation can be dramatically increased over evaporation without the introduction of water vapor. Comparative experiments have shown that at the same temperature, the evaporation rate can be increased by 5 to 10-fold, in particular 7 to 8-fold, when water vapor is introduced into the target polymer solution and the water vapor in the target polymer solution forms bubbles in the into which the solvent can evaporate.
  • the target polymer product formed after carrying out the process according to the invention with defined residual solvent content as an additive is granular or powdery, has excellent rheological properties, is dry and non-sticky when touched and is thus an ideal starting material for the preparation of new target polymer products obtained in this way Zielpoly mer. With the help of water vapor, the powdery target polymer product acquires a structure which, as explained below, is ideal for the storage of additives and other applications.
  • step b) of the process the solvent is first expelled gradually with the aid of the hot water vapor as a solvent-water vapor mixture. Thereafter, the described extruder is used to further deprive solvent and residual moisture / water.
  • An initially low-viscosity target polymer solution results in a concentrated target polymer solution, which becomes increasingly viscous at the prevailing temperature, but without losing its fluidity.
  • the increasingly viscous target polymer solution is concentrated to such an extent that the target polymer is obtained at the high process temperatures in step b) without cooling as a plastically deformable strand at the exit of the extruder, which still contains certain amounts of solvent and Contains water.
  • the target polymer product thus obtained preferably contains from 7 to 13% by weight of solvent, based on the total weight of the target polymer and solvent. More preferably, the solvent content is 9 to 11% by weight.
  • the water content is typically from 2 to 8% by weight and is one of the reasons for the excellent properties of the resulting target polymer product. While under the prevailing temperature conditions polymers usually form a tough solid during concentration, a product is obtained under the effect of water vapor.
  • the invention furthermore relates to the target polymer products obtainable by the above process.
  • the target polymer products substantially owe their properties to the effect of water vapor on the target polymer solution at a temperature above 100 ° C., so that the water used is present in gaseous form as water vapor, but chosen to be so low that the target polymer solution solution remains liquid without boiling.
  • water molecules are incorporated directly into the target polymer fluid. Under the prevailing temperature conditions, a dynamic equilibrium may arise in which water molecules which are incorporated into the target polymer solution are also desorbed again. In this dynamic equilibrium of absorption and desorption, the water molecules at least partially displace the organic solvent from the composite of the target polymer molecules. Initially, the heat drawn macromolecules are kept separate by organic solvent.
  • the granular or pulverulent target polymer product obtained in step b) which still contains 7 to 20% by weight of solvent and 2 to 8% by weight of water can be heated in a further step c) without supplying hot steam to a target polymer product having further reduced solvent content and significantly reduced water content.
  • the target polymer from step b) after processing in the extruder, for example in a mill or with the aid of heating screws, preferably in vacuo, dried, after which the solvent content of the target polymer product at 1 to 7 wt .-%, preferably at 3 to 5 % By weight.
  • the product with this residual solvent content is ideally suited for subsequent granulation or other applications.
  • the target polymer product from step b) can be granulated after leaving the extruder and initially further simply ground into a powder before it is dried in step c).
  • the drying is carried out at elevated temperature, the temperature being selected such that the solvent escapes from the target polymer at a sufficient rate, but at the same time does not soften the granular or pulverulent polymer particles and stick together or melt together.
  • the target polymer product obtained in step c) has surprising melting and flow properties.
  • a polyethylene product obtained by the process of the present invention is disclosed. While a powdered polyethylene containing no solvent has a melt flow index (MFI) of about 5, the inventive solvent content of 1 to 7 wt .-% and preferably 3 to 5 wt .-% results in that the MFI value of Polyethylene product when melting about 10 goes up.
  • MFI melt flow index
  • the MFI value thus increased corresponds to a higher fluidity of the polymer melt, which allows better processing in an extruder and, as will be shown below, better distribution of additives in the molten target polymer.
  • the MFI measurement is carried out according to the standardized method with the molten polyethylene produced according to the invention at 190 ° C., which flows through a defined bore under a pressure of 2.16 kg.
  • the target polymer particles formed in step b) of the process according to the invention are presumed to have an open and porous structure and have an increased melt flow index and increased surface area compared with the particles of the prior art. For these reasons, a surprisingly large amount of additives can be incorporated into the target polymer products obtained in step b).
  • a further preferred embodiment of the method according to the invention therefore consists in adding an additive or a mixture of additives in the course of carrying out step b).
  • the additive or the mixture of additives may be added in solid form, but in particular in liquid form, as a suspension or as a solution, wherein the solvent or the liquid for the preparation of the suspension is preferably the same liquid, which is also used for dissolving the target polymer.
  • the additive or mixture of additives is added, with the additive or mixture of additives - added to the target polymer solution as soon as the solvent evaporates Increased the ratio of target polymer to solvent to a value in the range of 1: 0.5 to 1: 4 parts by weight or - mixed into the target polymer solution before it is introduced into the first thin-film evaporator.
