CN115181358B - Waste polyester cotton fabric modified reinforced polypropylene composite material and preparation method thereof - Google Patents
Waste polyester cotton fabric modified reinforced polypropylene composite material and preparation method thereof Download PDFInfo
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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
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- 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
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- 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
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- 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
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- 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
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- 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
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- 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
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Abstract
The invention relates to recycling of waste clothes, 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 reutilization of 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 to 40 parts of regenerated modified polyester staple fiber, 0.1 to 3.0 parts of antioxidant and toner and the balance of polypropylene PP resin; the polypropylene resin refers to polypropylene with the material flow speed of 0.5-120 g/10min under the condition of 230 ℃ and 2.16 Kg. The regenerated polyester staple fiber reinforced polypropylene composite material with excellent performance is prepared by applying the polyester staple fibers extracted from the waste polyester cotton fabrics to the polypropylene material for modification of the automobile interior and exterior trim, and can be used for completely or partially replacing glass fibers or mineral reinforced polypropylene materials.
Description
Technical Field
The invention relates to recycling of waste clothes, in particular to a modified and reinforced polypropylene composite material of waste polyester cotton fabrics and a preparation method thereof.
Background
In recent years, along with the continuous improvement of national economy and living standard of people, the requirements and replacement frequency of people on clothes are higher and higher, so that a large amount of waste clothes are generated, wherein the polyester-cotton blended clothes are deeply favored by consumers due to the characteristics of stiffness, smoothness, quick drying, wearing resistance and the like, so that a considerable proportion of the waste clothes is occupied, the recycling technology of the waste clothes is started from the beginning, and the waste clothes are spread from the beginning to be buried or burned in the fields with lower technical threshold and material performance requirements. For example, patent CN201811149512.9 discloses a waste sole reclaimed rubber powder composite waste clothing regenerated fiber reinforced asphalt mixture and a preparation method thereof, wherein the asphalt mixture is prepared by mixing reclaimed rubber powder modified asphalt, aggregate, waste clothing regenerated fiber and mineral powder. As patent CN202110613463.5 discloses a wood-plastic plate and profile prepared by recycling waste clothes and a preparation method thereof, the wood-plastic profile prepared by using waste clothes uses waste clothes fiber to replace wood powder used in a large amount in traditional wood-plastic products, and the fiber in the waste clothes is completely melted into organic materials through chain extension and capacity expansion treatment, and is extruded into the plate or profile. However, how to recycle the waste clothes with higher added value is a research hot spot of many technological workers.
The automotive industry is an important national economic support industry, and low-carbon, green cycle has been an important direction and goal for future development of the automotive industry.
Disclosure of Invention
The invention aims to provide a new choice for reutilization of 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 to 40 parts 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 refers to polypropylene with the material flow speed of 0.5-120 g/10min under the condition 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 ester) 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%, 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 short fibers;
step s2, preparation of a polypropylene compound: melting 10-40 parts of regenerated modified polyester staple fibers obtained in the step s1, 0.1-3.0 parts of antioxidant and toner, and the balance of polypropylene PP resin raw materials through 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 region of the double-screw extruder is 135 ℃,165 ℃,180 ℃,190 ℃,200 ℃,210 ℃,215 ℃,220 ℃ and the main screw rotating speed is 300-500 r/min, and the water tank temperature is 23-50 ℃.
Specifically, in step s1, the operation of dry physical crushing is as follows: and cleaning the recovered pure terylene or polyester cotton blended fabric through a clear water tank, acidizing the fabric in a sulfuric acid tank (removing impurities, softening the fabric to facilitate subsequent crushing), drying, and crushing the fabric for a plurality of times through a crusher to obtain a PET/cotton fiber flocculent mixture with the fiber length of 0.5-5.0 mm.
Wherein the sulfuric acid pond is a dilute sulfuric acid solution with the concentration of 20-50%, 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 wet centrifugation 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 PET short fiber and wet state density of the polyester staple are 1.50-1.58 g/cm 3 Is a cotton fiber of (2).
In step s1, a PET/cotton fiber flocculent mixture with the PET purity of more than 93% is obtained after vertical gas cyclone separation treatment.
In the step s1, coarsening the PET short fiber subjected to vertical gas cyclone separation, carrying out surface treatment passivation by containing alkylsilane, and drying to obtain a modified regenerated PET fiber; the alkali solution for coarsening treatment is a solution containing 1-5% NaOH, the treatment temperature is 50-90 ℃, and the treatment time is 40-120 minutes; the alkyl siloxane solution.
The roughening treatment is to etch the fiber surface with alkali solution to make it rough, clean the surface alkali solution with clear water after treatment, and oven dry.
Preferably, the alkylsiloxane is dodecane to octadecyltrimethoxysilane.
Preferably, the alkyl siloxane is hexadecyltrimethoxysilane.
Specifically, the passivation treatment temperature is 30-60 ℃.
The invention has the beneficial effects that: according to the invention, from development demands of automobile industry, long-term research is carried out, a plurality of technical barriers are overcome, the technology is started from waste fabric treatment and fine inspection technology, and polyester fiber surface treatment and polypropylene material modification processing technology are combined, so that polyester staple fibers extracted from waste polyester cotton fabrics are finally successfully applied to polypropylene materials for automobile interior and exterior modification, a regenerated polyester staple fiber reinforced polypropylene composite material with excellent performance is prepared, and the composite material can be used for completely or partially replacing glass fibers or mineral reinforced polypropylene materials, and achieves high added value recycling of waste clothes while achieving low-carbon and green circulating industrial requirements.
