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CN115181358A - Waste polyester-cotton fabric modified and reinforced polypropylene composite material and preparation method thereof - Google Patents

Waste polyester-cotton fabric modified and reinforced polypropylene composite material and preparation method thereof Download PDF

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Publication number
CN115181358A
CN115181358A CN202210754907.1A CN202210754907A CN115181358A CN 115181358 A CN115181358 A CN 115181358A CN 202210754907 A CN202210754907 A CN 202210754907A CN 115181358 A CN115181358 A CN 115181358A
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fiber
modified
regenerated
polypropylene
polyester
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CN115181358B (en
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郭阳光
韦啸
明星星
冯刚
王志白
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Chongqing Changan Automobile Co Ltd
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Chongqing Changan Automobile Co Ltd
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    • 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
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
    • D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
    • D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
    • 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
    • C08J2323/10—Homopolymers or copolymers of propene
    • C08J2323/12—Polypropene
    • 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
    • C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
    • C08J2401/02—Cellulose; Modified cellulose
    • 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
    • C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2467/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/04—Vegetal fibres
    • D06M2101/06—Vegetal fibres cellulosic
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32—Polyesters
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
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  • Manufacturing & Machinery (AREA)
  • Textile Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
  • Reinforced Plastic Materials (AREA)

Abstract

The invention relates to waste clothes recycling, in particular to a modified and reinforced polypropylene composite material of waste polyester-cotton fabrics and a preparation method thereof. The invention aims to provide a new choice for recycling waste polyester cotton. The technical scheme of the invention is that the waste polyester-cotton fabric modified reinforced polypropylene composite material comprises the following raw materials in parts by weight: 10-40 parts of regenerated modified polyester staple fiber, 0.1-3.0 parts of antioxidant and toner, and the balance of polypropylene PP resin; the polypropylene resin is polypropylene with the material flow speed of 0.5-120 g/10min under the conditions of 230 ℃ and 2.16 Kg. The polyester staple fibers extracted from waste polyester cotton fabrics are applied to polypropylene materials for modifying the interior and exterior trim of automobiles to prepare the regenerated polyester staple fiber reinforced polypropylene composite material with excellent performance, and the regenerated polyester staple fiber reinforced polypropylene composite material can be used for completely or partially replacing glass fiber or mineral reinforced polypropylene materials.

Description

Waste polyester-cotton fabric modified and reinforced polypropylene composite material and preparation method thereof
Technical Field
The invention relates to waste clothes recycling, in particular to a waste polyester-cotton fabric modified and reinforced polypropylene composite material and a preparation method thereof.
Background
Along with the continuous improvement of national economy and people's living standard in recent years, people have higher and higher requirements on clothing and replacement frequency, so that a large amount of waste clothes are generated, wherein the polyester-cotton blended clothes are deeply favored by wide consumers due to the characteristics of stiffness, smoothness, quick drying, wear resistance and the like, so that the polyester-cotton blended clothes account for a considerable proportion of the waste clothes, the recycling technology of the waste clothes in the world starts at present, and the waste clothes are used in fields with lower technical threshold and material performance requirements from the beginning of landfill or incineration. For example, patent CN201811149512.9 authorizes a waste sole regenerated rubber powder composite waste clothing regenerated fiber reinforced asphalt mixture and a preparation method thereof, and the asphalt mixture is prepared by mixing regenerated rubber powder modified asphalt, aggregate, waste clothing regenerated fiber and mineral powder. For example, patent CN202110613463.5 discloses a wood-plastic plate and a profile prepared by recycling waste clothes and a preparation method thereof, wherein the wood-plastic profile prepared by waste clothes is used, waste clothes fibers are used for replacing wood flour largely used by traditional wood-plastic products, and the fibers in the waste clothes are completely melted into organic materials through chain extension and compatibilization treatment to be extruded into the plate or the profile. But it is a research focus of many technologists on how to realize the higher value-added recycling of these waste clothes.
The automotive industry, as an important national economy industry, has adopted the low carbon, green cycle as an important direction and goal for future development of the automotive industry.
Disclosure of Invention
The invention aims to provide a new choice for recycling waste polyester cotton.
The technical scheme of the invention is that the waste polyester-cotton fabric modified and reinforced polypropylene composite material comprises the following raw materials in parts by weight:
10 to 40 portions of regenerated modified polyester staple fiber,
0.1 to 3.0 portions of antioxidant and toner,
60-90 parts of polypropylene resin;
the polypropylene resin is polypropylene with the material flow speed of 0.5-120 g/10min under the conditions of 230 ℃ and 2.16 Kg;
the antioxidant is at least one of an antioxidant 1010 (tetra (beta-3, 5-di-tert-butyl-4-hydroxyphenyl) pentaerythritol ester), an antioxidant 168 (tri (2, 4-di-tert-butylphenyl) phosphite) and an antioxidant DSTP (dioctadecyl thiodipropionate);
the toner is at least one of carbon black, titanium dioxide, iron oxide red and yellow; the purity of PET fiber in the regenerated polyester staple fiber is more than or equal to 90 percent, and the average length of the fiber is 0.5 mm-5.0 mm.