  • an additive can also be supplied via the extruder.
  • an additive-containing granular or pulverulent target polymer product can thus be obtained, after carrying out step c), a dried additive-containing pulverulent or granular target polymer product.
  • the additive content may be more than 50% by weight, based on the total weight of target polymer, additive and residual solvent.
  • the excellent theological and haptic properties of the granular or powdery target polymer products and their ability to take up large amounts of additives, thereby enabling the preparation of high additive masterbatches (compounds), are essential features of the process of the present invention and the target polymer products of the present invention It is believed that the high absorbency for additives is due to a highly loosened microscopic structure of the granular or powdery target polymer particles as a result of a greatly increased specific surface area due to the continuous exposure to water vapor upon expulsion of the solvent and the high melt flow index as a result defined residual solvent content is caused.
  • a further additive or mixture of additives is added.
  • the addition of various additives at different times of the process according to the invention enables the targeted introduction of various additive combinations into the gradually solidifying target polymer product. For example, during the execution of step b), a soot can be added.
  • a reinforcing filler of fibers with a high fiber length can be added.
  • the additives can be solid additives which are advantageously selected from carbon blacks, organic pigments, inorganic pigments, dyes, reinforcing inorganic or organic fillers such as talc, glass fibers, carbon fibers, glass balls, metallic particles and mixtures thereof.
  • the target polymer product provided with additives can be in the form of a pulverulent or granular material or can be processed in a further step to form a granulate.
  • the additive which may be incorporated into the target polymer product in accordance with the present invention is preferably a carbon black which may be added to the target polymer solution having a target polymer to solvent ratio of from 1: 0.5 to 1 : 4 parts by weight.
  • the proportion of the carbon black in the soot-containing target polymer is more than 50% by weight, preferably 60% by weight and more than 60% by weight, based on the total weight of the target polymer, additive and residual solvent.
  • preferably 51 to 70% by weight of carbon black or even more than 70% by weight of carbon black can be introduced into the masterbatch from a polymer, in particular polyethylene.
  • the masterbatch can be present as a target polymer product according to the invention as a pulverulent material or can be processed into a granulate in a further step.
  • a type of carbon black can be used as additives with which an electrically conductive plastic can be produced, for example PEel, conductive polyethylene. Due to their fine powderiness, these types of carbon black can only be incorporated with great difficulty using conventional methods with high concentrations in plastics as an additive.
  • the additive introduced according to the invention may furthermore advantageously be fiber reinforcements which have a fiber length of about 1.5 to 6 mm.
  • the open and loose structure and the high melt flow index of the target polymer products according to the invention allow a particularly gentle admixture of the fibers, which allows the incorporation of fillers with particularly long fibers. With the polymer granules of the prior art usually fibers with a maximum length of up to 1, 5 mm can be introduced.
  • the subject of the present invention is also a target polymer product which can be reinforced with fibers having a length of 1.5 to at least 6 mm.
  • the process can be carried out with polar target polymers as with nonpolar target polymers, since, in particular, the essential function of the water vapor to form gas bubbles in the target polymer solution are independent of the physical and chemical properties of the individual target polymer.
  • the recycling of polyolefins, such as polyethylenes and polyphenylenes, by the process according to the invention is particularly preferred in order to prepare corresponding target polyolefin products.
  • all solvents can be used according to the invention, which are given above for the dissolution of nonpolar polymers.
  • the inventors have found that the recycling of polyethylenes is particularly preferably carried out under the temperature conditions mentioned in the exemplary embodiment, and that for the recycling of polypropylenes, the solution / process temperature in about 20 to 30 ° C higher than polyethylene should be.
  • the process is preferably carried out with hot steam, which may be wet steam, superheated steam or saturated steam, with hot steam being preferred.
  • the steam at atmospheric pressure can have a temperature in the range from 100 to 250.degree. C., preferably from 120 to 200.degree. C., particularly preferably in the range from 140 to 180.degree. At other pressure conditions correspondingly different temperatures may be present.
  • the temperature of the water vapor may be at or just above the boiling point of the solvent, which may result in the solvent also boiling.
  • the evaporation rate can also be adapted to the design of an evaporation device.
  • the invention further relates to a system for carrying out the method.
  • An embodiment of this system is shown schematically in Fig. 2.
  • the dissolution of the target polymer can for example be distributed to two process vessels 1, 2, wherein in the first process vessel 1 a first target polymer solution is obtained and in the second process vessel 2 the insoluble constituents from the first process vessel 1 with fresh solvent seffen be brought into contact; the process containers 1, 2 are heated, for example, with steam from the steam boiler system; the mixture of the target polymer and solvent is permanently pumped around in the container 1, 2 in order to accelerate the dissolution process via the resulting friction; by pumping the dissolution of the target polymer can be achieved without the installation of a mechanical stirrer;
  • a conveyor screw 5 for filling the process containers 1, 2 with unmixed target polymer or with a composite material containing the target polymer in combination with insoluble constituents;
  • a pump for pumping out the insoluble constituents of a composite material from the process containers 1, 2, which remain after the selective dissolution of the target polymer;
  • One or more devices for processing the insoluble components such as centrifuges, screw conveyors for removing the centrifuged insoluble constituents, vacuum dryers, solid dryers, as well as a filling device, when the insoluble constituent is a single-grade polymer, the should be packaged after drying and put on the market;
  • the target polymer solution is brought into contact with hot steam and the solvent is expelled continuously by the hot steam, whereby a highly viscous target polymer solution is obtained;
  • the hot steam is preferably introduced into the feed pipe 9 through which the target polymer solution is fed, or introduced directly into the head region 10 of the falling film evaporator 7, 8; in the region of the closed head 10 or distributor head of the falling film evaporator 7, 8, the pressure is about 2 bar, in the bottom outlet 11, 12 at 1, 2 bar to 1 bar;
  • the target polymer solution is further heated by the water vapor and enriched with water vapor bubbles into which the solvent evaporates; the formation of the gas bubbles increases the evaporation surface in the case film evaporators many times over;
  • a Fleizvortechnisch 13, 14 for heating the falling film evaporator 7, 8 can be introduced into the hot steam from the boiler plant.
  • One or more thin film evaporator 15 in which the highly viscous liquid from the falling film evaporators 7, 8 is passed, in which 10 hot steam is passed into the product stream in the head area to drive off a solubilizer ittel-water vapor mixture and the target polymer in the in thin-film evaporator 15 to obtain high temperature as granular or powdery material;
  • the principle is also used in the thin film evaporator 15 to form a large amount of fine steam bubbles by introducing steam, into which the solvent can evaporate;
  • the suspension if appropriate mixed with the additive (s), is concentrated; the thin film evaporator 15 applies the mixture to the wall via its scrapers;
  • the product guide is preferably in three parts: in the upper area, the wall is heated, whereby the mixture remains liquid; two further heating stages heat the material until the material granular or powdered. This process takes place at a vacuum of 0.5-0.9 bar.
  • a heating device for heating the thin-film evaporator 15, in the hot steam can be introduced from the steam boiler system.
  • an extruder 30 with a distillation zone for discharging outgoing solvent and / or water.
  • one or more heatable drying devices such as a drying screw, not shown, in which the solid granular or pulverulent target polymer leaving the extruder is further dried with heating, but without the supply of steam (step c), to a granular or powdered dried one Target polymer is obtained;
  • a receiver tank 18 for the thin film evaporator 15 in which the target polymer solution and the solution or suspension of the additive or additives are mixed, after which the mixture obtained is conveyed into the thin film evaporator 15;
  • a control device which is provided as necessary for controlling the individual Analgenkompo- nenten. It can have one or more control components, in particular one or more networked or mutually independent digital components, in particular programmable computers. It can also have analog electrical and optionally also mechanical components. It has sensors for recording process and process parameters, which are connected to the control components, and actuators for influencing them (control, regulation) according to the results of the control components.
  • One or more memories may be provided to store process data and / or program data and / or control parameter data.
  • One or more operator interfaces may be provided for process control and management and for data and program maintenance. The interfaces may be designed for operators or for communication with other or higher ranking automatic components. Electrical or digital control components can be located locally directly on the system components and / or more remotely and via lines or networks (LAN, WLAN, Bluetooth, Internet,...) With local digital components and / or sensors and / or Actuators connected.
  • the vapor water and the water-solvent vapor to be condensed can be discharged.
  • the condensate of water and solvent forms two separate phases when water and solvent are not miscible with each other. If the solvent is lighter than water, it is separated as the supernatant of the two-phase system. Both phases can be recycled back into the process.
  • Some or all of the containers and lines may be closed and under pressure, preferably overpressure. On the other hand, the essential process steps can also take place at atmospheric pressure.
  • the system can be closed and filled with inert gas.
  • the process is preferably carried out continuously.
  • the process may provide that the solvent is expelled with hot steam from a target polymer solution in a falling film evaporator, the water vapor transferring both the head of the falling film evaporator to the target polymer solution. is introduced as well as in the bottom of the falling film evaporator in countercurrent to the flowing liquid is applied to the liquid film.
  • a resulting solvent-containing polymer product in particular polyolefin, especially polyethylene, with or without additive additive, is dried to such an extent that its residual content of solvent is in the range from 1 to 7% by weight, preferably 3 to 5% by weight. It was found that with a virgin product of the polymer, which contains no solvent, the MFI MFI is about 5, while for a polymer product with the above-mentioned solvent content, an MFI value of about 10 is obtained. The higher MFI value corresponds to higher fluidity of the polymer melt, resulting in better extruder processability and other advantages for applications listed above.