The invention also provides a preparation method of the polypropylene composite material, which comprises the following steps:
step s1, preparing regenerated modified polyester staple fibers: sequentially carrying out dry physical crushing, wet centrifugal separation, vertical gas cyclone separation and surface passivation modification treatment on the recovered pure polyester or polyester-cotton blended fabric to obtain regenerated modified polyester staple fibers;
step s2, preparation of the polypropylene compound: melting 10-40 parts of the regenerated modified polyester staple fiber obtained in the step s1, 0.1-3.0 parts of antioxidant and toner and the balance of polypropylene PP resin by a double-screw extruder, extruding, cooling and granulating to prepare a regenerated modified polyester staple fiber reinforced polypropylene composite modified material; the processing set temperature of the I-X area of the double-screw extruder is 135 ℃,165 ℃,180 ℃,190 ℃,200 ℃,210 ℃,215 ℃ and 220 ℃ in sequence, the rotating speed of the main screw is 300-500 r/min, and the temperature of the water tank is 23-50 ℃.
Specifically, in step s1, the operation of dry physical crushing is as follows: the recycled pure polyester or polyester-cotton blended fabric is cleaned by a clean water tank, is acidized by a sulfuric acid tank (removing impurities and softening the fabric for convenient subsequent crushing), is crushed for a plurality of times by a crusher after being dried, and then is crushed into a PET/cotton fiber flocculent mixture with the fiber length of 0.5 mm-5.0 mm.
Wherein the sulfuric acid pool is a dilute sulfuric acid solution with the concentration of 20-50 percent, and the treatment time is generally 4-12 h.
Preferably, the fiber length of the PET/cotton fiber flocculent mixture is 0.5 mm-1.5 mm.
In step s1, the operation of wet centrifugal separation is as follows: separating the PET/cotton fiber flocculent mixture into wet density of 1.38-1.41 g/cm by wet horizontal centrifugal equipment 3 The wet density of the PET short fibers is 1.50-1.58 g/cm 3 The cotton fiber of (2).
Further, in the step s1, a PET/cotton fiber flocculent mixture with PET purity of more than 93% is obtained after the separation treatment of the vertical gas cyclone.
In the step s1, roughening treatment is carried out on PET short fibers after vertical gas cyclone separation, surface treatment and passivation are carried out on the PET short fibers containing alkyl silane, and drying is carried out to prepare modified regenerated PET fibers; the aqueous alkali for the roughening treatment is NaOH solution with the concentration of 1-5 percent, the treatment temperature is 50-90 ℃, and the treatment time is 40-120 minutes; the alkylsiloxane solution.
The coarsening treatment is to use alkali solution to etch the surface of the fiber to be rough and uneven, and after the treatment is finished, the surface alkali solution is cleaned by clean water and then is dried.
Preferably, the alkylsiloxane is dodecane to octadecyltrimethoxysilane.
Preferably, the alkylsiloxane is hexadecyltrimethoxysilane.
Specifically, the passivation treatment temperature is 30-60 ℃.
The invention has the beneficial effects that: the invention starts from the development requirements of the automobile industry, overcomes numerous technical barriers through long-term research and exploration, starts from the treatment and fine inspection process of waste fabrics, combines the polyester fiber surface treatment and the polypropylene material modification processing technology, and finally successfully applies the polyester staple fibers extracted from the waste polyester cotton fabrics to the polypropylene material for the modification of the interior and exterior trim of the automobile to prepare the regenerated polyester staple fiber reinforced polypropylene composite material with excellent performance, which can be used for completely or partially replacing glass fibers or mineral reinforced polypropylene materials, and realizes the high added value reutilization of waste clothes while achieving the industrial appeal of low carbon and green cycle.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be emphasized that these examples are merely intended to further illustrate the present invention and should not be interpreted as limiting the scope of the invention. Further, it should be understood that various changes or modifications can be made to the present invention by those skilled in the art after reading the present specification, and these equivalents also fall within the scope of the present invention defined by the appended claims.
The high flow rate polypropylene in the following examples is preferably a medium petrochemical homopolypropylene resin having the M1200HS designation, which has a material flow rate of 12g/min at 230 ℃ and 2.16 Kg.
EXAMPLE 1 preparation of Polypropylene composite
1. The preparation treatment process of the regenerated modified polyester staple fiber comprises the following steps:
1. dry physical disruption stage
The recycled polyester or polyester-cotton blended fabric is cleaned, then moved into a sulfuric acid tank for acidification treatment (impurity removal and convenient subsequent crushing of softened fabric), dried after the treatment is finished, and then fed into a physical crusher for crushing treatment, and the crushing times are controlled during the treatment so that the length of the obtained fiber is 0.5-5 mm. The sulfuric acid pool is a dilute sulfuric acid solution with the concentration of 50 percent of sulfuric acid solution, and the treatment time is 4 hours.