  • the invention finally relates to the use of from 1 to 7% by weight of solvent, preferably from 3 to 5% by weight of solvent, in an additive-free or additive-containing polymer product for improving the melt flow index over the pure polymer.
  • FIG. 1
  • Fig. 3 shows schematically an extruder
  • Fig. 3 shows an extruder 30, as shown schematically in Fig. 2 bottom left in the overall system.
  • the various arrows 37a, 37b, 37c and 37d symbolize material flow directions, namely 37a the direction of the incoming Material, 37b the main material flow within the extruder, 37c the effluent and 37d distilled solvent or water.
  • the extruder 30 has an extruder body 31 with a material inlet 32 at the upstream end of the body 31 and a material outlet 33 at the downstream end.
  • 35 symbolizes a worm rotating in the body 31 with a worm core 35a and a spiral worm 35b.
  • the envelope surface of the outer dimension of the rotating Schneckenplanetaryis 35b may be viewed in the radial direction at least partially form-fitting with the inner peripheral surface of the surrounding recess in the body 31 or may be compared to its slightly reduced, about max. 2mm or max 1mm or max. 0.5 mm in the radial direction.
  • 34 is a drive for the screw, which rotates the screw in such a way that the flow of material along arrow 37b is effected.
  • the screw core 35a may have a constant or non-constant diameter over its length, and that the helical pitch may also be constant or variable over the length of the screw.
  • distillation areas With 36a to 36d several (concrete: four) distillation areas are drawn. Quite generally, at least one of them is provided, but two, three, four, five, six or even more distillation regions may also be provided along the material flow according to arrow 37b and be one behind the other in the transport direction 37b and delimited from one another.
  • the extruder 30 receives the mixture to be treated of target polymer, solvent and optionally other substances, including water from previous process steps.
  • the system control or design is such that at the inlet 32 viscous material (such as honey-like) is supplied. Expressed in figures, it can contain from 10% to 50% of solvent (and possibly water) at the inlet. based on the total weight including additives or without additives, the percentage being based on weight. Preferably, values between 15% and 35% are used, more preferably between 20% and 25% at the material inlet. It should be noted here that at the outlet residual moisture between 0.1% and 5% can be present, preferably 0.2% to 2%, more preferably 0.5% to 1%. Again, the percentages are by weight and in terms of the proportion of solvent and optionally water based on the total weight with or without additives.
  • the design of the screw 35 may be such that at the inlet 32, the screw is self-tightening, or the material may be forcibly inserted at the inlet 32.
  • the driven screw 35 causes the material in the extruder body 31 is transported along arrow 37b, in the drawing of Fig. 3 as to the right. It happens in this way the distillation region 36a to 36d.
  • One of these areas, namely 36a, is shown schematically in FIG.
  • a plastically deformable polymer material can be present, which has a very low residual moisture content or a residual moisture of a desired value or within a desired value range, for example for further processing in other machines or equipment.
  • the material may then finally be extruded at the outlet 33, for example as an initially continuous strand of the material having the desired cross-sectional shape. But it can also right here at the outlet another
  • the extruder may have at the outlet a single opening or a plurality of parallel, from which extruded parallel strands of material.
  • the inlet of the extruder 30 may receive material from a thin film evaporator 15 or from a falling film evaporator 13, 14.
  • the exit of the extruder 30 may be connected to other equipment, such as a drying screw (not shown) for further drying of the extruded material, or a mill 21 or the like.
  • FIG. 4 shows schematically a distillation region 36a. It has an opening 47 in the wall 31 of the extruder body. Preferably, the opening 47 is up (with respect to the direction of gravity) so that material does not flow away.
  • An attachment 41 is provided which leads away from the housing wall 31 radially with respect to the screw rotation and which can be provided with a distal flange 42.
  • the extruder 30 is a closed system without immediate external or external access.
  • the distillation regions 36 can also be closed regions.
  • At the neck 41 and flange 42 may be attached at example as a domed dome or coupling 43, which in turn has a nozzle 44 to which a line 45 can begin.
  • the dome 43 is used for collecting and guiding the emerging material (solvent and, if necessary, water, vapor or already liquid), and nozzle 44 and line 45 serve its derivation.
  • water and / or solvents are gaseous / vaporous emerge from the material and then discharged through port 44 and line 45.
  • This can be done passively by adjusting the steam pressure according to the pressure conditions along arrow 37d on the nozzle 44 to line 45 wanders. Or it can be actively sucked / sucked off.
  • 46 symbolizes the existing and transported material in the extruder.
  • 46a is the surface of the material in the distillation region 36a. It can be seen that the volume 48 bounded in the distillation zone is not completely occupied by the material 46. Rather, free volume is present, which is intended to increase the exposed surface 46a of the material 46, so that corresponding residual moisture from the material 46 can evaporate, similar to a distillation. It may be provided in a distillation area a not shown level sensor. The system parameters can be controlled or regulated in such a way that the complete filling of the free volume of the distillation zone 36 is avoided or that a desired fill level is not exceeded.