2. Wet centrifugal separation
The dried material is physically crushedSeparating the PET/cotton fiber flocculent mixture obtained after the process treatment to obtain pure cotton fibers and regenerated PET fibers, and utilizing the wet density difference of the PET fibers and the cotton fibers and adopting wet horizontal centrifugal equipment to enable the wet density to be 1.38-1.41 g/cm 3 The wet density of the PET short fiber is 1.50-1.58 g/cm 3 The purity of the PET fibers before and after wet centrifugation is shown in Table 1 below, wherein the wet separation is preferably facilitated by a fibrous fluff mixture having a fiber length of 0.5mm to 1.5mm. The centrifugal equipment is a horizontal centrifuge, and the manufacturer is Zhang Jia gang city Zhuo navigation machinery Co., ltd, and the equipment model is GK800.
TABLE 1 average purity of PET fibers before and after centrifugation for different fiber lengths
Figure BDA0003722107210000031
3. Vertical cyclone gas separation
The fiber flocculent mixture after wet process treatment is further separated by a vertical gas cyclone separation device (HCXF-800 cyclone separator of the environmental protection machinery Co., ltd. Of the North and Hebei Proc.). The dried fiber flocks enter the equipment through an inlet at the left side of the equipment, are fine under the pushing of rotating air in the equipment, uniformly dispersed fiber particles are directly rotated by 90 degrees and are output from the upper end of the equipment, and large and coarse non-separated fiber clusters, related metals and other impurities are removed from the bottom of the equipment along with the two sides of the equipment.
As can be seen from the table 2, through the process, on one hand, PET/cotton fiber flocks which are not separated by a wet separation process can be further cleaned from the fiber flocks, the purity of the PET fiber flocks is further improved, and simultaneously, lump dispersed terylene/cotton fiber entanglement which is removed in the processes of dry physical crushing and wet centrifugal vertical separation can be effectively removed, the crude terylene/cotton fiber entanglement which is not separated by the previous dry-method and wet-method processes is removed, and the purity of the PET fiber flocks can be further improved while the cotton fiber entanglement or the terylene fiber entanglement is removed, so that the performance of the subsequent terylene fiber modified polypropylene material is further improved.
TABLE 2 average purity of PET fibers before and after vertical gas cyclone separation Process
Figure BDA0003722107210000041
4. Surface passivation modification treatment of regenerated polyester staple fiber
In order to further improve the performance of the subsequent polyester fiber modified polypropylene material, the PET short fiber after being carefully selected by the vertical gas cyclone separation process is etched by a surface 3 percent NaOH solution, treated at 60 ℃ for 90 minutes, cleaned by clear water, dried, and then subjected to surface treatment passivation by hexadecyl trimethoxy silane at 60 ℃, and dried to prepare the modified regenerated PET fiber with the surface polarity close to that of PP resin. Selecting modified polyester staple fiber with the content of the polyester/cotton fiber controlled at 99.5/0.5% and the average length of 0.5mm for later use.
2. The preparation method of the regenerated modified polyester staple fiber reinforced polypropylene compound comprises the following steps:
according to the weight parts, the regenerated modified polyester staple fibers, the antioxidant, the toner and the polypropylene resin prepared in the step one are melted by a double-screw extruder, extruded, cooled and cut into particles to prepare the regenerated modified polyester staple fiber reinforced polypropylene composite modified material, and relevant material performance evaluation is carried out.
The processing set temperature of the I-X area of the double-screw extruder is 135 ℃,165 ℃,180 ℃,190 ℃,200 ℃,210 ℃,215 ℃,215 ℃ and 220 ℃ in sequence. The rotation speed of the main screw is set to 400r/min, and the temperature of the water tank is 40 ℃.
EXAMPLE 2 preparation of Polypropylene composite
1. The preparation treatment process of the regenerated modified polyester staple fiber comprises the following steps:
1. dry physical crushing stage
The recycled polyester or polyester-cotton blended fabric is cleaned, then moved into a sulfuric acid tank for acidizing treatment (impurity removal and convenient subsequent crushing of softened fabric), dried after the treatment is finished, and then fed into a physical crusher for crushing treatment, and the crushing times are controlled during the treatment so that the length of the obtained fiber is 0.5-5 mm. The sulfuric acid pool is a dilute sulfuric acid solution with the concentration of the sulfuric acid solution being 30 percent, and the treatment time is 8 hours.
2. Wet centrifugal separation
Separating the PET/cotton fiber flocculent mixture obtained after the dry physical crushing process to obtain pure cotton fibers and regenerated PET fibers, and utilizing the wet density difference of the PET fibers and the cotton fibers and adopting wet horizontal centrifugal equipment to enable the wet density to be 1.38-1.41 g/cm 3 The wet density of the PET short fibers is 1.50-1.58 g/cm 3 The cotton fibers are separated.