  • the evaporation or distillation effect can be increased by providing a heater 49, indicated only schematically, which heats the material 46 in the distillation region 36 or upstream thereof.
  • the heating can work electrically or by means of radiation (microwaves) or via a heat exchanger.
  • kneading devices 50 can be provided, which mix the material 46 kneading.
  • a kneader 50 may be provided outside of a distillation zone 36, such as upstream thereof, and / or within a distillation zone 36.
  • the worm core is symbolized, with 35b the worm spiral.
  • Their design may be such that at the downstream end of a distillation zone 36a the screw is self-withdrawing and therefore reliably removes material 46 from the distillation zone 36, thus ensuring that the flow is maintained. Lumen 48 in the distillation section 36 is not filled with material 46.
  • the desired transport properties of the screw can be designed by variable design of the core diameter and / or the outside diameter and / or the pitch of the screw.
  • the conduit 45 may be a rigid conduit or a hose. It may, for example, lead to a condenser in which the derived vapors are condensed to liquid. However, the line 45 can also lead, for example, directly into a storage store of raw material to be dissolved, so that it is directly dissolved by solvent vapors there.
  • the extruder does not operate at negative pressure or only slightly below the atmospheric pressure (not below 500 hPa). Insofar as the vapors emerging in the distillation zone 36 are sucked off, small underpressures (not below 500 hPa) may result.
  • the extruder places the material in areas under overpressure (vs. atmospheric pressure), at least at the outlet to extrude the residual material.
  • an additive is added in the extruder and mixed with the other material.
  • a separate inlet (not shown) may be provided for this purpose, or the additive may be added via the already mentioned inlet 32 as the main material. It then takes place by means of the screw 35 and possibly the kneading device 50, a mixing of the materials, so that the additive at the outlet 33 of the extruder is intimately and homogeneously mixed with the other material and mixed.
  • the extruder may include a controller, not shown. It can be connected on the input side with sensors on the extruder or elsewhere in the process and / or on the output side with actuators on the extruder.
  • the sensors can be one or more temperature sensors, possibly over the length of the extruder or distributed over the plurality of distillation regions, have, and / or one or more residual moisture sensors, possibly also distributed over the length of the extruder or over the plurality of distillation regions, and / or one or more level sensors approximately at a distillation region 36, possibly also over the length of the extruder or distributed over the multiple distillation zones.
  • the actuators may be the heater 49 and / or the kneading device 50 and / or the extruder drive 34 and / or a material feed, not shown. Elements of the actuators can be actuated in accordance with signals from the sensor. For example. If desired, the heating and / or the drive speed can be set in accordance with the residual moisture measured at the extruder output, and / or the material feed can be operated in accordance with a measured fill level.
  • the control can be provided separately for the extruder or be part of the entire system control.
  • an extruder is used to extrude a solution received on the inlet side towards the outlet and thereby to divert residual moisture from the solvent and optionally also water into the distillation zones.
  • the material can be heated or kneaded through , It can pass several distillation areas.
  • the method comprises supplying input material of said input composition with respect to water, solvent and target polymer and optionally filler, and operating the extruder to produce material having the desired starting composition. There may be added a filler / additive. In the same way, however, the material supplied to the extruder may already have added additives (for example in the falling-film evaporator or in the thin-film evaporator).
  • the extruder In accordance with the residual moisture measured at the extruder outlet, it is possible to heat and / or set the drive speed, and / or the material supply (amount per time) can be operated or adjusted in accordance with a measured fill level. It may be preferred for the extruder to process material without fillers / additives, ie, apart from impurities, a mixture only of solvent and dissolved agent and optionally water. However, the extruder can also receive material already provided with fillers / additives and / or mix in the filler / additives themselves. It may then be desirable to have mixtures with not too large amounts of fillers / additives at the end, for example with a share of the total weight of more than 0.1% or more than 1% but less than 20% or less than 10%.
  • the process comprises a first stage in which a polyethylene product is recovered using the process of the invention from a multilayer film having a polyamide layer and a polyethylene layer, and a second stage wherein carbon black can be added to the polyethylene product.
  • the PA-PE multilayer film is destroyed by granulation to make the polyethylene more accessible to the dissolution process. As comparative tests have shown, the granules are dissolved much easier than chips from the PA-P multi-layer film.
  • the PA-PE granulate is subsequently conveyed by means of a conveyor screw 5 into the process vessel 1 in FIG. 2, which is kept at a temperature of 100 ° C.-120 ° C. with hot steam 19.
  • Type 4 white spirit is heated to 120 ° C in the solvent reservoir 4 and then injected into the 1, where it dissolves the polyethylene from the granules at a temperature of 100-120 ° C. The temperature is kept at 100-120 ° C by hot steam.
  • the contents of process container 1 are constantly pumped around.
  • the associated movement replaces the agitator and speeds up the dissolution process.
  • a solution is obtained which contains 90% of the submitted polyethylene in dissolved form.
  • the polyethylene solution is prepared using 1 part by weight of polyethylene and 8 parts by weight of testbenzene.
  • the insoluble in the white spirit polyamide settles quickly with not yet dissolved polyethylene at the bottom of the process container 1.
  • the polyethylene solution forms the supernatant and is pumped off into a collecting container. In the continuous process, the dissolving process is repeated every 30 min with a new batch of the processed PA-PE multilayer film.
  • the suspension of polyamide particles, undissolved polyethylene and polyethylene solution obtained at the bottom of process vessel 1 is pumped into a further process vessel 2 in which polyethylene which has not yet been dissolved is dissolved out with fresh white spirit at 100-120 ° C.
  • the container contents are pumped here too.
  • the ratio of solid-open to solvent is 1 to 3.
  • the polyethylene solution is combined with the main solution in the sump.
  • the suspension of polyamide particles in white spirit is pumped onto a dewatering screw 20, rinsed again with 100-120 ° C hot white spirit, to obtain a material which consists of 98% polyamide with a residual content of polyethylene.
  • the suspension is centrifuged, the precipitated polyamide is rinsed with water vapor at a temperature of 150 °, then removed from the centrifuge and placed in a heated screw conveyor.
  • the heating of the screw conveyor serves to evaporate the solvent, which is amplified by a stream of hot air.
  • the polyamide is fed to a vacuum dryer in which a last time on Polyamide adhering white spirit is removed with 150 ° C hot steam and then the predrying of the polyamide at 130 ° C in vacuo. After further drying in a solids dryer, the granular polyamide can be filled into sacks for further use.
  • the condensates produced in the various process steps are conveyed into a settling tank.
  • the solvent precipitates at a density of 0.7 g / cm 3 as the top layer.
  • An intermediate layer consists of entrained polymer particles with a density of 0, 9 g / cm3, which is deposited.
  • the lower layer consists of water with a density of 1, 0 g / cm3. All three phases are returned to the manufacturing process.
  • the polyethylene solution freed of polyamide in the collecting container 6 is kept at a temperature of 90 ° C. by means of hot water in an external heating device.
  • the polyethylene solution is passed through an inlet pipe 9 in the head portion 10 of a falling-film evaporator 7, which comprises 96 tubes, with the aid of hot water vapor, which flows at a pressure of 0.9 bar through tubes 13, at a temperature of 140 ° C. being held.
  • the head region 10 is filled with the target polymer solution to ensure uniform filling of the 96 tubes.
  • high-pressure steam at a temperature of 160 ° C. is introduced via one or more nozzles, which also reduce the pressure, preferably with the stream, if appropriate additionally in countercurrent to the stream of the polyethylene solution.
  • the hot steam heats the polyethylene solution and, at initiation, results in the formation of vapor bubbles and bubbles in the target polymer solution into which the solvent evaporates.
  • the water vapor can with another gas, eg. B. inert gas, nitrogen) are introduced mixed.
  • the introduction mechanism may be designed to optimize bubble formation, such as by having a high number of relatively small cross-section nozzles (n> 5 or> 10 or> 20) submerged in the solution.
  • the orientation of the nozzles ie the fluid stream out of them) can be parallel. But you can at least partially not in pairs not parallel or intersecting.
  • the steam injection can z. B. in a solution supply line for the solvent / PE solution of an evaporator, for example shortly upstream of the Zulei- end.
  • the heated polyethylene solution mixed with the steam and enriched with steam and optionally gas bubbles enters the 96 tubes of the falling-film evaporator 7 and flows as a thin film on the heated surface of the tubes 13 in the direction of the bottom draw 11 of the falling-film evaporator 7. Under these conditions A mixture of test gasoline vapors and water vapor is expelled and water molecules are embedded in the polyethylene structure.
  • the temperature, due to the external Fleizung and the hot steam, and the properties of the solvent and polymer are such that halved until the bottom take-off 11 of the falling film evaporator 7, the amount of solvent.
  • the vapor is separated from the liquid with a separator and fed to the condensation and recovery of water and solvent.
  • the ratio of polyethylene to white spirit is then 1: 4.
  • the concentrated heated polyethylene solution is passed into a second falling-film evaporator 7 whose construction is identical to the construction of the first falling-film evaporator 7.
  • the hot steam at a temperature of 140-160 ° C in the head portion 10 of the falling-film evaporator 8 is introduced, which leads to further heating of the target polymer solution and the accumulation of glass bubbles in the target polymer solution, which increase the evaporation surface.
  • the water vapor bubbles accumulate with solvent.