3. Vertical gas cyclone separation
Drying the fiber flocculent mixture treated by the wet process, and further separating by a vertical gas cyclone separation device. The dried fiber flocks enter the equipment through an inlet at the left side of the equipment, are fine under the pushing of rotating air in the equipment, uniformly dispersed fiber particles are directly rotated by 90 degrees and are output from the upper end of the equipment, and large and coarse non-separated fiber clusters, related metals and other impurities are removed from the bottom of the equipment along with the two sides of the equipment. The fibres with a length of 1.5mm are selected for use.
4. Surface passivation modification treatment of regenerated polyester staple fiber
In order to further improve the performance of the subsequent polyester fiber modified polypropylene material, the PET short fiber after being carefully selected by the vertical gas cyclone separation process is etched by a surface 3 percent NaOH solution, treated at 60 ℃ for 90 minutes, cleaned by clear water, dried, and then subjected to surface treatment passivation by hexadecyl trimethoxy silane at 50 ℃, and dried to prepare the modified regenerated PET fiber with the surface polarity close to that of PP resin. Wherein the content of the terylene/cotton fiber is 98.7/1.3 percent, and the modified fiber prepared by the method is modified terylene short fiber with the average length of 1.5 mm;
2. the preparation method of the regenerated modified polyester staple fiber reinforced polypropylene compound comprises the following steps:
according to the weight parts, the regenerated modified polyester staple fibers, the antioxidant, the toner and the polypropylene resin prepared in the step one are melted by a double-screw extruder, extruded, cooled and cut into particles to prepare the regenerated modified polyester staple fiber reinforced polypropylene composite modified material, and relevant material performance evaluation is carried out.
The processing set temperature of the I-X area of the double-screw extruder is 135 ℃,165 ℃,180 ℃,190 ℃,200 ℃,210 ℃,215 ℃,215 ℃ and 220 ℃ in sequence. The rotation speed of the main screw is set to 400r/min, and the temperature of the water tank is 40 ℃.
EXAMPLE 3 preparation of Polypropylene composite
1. The preparation treatment process of the regenerated modified polyester staple fiber comprises the following steps:
1. dry physical crushing stage
The recycled polyester or polyester-cotton blended fabric is cleaned, then moved into a sulfuric acid tank for acidizing treatment (impurity removal and convenient subsequent crushing of softened fabric), dried after the treatment is finished, and then fed into a physical crusher for crushing treatment, and the crushing times are controlled during the treatment so that the length of the obtained fiber is 0.5-5 mm. The sulfuric acid pool is a dilute sulfuric acid solution with the concentration of 50 percent of sulfuric acid solution, and the treatment time is 4 hours.
2. Wet centrifugal separation
Separating the PET/cotton fiber flocculent mixture obtained after the treatment of the dry physical crushing process to obtain pure cotton fibers and regenerated PET fibers, and adopting wet horizontal centrifugal equipment to ensure that the wet density is 1.38-1.41 g/cm by utilizing the wet density difference of the PET fibers and the cotton fibers 3 The wet density of the PET short fiber is 1.50-1.58 g/cm 3 The cotton fibers are separated.
3. Vertical cyclone gas separation
Drying the fiber flocculent mixture treated by the wet process, and further separating by a vertical gas cyclone separation device. The dried fiber flocks enter the equipment through an inlet at the left side of the equipment, are fine under the pushing of rotating air in the equipment, uniformly dispersed fiber particles are directly rotated by 90 degrees and are output from the upper end of the equipment, and large and coarse non-separated fiber clusters, related metals and other impurities are removed from the bottom of the equipment along with the two sides of the equipment. The fibers with a length of 2mm were selected for use.
4. Surface passivation modification treatment of regenerated polyester staple fiber
In order to further improve the performance of the subsequent polyester fiber modified polypropylene material, the PET short fiber after being carefully selected by the vertical gas cyclone separation process is subjected to surface 5 percent NaOH solution etching, the treatment time is 40 minutes at 90 ℃, the surface alkali liquor is cleaned by clear water, then the drying is carried out, the surface treatment passivation is carried out by dodecyl trimethoxy silane at 60 ℃, and the drying is carried out, thus preparing the modified regenerated PET fiber with the surface polarity close to that of PP resin.
Wherein the content of the terylene/cotton fiber is 97.1/2.9 percent, and the modified fiber prepared by the method is modified terylene short fiber with the average length of 2 mm.
2. The preparation method of the regenerated modified polyester staple fiber reinforced polypropylene compound comprises the following steps:
according to the weight parts, the regenerated modified polyester staple fibers, the antioxidant, the toner and the polypropylene resin prepared in the step one are melted by a double-screw extruder, extruded, cooled and cut into particles to prepare the regenerated modified polyester staple fiber reinforced polypropylene composite modified material, and relevant material performance evaluation is carried out.
The processing set temperature of the I-X area of the double-screw extruder is 135 ℃,165 ℃,180 ℃,190 ℃,200 ℃,210 ℃,215 ℃,215 ℃ and 220 ℃ in sequence. The rotation speed of the main screw is set to 400r/min, and the temperature of the water tank is 40 ℃.