  • the weight-related quantitative ratio of polyethylene to white spirit is 1: 1.
  • the vapor is separated from the liquid with a separator and fed to the condensation and recovery of water and solvent.
  • the solution is much more viscous, similar hot honey. When this highly viscous solution is cooled, a waxy solid is obtained, which is easily crumbled mechanically.
  • a concentrated slurry of carbon black in white spirit is prepared.
  • the carbon black may be a carbon black type for coloring and / or a carbon black grade for obtaining electrical conductivity in the polyethylene. Soot and white spirit are mixed.
  • the temperature is adjusted to 160-180 ° C with hot steam.
  • the polyethylene solution from the second falling-film evaporator 8, with a ratio of 1: 1 (target polymer: white spirit) and the carbon black suspension from the additive container 17, are combined in a mixing device 18 with the addition of hot steam and mixed.
  • the viscous polyethylene solution enriched with carbon black is then introduced into a thin-film evaporator 15. Hot water vapor at a temperature of 140-160 ° C is passed into or over the product stream.
  • the thin film evaporator 15 itself is heated with hot steam of 140 ° C at a slight negative pressure of 0.9 bar, which flows through a piping system in the thin film evaporator 15.
  • a mixture of water vapor and test gasoline vapor is expelled until the liquid content of the target polymer is only 10-20 wt .-%.
  • the soot-containing polyethylene is present as a black crumbly polyethylene having a carbon black content of 60% by weight.
  • the mixture is then added to the described extruder 30 and further processed as described.
  • the masterbatch of polyethylene and trapped soot is transported to a mill 21.
  • the masterbatch is crushed and discharged via a screw 22.
  • the masterbatch is dried at 100 ° C to a residual moisture content of solvent and possibly water of 3-5%.
  • the masterbatch with a residual solvent content of 3-5% is then fed to the final granulation process.
  • the residual moisture increases the melt flow index of the masterbatch in the screw from 5 to 10, which facilitates the incorporation of the carbon black into the polyethylene while optimally distributing the carbon black and improving granule formation.
  • the masterbatch in granular form with a carbon black content of 60% by weight.
  • the masterbatch may be dried as a target polymer product not in granule but in powder form, which may have advantages when used as a masterbatch.
  • Feature combinations K1 ff which may be in connection with the extruder, the described plant and the process, can be described as follows:
  • a method of making a target solid polymer product from a target polymer solution comprising the steps of: a) preparing the target polymer solution by dissolving the target polymer in a solvent or leaching the target polymer with a composite or mixture solvent and separating the target polymer solution from the target polymer insoluble constituents, b) concentrating the target polymer solution, which has a temperature of at least the boiling point of water, by contacting the target polymer solution.
  • Method according to K1 or K2 characterized in that the quantitative ratio of target polymer to solvent in the process steps independently of one another in the following ranges: - before step b) in the range from 1: 5 to 1: 20 parts by weight, - after Step b) and before step c) in the range of 7 to 16 wt .-% solvent at an additional water content of 2 to 8 wt .-% and - after step c) in the range of 1 to 7 wt .-% solvent.
  • Step b) in one or more falling-film evaporators (7, 8) and / or one or more thin film evaporators (15) is performed.
  • K5. Method according to K4, characterized in that in the one or more falling film evaporators (7, 8) so much solvent is driven off that the quantitative ratio of target polymer to solvent is in the range from 1: 0.5 to 1: 4 parts by weight, and that enough solvent is expelled in the thin film evaporator (s) (15) such that the target polymer solution contains from 7 to 16 percent by weight of solvent, based on the total weight of the target polymer and solvent.
  • Method according to one of the preceding K characterized in that in the implementation of step b) an additive or a mixture of additives is added, wherein the additive or the mixture of additives - is added to the target polymer solution, as soon as by the evaporation of Solvent, the ratio of target polymer to solvent has risen to a value in the range of 1: 0.5 to 1: 4 parts by weight or - is mixed into the target polymer solution before it is introduced into the first thin film evaporator (15). 7.
  • Method according to one of the preceding K characterized in that after step b) and before step c) and / or after step c) a further additive or mixture of additives is added.
  • K8 Process according to K6 or K 7, characterized in that the additives are solid additives selected from carbon blacks, organic pigments, inorganic pigments, dyes, reinforcing fillers such as talc, glass fibers, carbon fibers, glass balls, metallic particles and mixtures thereof where the additive or mixture of additives is in solid form, in liquid form, as a suspension or as a solution.
  • the additives are solid additives selected from carbon blacks, organic pigments, inorganic pigments, dyes, reinforcing fillers such as talc, glass fibers, carbon fibers, glass balls, metallic particles and mixtures thereof where the additive or mixture of additives is in solid form, in liquid form, as a suspension or as a solution.
  • K10 Method according to one of the preceding K, characterized in that the target polymer is a polyolefin.