EXAMPLE 4 preparation of Polypropylene composite
1. The preparation treatment process of the regenerated modified polyester staple fiber comprises the following steps:
cleaning recycled polyester or polyester-cotton blended fabric, moving the fabric into a sulfuric acid tank for acidizing (removing impurities and softening the fabric for subsequent crushing), drying the fabric after the acidizing is finished, feeding the fabric into a physical crusher for crushing, controlling the crushing times during the treatment so that the length of the obtained fiber is 0.5-5 mm, performing wet centrifugation and air cyclone separation on the obtained fiber, selecting the fiber with the length of 2.5mm, treating the fiber with hexadecyl trimethoxy silane for later use, wherein the content of the polyester/cotton fiber is 96.6/3.4%, and the modified fiber prepared by the method is modified polyester staple fiber with the average length of 2.5 mm;
2. the preparation method of the regenerated modified polyester staple fiber reinforced polypropylene compound comprises the following steps:
according to the weight parts, the regenerated modified polyester staple fibers, the antioxidant, the toner and the polypropylene resin prepared in the step one are melted by a double-screw extruder, extruded, cooled and cut into particles to prepare the regenerated modified polyester staple fiber reinforced polypropylene composite modified material, and relevant material performance evaluation is carried out.
The processing set temperatures of the I-X area of the double-screw extruder are 135 ℃,165 ℃,180 ℃,190 ℃,200 ℃,210 ℃,215 ℃,215 ℃ and 220 ℃ in sequence. The rotation speed of the main screw is set to 400r/min, and the temperature of the water tank is 40 ℃.
EXAMPLE 5 preparation of Polypropylene composite
1. The preparation treatment process of the regenerated modified polyester staple fiber comprises the following steps:
cleaning recycled polyester or polyester-cotton blended fabric, moving the fabric into a sulfuric acid tank for acidizing (removing impurities and softening the fabric for subsequent crushing), drying the fabric after the acidizing is finished, feeding the fabric into a physical crusher for crushing, controlling the crushing times during the treatment so that the length of the obtained fiber is 0.5-5 mm, performing wet centrifugation and air cyclone separation on the obtained fiber, selecting the fiber with the length of 3.0mm, treating the fiber with hexadecyl trimethoxy silane for later use, wherein the content of the polyester/cotton fiber is 94.6/5.4%, and the modified fiber prepared by the method is modified polyester staple fiber with the average length of 3.0 mm;
2. the preparation method of the regenerated modified polyester staple fiber reinforced polypropylene compound comprises the following steps:
melting the regenerated modified polyester staple fiber prepared in the step one, the antioxidant, the toner and the polypropylene resin by a double-screw extruder, extruding, cooling and granulating to prepare a regenerated modified polyester staple fiber reinforced polypropylene composite modified material, and evaluating the performance of related materials.
The processing set temperatures of the I-X area of the double-screw extruder are 135 ℃,165 ℃,180 ℃,190 ℃,200 ℃,210 ℃,215 ℃,215 ℃ and 220 ℃ in sequence. The rotation speed of the main screw is set to 400r/min, and the temperature of the water tank is 40 ℃.
EXAMPLE 6 preparation of Polypropylene composite
1. The preparation treatment process of the regenerated modified polyester staple fiber comprises the following steps:
cleaning recycled polyester or polyester-cotton blended fabric, moving the fabric into a sulfuric acid tank for acidizing (removing impurities and softening the fabric for subsequent crushing), drying the fabric after the acidizing is finished, feeding the fabric into a physical crusher for crushing, controlling the crushing times during the treatment so that the length of the obtained fiber is 0.5-5 mm, performing wet centrifugation and air cyclone separation on the obtained fiber, selecting the fiber with the length of 4.0mm, treating the fiber with hexadecyl trimethoxy silane for later use, wherein the content of the polyester/cotton fiber is 93.5/6.5%, and the modified fiber prepared by the method is modified polyester staple fiber with the average length of 4.0 mm;
2. the preparation method of the regenerated modified polyester staple fiber reinforced polypropylene compound comprises the following steps:
according to the weight parts, the regenerated modified polyester staple fibers, the antioxidant, the toner and the polypropylene resin prepared in the step one are melted by a double-screw extruder, extruded, cooled and cut into particles to prepare the regenerated modified polyester staple fiber reinforced polypropylene composite modified material, and relevant material performance evaluation is carried out.
The processing set temperatures of the I-X area of the double-screw extruder are 135 ℃,165 ℃,180 ℃,190 ℃,200 ℃,210 ℃,215 ℃,215 ℃ and 220 ℃ in sequence. The rotation speed of the main screw is set to 400r/min, and the temperature of the water tank is 40 ℃.