  • K11 Method according to one of the preceding K, characterized in that the solvent is selected from fatty acid esters, petroleum fractions, gasoline fractions, diesel fuels, aliphatic hydrocarbons, alicyclic hydrocarbons, aromatic hydrocarbons, individually or in a mixture.
  • K13 Method according to one of K1 to K11, characterized in that the solvent is biodiesel with a boiling range of about 300 to 570 ° C, rapeseed oil, fuel oil with a boiling range of 170 to 390 ° C, diesel fuel with a boiling range of 170 to 390 ° C, white spirit of type 1 (boiling range 130-185 ° C), type 2 (boiling range 140-200 ° C), type 3 (boiling range 150-190 ° C), type 4 (boiling range 180-220 ° C) and Type 5 (boiling range 130-220 ° C), Type 2 boiling-point petrol (boiling range 80-110 ° C), Type 3 boiling-point benzene (boiling range 100-140 ° C), petroleum benzine with a sieving range of 80 to 110 ° C, aliphatin having a boiling range of 100 to 160 ° C, ligroin having a boiling range of 150 to 180 ° C,
  • K15 Method according to one of the preceding K, characterized in that the target polymer solution in step b) is additionally heated by one or more heating devices (13, 14).
  • K16 Method according to K15, characterized in that the evaporation surfaces of the falling film evaporators (7, 8) and / or the thin film evaporator (15) are kept at a temperature of 80 to 200 ° C.
  • K17 Method according to one of K4 to K16, characterized in that the hot water vapor in the feed line (9) to the falling film evaporator (7, 8) or in the head region (10) of the falling film evaporator (7, 8) is introduced into the target polymer solution and in water vapor bubbles are formed in the target polymer solution into which the solvent evaporates, thereby increasing the overall evaporation surface area.
  • the solvent has a boiling temperature in the range of 180 to 220 ° C
  • the target polymer is dissolved in the solvent at 50 to 150 ° C
  • the target polymer solution in the one or more falling film evaporators and / or the one or more thin film evaporators is mixed with high pressure steam at a temperature of 140 to 180 ° C to expel a solvent-vapor mixture
  • the one or more falling film evaporators and / or the one or more thin film evaporators additionally externally with steam at a temperature heated from 120 to 140 ° C.
  • K20 Additive-free or additive-containing target polymer product, obtainable by the process according to one of K1 to K19.
  • K21 A target polymer product as a masterbatch comprising a polymer and carbon black, wherein the carbon black content is at least 51% by weight, based on the total weight of the masterbatch, preferably at least 60% by weight.
  • Target polymer product as a masterbatch, which comprises a polymer and color pigments and has a granular or powdery structure.
  • a target polymer product as a fiber-reinforced compound material comprising a polymer and, among other additives, fibers having a length of at least 2 mm.
  • Additive-free or additive-containing polymer product having a solvent content of 1 to 7 wt .-%, preferably 3 to 5 wt .-% to improve the melt flow index.
  • K26 Device for carrying out any of the above methods without mechanical stirrers, comprising: - one or more process containers (1, 2) for the preparation of the target polymer solution, in which the solution is circulated by pumping,

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Abstract

L'invention concerne une extrudeuse (30) comprenant un boîtier (31), une première entrée de matière (32) destinée à un mélange (46) au moins constitué d'un solvant et d'un agent dissous, une sortie de matière (33), une vis (35) tournant dans le boîtier, un entraînement de vis (34) et au moins un intervalle de distillation (36a-d) entre l'entrée (32) et la sortie (33), qui permet l'évacuation du solvant, et une conduite d'évacuation (43 –45) destinée au solvant.
EP19705143.6A 2018-02-08 2019-02-07 Extrudeuse, système comprenant une extrudeuse, procédé de production de produits polymères cibles à partir d'un matériau contenant du plastique à partir d'une solution à l'aide d'une telle extrudeuse Pending EP3749499A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102018102811.3A DE102018102811A1 (de) 2018-02-08 2018-02-08 Extruder, Anlage mit einem Extruder, Verfahren zur Herstellung von Zielpolymerprodukten aus einem kunststoffhaltigen Material aus einer Lösung unter Verwendung eines solchen Extruders
PCT/EP2019/052960 WO2019154889A1 (fr) 2018-02-08 2019-02-07 Extrudeuse, système comprenant une extrudeuse, procédé de production de produits polymères cibles à partir d'un matériau contenant du plastique à partir d'une solution à l'aide d'une telle extrudeuse

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EP3749499A1 true EP3749499A1 (fr) 2020-12-16

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US (1) US11931921B2 (fr)
EP (1) EP3749499A1 (fr)
CA (1) CA3090733A1 (fr)
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WO (1) WO2019154889A1 (fr)

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US11931921B2 (en) 2024-03-19
US20210008763A1 (en) 2021-01-14
DE102018102811A1 (de) 2019-08-08

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