EXAMPLE 7 preparation of Polypropylene composite
1. The preparation treatment process of the regenerated modified polyester staple fiber comprises the following steps:
the recycled polyester or polyester-cotton blended fabric is cleaned, then the polyester or polyester-cotton blended fabric is moved into a sulfuric acid tank to be acidified (impurity removal and fabric softening are convenient for subsequent crushing), the polyester or polyester-cotton blended fabric is dried after the treatment is finished, then the polyester or polyester-cotton blended fabric is fed into a physical crusher to be crushed, the crushing frequency is controlled during the treatment so that the length of the obtained fiber is 0.5-5 mm, then the obtained fiber is subjected to wet centrifugation and air cyclone separation, the fiber with the length of 4.5mm is selected and treated by hexadecyl trimethoxy silane for later use, wherein the content of the polyester/cotton fiber is 93.1/6.9%, and the modified fiber prepared by the method is modified polyester staple fiber with the average length of 4.5 mm.
2. The preparation method of the regenerated modified polyester staple fiber reinforced polypropylene compound comprises the following steps:
according to the weight parts, the regenerated modified polyester staple fibers, the antioxidant, the toner and the polypropylene resin prepared in the step one are melted by a double-screw extruder, extruded, cooled and cut into particles to prepare the regenerated modified polyester staple fiber reinforced polypropylene composite modified material, and relevant material performance evaluation is carried out.
The processing set temperature of the I-X area of the double-screw extruder is 135 ℃,165 ℃,180 ℃,190 ℃,200 ℃,210 ℃,215 ℃,215 ℃ and 220 ℃ in sequence. The rotation speed of the main screw is set to 400r/min, and the temperature of the water tank is 40 ℃.
Comparative example 1
In order to better embody the improvement effect of the wet centrifugal separation process of the polyester staple fibers on the improvement of the performance of the polyester staple fiber reinforced composite in the preparation method of the regenerated modified polyester staple fiber reinforced polypropylene composite in comparison with the embodiment 2, the polypropylene material is directly filled and modified by directly adopting the fiber floc after crushing treatment in the corresponding comparative example 1, and the preparation method mainly comprises the following specific implementation steps:
according to the weight parts, the regenerated modified polyester staple fiber reinforced polypropylene composite modified material is prepared by directly adopting the fiber floccule, the antioxidant, the toner and the polypropylene resin after the first physical crushing treatment through melting, extruding, cooling and granulating by a double-screw extruder, and related material performance evaluation is carried out.
The processing set temperature of the I-X area of the double-screw extruder is 135 ℃,165 ℃,180 ℃,190 ℃,200 ℃,210 ℃,215 ℃ and 220 ℃ in sequence. The rotation speed of the main screw is set to 400r/min, and the temperature of the water tank is 40 ℃.
Comparative example 2
In order to better embody the improvement effect of the vertical gas cyclone separation process of the polyester-cotton short fibers on the performance improvement of the polyester-short fiber reinforced composite in the preparation method of the regenerated modified polyester-short fiber reinforced polyolefin composite compared with the embodiment 2, the corresponding comparative example 2 directly adopts the fiber floccule after physical crushing and wet centrifugal separation process treatment to directly fill and modify the polypropylene material, and mainly comprises the following specific implementation steps:
according to parts by weight, the fiber floccule, the antioxidant, the toner and the polypropylene resin which are treated by a first physical crushing process and a second wet centrifugal separation process are directly adopted in the steps, and are melted, extruded, cooled and cut into granules by a double-screw extruder to prepare the regenerated modified polyester short fiber reinforced polypropylene composite modified material, and the performance evaluation of related materials is carried out.
The processing set temperature of the I-X area of the double-screw extruder is 135 ℃,165 ℃,180 ℃,190 ℃,200 ℃,210 ℃,215 ℃,215 ℃ and 220 ℃ in sequence. The rotation speed of the main screw is set to 400r/min, and the temperature of the water tank is 40 ℃.
Comparative example 3
In order to better embody the improvement effect of the surface passivation modification treatment on the polyester staple fibers on the performance improvement of the polyester staple fiber reinforced composite in the preparation method of the regenerated modified polyester staple fiber reinforced polypropylene composite compared with the embodiment 2, the corresponding comparative example 3 directly adopts the fiber floccule after the crushing and the wet centrifugal separation process and the vertical gas cyclone separation process to directly fill and modify the polypropylene material, and mainly comprises the following specific implementation steps:
according to the weight parts, the steps are directly adopted from a comparative example 3, the fiber flocculent fiber, the antioxidant, the toner and the polypropylene resin are directly adopted, the fiber flocculent fiber, the antioxidant, the toner and the polypropylene resin are subjected to melting, extruding, cooling and grain cutting by a double-screw extruder, the regenerated modified polyester short fiber reinforced polypropylene composite modified material is prepared, and related material performance evaluation is carried out.
The processing set temperature of the I-X area of the double-screw extruder is 135 ℃,165 ℃,180 ℃,190 ℃,200 ℃,210 ℃,215 ℃,215 ℃ and 220 ℃ in sequence. The rotation speed of the main screw is set to 400r/min, and the temperature of the water tank is 40 ℃.
Comparative example 4
In order to better embody the performance advantages of the regenerated modified polyester staple fiber reinforced polypropylene composite in comparison with the embodiment 2, the corresponding comparative example 4 directly adopts the talcum powder commonly used in the field of the current automobile modified material industry to directly fill and modify the polypropylene material, and mainly comprises the following specific implementation steps:
according to parts by weight, the talcum powder, the antioxidant, the toner and the polypropylene resin which are commonly used in the automobile industry and have 3000 meshes are directly adopted in the steps, and are melted, extruded, cooled and cut into granules through a double-screw extruder to prepare the talcum powder reinforced polypropylene composite modified material, and the performance evaluation of related materials is carried out.
The processing set temperatures of the I-X area of the double-screw extruder are 135 ℃,165 ℃,180 ℃,190 ℃,200 ℃,210 ℃,215 ℃,215 ℃ and 220 ℃ in sequence. The rotation speed of the main screw is set to 400r/min, and the temperature of the water tank is 40 ℃.
Comparative example 5
In order to better embody the performance advantages of the regenerated modified polyester staple fiber reinforced polypropylene composite in comparison with the embodiment 2, the corresponding comparative example 4 directly adopts the commonly used glass fiber in the field of the current automobile modified material industry to directly fill and modify the polypropylene material, and mainly comprises the following specific implementation steps:
according to the weight parts, the glass fiber reinforced polypropylene composite modified material is prepared by directly adopting the glass fiber with the fiber diameter of 13 mu m, the antioxidant, the toner and the polypropylene resin which are commonly used in the automobile industry, melting through a double-screw extruder, extruding, cooling and granulating, and related material performance evaluation is carried out.
The processing set temperatures of the I-X area of the double-screw extruder are 135 ℃,165 ℃,180 ℃,190 ℃,200 ℃,210 ℃,215 ℃,215 ℃ and 220 ℃ in sequence. The rotation speed of the main screw is set to 400r/min, and the temperature of the water tank is 40 ℃.
The reinforced modified polypropylene composite materials prepared in the above examples 1 to 7 and the corresponding comparative examples 1 to 5 were subjected to performance tests according to the test standards and conditions in the following table 3, the processing process and the formula information of the reinforced modified polypropylene products of the examples 1 to 7 and the comparative examples 1 to 5 are shown in table 4, the test performance of the reinforced modified polypropylene products of the examples 1 to 7 and the comparative examples 1 to 5 is shown in table 5, and the performance comparison ratio of the modified polypropylene materials prepared in the examples 2 and the comparative examples 1 to 5 is shown in table 6.
Table 3 shows the performance test standards and conditions of the reinforced polypropylene composite material
Serial number Inspection index Inspection method Unit of Test conditions
1 Density of GB/T 1033.1 g/cm^3 23℃
2 Tensile strength GB/T 1040.2 MPa 50mm/min
3 Elongation at break GB/T 1040.2 ％ 50mm/min
4 Notched impact strength GB/T 1043 kJ/m^2 23℃
5 Flexural modulus GB/T9341 MPa 2mm/min
TABLE 4 treatment Process and formulation information for reinforced modified Polypropylene products of examples 1-7 and comparative examples 1-5
Figure BDA0003722107210000091
Figure BDA0003722107210000101
TABLE 5 Effect of average PET fiber length on the Properties of modified Polypropylene materials in examples 1-7
Figure BDA0003722107210000102
Figure BDA0003722107210000111
Remarking: for screening out the appropriate modified fiber length.
TABLE 6 comparison of the Properties of the modified Polypropylene materials prepared in example 2 and comparative examples 1 to 5
Figure BDA0003722107210000112
Figure BDA0003722107210000121
Table 4 shows the processing process and formula information of the reinforced modified polypropylene products of examples 1 to 7 and comparative examples 1 to 5, table 5 shows the influence of the average length of the PET fiber in examples 1 to 7 on the performance of the modified polypropylene material, and the test results show that the strength, especially the tensile strength and the impact strength of the prepared regenerated modified polyester staple fiber reinforced polypropylene product are greatly influenced by the average length of the regenerated PET fiber, mainly because the reinforcing effect of the PET fiber on the polypropylene resin is increased along with the increase of the average length of the regenerated PET fiber, which is reflected in that the tensile strength and the impact strength of the final modified product are increased, but when the average length of the PET fiber is increased to 1.5mm, the compatibility of the PET fiber and the polypropylene matrix resin is influenced due to the decrease of the purity of the PET fiber/cotton fiber, and the impact performance of the final modified polypropylene product is obviously reduced, so how to balance the average length of the PET fiber and the final mechanical performance of the final modified polypropylene product is important, and the technical team of the method screens out the preferable patent scheme of the invention with the average length of 0.5mm to 0.5 mm.
In order to further verify the invention effect of the scheme of the invention, the invention effect of the patent of the invention is fully verified by comparing the performance of the modified polypropylene material prepared in the example 2 and the comparative examples 1 to 5 in the table 6, and as shown in the table 6, the wet centrifugation and suspended air flow separation process in the technical scheme is beneficial to increasing the purity of the PET short fiber prepared by the dry crushing process, and reducing the content of cotton fiber and related impurities which affect the performance of the final modified polypropylene product, thereby improving the mechanical performance of the final modified product, especially the improvement on the impact performance. In addition, as shown in the test data in table 6, the compatibility of the PET fiber and the polypropylene resin is improved by the introduction of the fiber surface passivation treatment process, and the impact property on the final product is obviously improved.
As shown in the embodiment 2 and the comparative examples 4 and 5-6 in the table 6, the prepared regenerated modified polyester short fiber reinforced polypropylene composite has better material strength and lower material density advantage compared with mineral talcum powder filling commonly used in the automobile industry while achieving the industry appeal of low carbon and green cycle, and compared with the conventional short glass fiber reinforced polypropylene material, the regenerated modified polyester short fiber reinforced polypropylene composite prepared by the method has lower material density while the material strength is close to that of the conventional short glass fiber reinforced polypropylene material, can be used for completely or partially replacing glass fiber or mineral reinforced polypropylene materials, and provides a brand new innovative application for realizing the recycling of waste clothes with higher added value in the application field of automobile modified polypropylene materials and related modified materials.

Claims (10)

1. The modified and reinforced polypropylene composite material of the waste polyester-cotton fabric is characterized by comprising the following raw materials in parts by weight: 10-40 parts of regenerated modified polyester staple fiber, 0.1-3.0 parts of antioxidant and toner and 60-90 parts of polypropylene resin; the polypropylene resin is polypropylene with the material flow speed of 0.5-120 g/10min under the conditions of 230 ℃ and 2.16 Kg; the antioxidant is at least one of antioxidant 1010 (tetra (beta-3, 5-di-tert-butyl-4-hydroxyphenyl) pentaerythritol ester), antioxidant 168 (tri (2, 4-di-tert-butylphenyl) phosphite) and antioxidant DSTP (dioctadecyl thiodipropionate); the toner is at least one of carbon black, titanium dioxide, iron oxide red and yellow; the purity of PET fiber in the regenerated polyester staple fiber is more than or equal to 90 percent, and the average length of the fiber is 0.5 mm-5.0 mm.
2. A method for preparing the polypropylene composite material according to claim 1, comprising the steps of:
step s1, preparing regenerated modified polyester staple fibers: sequentially carrying out dry physical crushing, wet centrifugal separation, vertical gas cyclone separation and surface passivation modification treatment on the recovered pure polyester or polyester-cotton blended fabric to obtain regenerated modified polyester staple fibers;
step s2, preparation of the polypropylene compound: melting, extruding, cooling and granulating 10-40 parts of the regenerated modified polyester staple fiber obtained in the step s1, 0.1-3.0 parts of antioxidant and toner and the balance of polypropylene PP resin by a double-screw extruder to prepare a regenerated modified polyester staple fiber reinforced polypropylene composite modified material; the processing set temperature of the I-X area of the double-screw extruder is 135 ℃,165 ℃,180 ℃,190 ℃,200 ℃,210 ℃,215 ℃,220 ℃, the rotation speed of the main screw is 300-500 r/min, and the temperature of the water tank is 23-50 ℃ in sequence.
3. The method of claim 2, wherein in step s1, the dry physical disruption is performed by: the method comprises the following steps of cleaning the recycled pure polyester or polyester-cotton blended fabric through a clear water tank, carrying out acidizing treatment (removing impurities and softening the fabric for convenient follow-up crushing) through a sulfuric acid tank, drying, and carrying out crushing treatment for multiple times through a crusher to obtain the PET/cotton fiber flocculent mixture with the fiber length of 0.5-5.0 mm.
4. The preparation method according to claim 3, characterized in that the sulfuric acid pool is a dilute sulfuric acid solution with a sulfuric acid solution concentration of 20% to 50% and the treatment time is generally 4 to 12 hours.
5. The method of claim 3, wherein the PET/cotton fiber fluff mixture has a fiber length of 0.5mm to 1.5mm.
6. The method according to claim 2, wherein the wet centrifugation in step s1 is performed as follows: separating the PET/cotton fiber flocculent mixture into wet density of 1.38-1.41 g/cm by wet horizontal centrifugal equipment 3 The wet density of the PET short fibers is 1.50-1.58 g/cm 3 The cotton fiber of (2).
7. The process according to claim 3, wherein in step s1, the PET/cotton fiber fluff mixture having a PET purity of 93% or more is obtained after the separation treatment with the vertical gas cyclone.
8. The method according to claim 3, wherein in step s1, the PET short fibers separated by the vertical gas cyclone are subjected to coarsening treatment, then subjected to surface treatment containing alkylsilane to passivate, and dried to prepare modified regenerated PET fibers; the aqueous alkali for the roughening treatment is a solution containing 1 to 5 percent of NaOH, the treatment temperature is between 50 and 90 ℃, and the treatment time is between 40 and 120 minutes; the alkylsiloxane solution.
9. The method of claim 8, wherein the alkylsiloxane is dodecane to octadecyltrimethoxysilane.
10. The method of claim 8, wherein the passivation temperature is 30 ℃ to 60 ℃.
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