Detailed Description
The present invention will be further illustrated with reference to specific examples. It should be emphasized that these examples are merely provided to further illustrate the invention and should not be construed as limiting the scope of the invention. Further, it is understood that various changes and modifications of the present invention may be made by those skilled in the art after reading the description of the present invention, and such equivalents are intended to fall within the scope of the claims appended hereto.
The high flow rate polypropylene in the following examples is preferably medium petrochemical grade M1200HS homopolymerized polypropylene resin, and the flow rate of the resin under the conditions of 230 ℃ and 2.16Kg is 12g/min respectively.
Example 1 preparation of Polypropylene composite Material
1. The preparation treatment process of the regenerated modified polyester staple fiber comprises the following steps:
1. dry physical crushing stage
And (3) cleaning the recovered terylene or polyester-cotton blended fabric, then transferring the cleaned terylene or polyester-cotton blended fabric into a sulfuric acid tank for acidizing treatment (impurity removal, fabric softening and convenient subsequent crushing), drying the terylene or polyester-cotton blended fabric after the treatment is finished, and then feeding the terylene or polyester-cotton blended fabric into a physical crusher for crushing treatment, wherein the crushing times are controlled during the treatment so that the length of the obtained fiber is between 0.5 and 5mm. The sulfuric acid pool is a dilute sulfuric acid solution with the concentration of 50 percent, and the treatment time is 4 hours.
2. Wet centrifugal separation
In order to separate the PET/cotton fiber flocculent mixture obtained after the dry physical crushing process treatment so as to obtain pure cotton fibers and regenerated PET fibers, wet density difference between the PET fibers and the cotton fibers is utilized, and wet horizontal centrifugal equipment is adopted to ensure that the wet density is 1.38-1.41 g/cm 3 The PET short fiber and wet state density of the polyester staple are 1.50-1.58 g/cm 3 The cotton fiber separation of (2) is shown in Table 1 below as the purity of PET fiber before and after wet centrifugation, whereinPreferably, the fiber floc mixture with a fiber length of 0.5mm to 1.5mm facilitates wet separation. The centrifugal equipment uses a horizontal centrifuge, and the manufacturer is Zhuo Hangji mechanical limited company in Zhangjinggang, and the equipment model GK800.
TABLE 1 average purity of PET fibers before and after the centrifugation process for different fiber lengths
3. Vertical gas cyclone separation
The fiber flocculent mixture treated by the wet process is further separated by a vertical gas cyclone separation device (HCXF-800 cyclone separator of Hebei Seisakusho environmental protection mechanical Co., ltd.) after being dried. The dried fiber wadding enters the equipment through an inlet at the left side of the equipment, is fine under the pushing of rotating air in the equipment, and uniformly dispersed fiber particles are directly output from the upper end of the equipment at a 90-degree angle, and large, coarse and unseparated fiber clusters, related metals and other impurities are discharged from the bottom of the equipment along with the two sides of the equipment.
As can be seen from Table 2, the PET/cotton fiber flock which is not separated in the wet separation process can be further cleaned from the fiber flock by the process, the purity of the PET fiber flock is further improved, meanwhile, the polyester/cotton fiber winding clusters which are dispersed in the process of vertical separation of dry physical crushing and wet centrifugation are also effectively removed, the crude polyester/cotton fiber winding clusters which are not separated in the previous dry wet process are removed, the cotton fiber winding clusters or the polyester fiber clusters are also further improved, and the performance of the subsequent polyester fiber modified polypropylene material is further improved.
TABLE 2 average purity of PET fibers before and after vertical gas cyclone separation process
4. Surface passivation modification treatment for regenerated polyester staple fibers
In order to further improve the performance of the subsequent polyester fiber modified polypropylene material, the PET short fiber carefully selected by the vertical gas cyclone separation process is etched by a NaOH solution with the surface of 3 percent, the treatment time is 90 minutes at the temperature of 60 ℃, the surface alkali liquor is cleaned by clear water, and then the PET short fiber is dried, subjected to surface treatment passivation by hexadecyl trimethoxy silane at the temperature of 60 ℃ and dried, so that the modified regenerated PET fiber with the surface polarity close to that of PP resin is prepared. And selecting modified polyester staple fibers with the average length of 0.5mm, wherein the content of the polyester/cotton fibers is controlled to be 99.5/0.5 percent.
2. The preparation method of the regenerated modified polyester staple fiber reinforced polypropylene compound comprises the following steps:
according to the parts by weight, the regenerated modified polyester staple fiber, the antioxidant, the toner and the polypropylene resin prepared in the step one are melted, extruded, cooled and pelletized through a double screw extruder to prepare the regenerated modified polyester staple fiber reinforced polypropylene compound modified material, and the performance of the related material is evaluated.
The processing set temperature of the I-X region of the double-screw extruder is 135 ℃,165 ℃,180 ℃,190 ℃,200 ℃,210 ℃,210 ℃,215 ℃,215 ℃ and 220 ℃ in sequence. The main screw speed was set at 400r/min and the water bath temperature was 40 ℃.
Example 2 preparation of Polypropylene composite Material
1. The preparation treatment process of the regenerated modified polyester staple fiber comprises the following steps:
1. dry physical crushing stage
And (3) cleaning the recovered terylene or polyester-cotton blended fabric, then transferring the cleaned terylene or polyester-cotton blended fabric into a sulfuric acid tank for acidizing treatment (impurity removal, fabric softening and convenient subsequent crushing), drying the terylene or polyester-cotton blended fabric after the treatment is finished, and then feeding the terylene or polyester-cotton blended fabric into a physical crusher for crushing treatment, wherein the crushing times are controlled during the treatment so that the length of the obtained fiber is between 0.5 and 5mm. The sulfuric acid pool is a dilute sulfuric acid solution with the concentration of 30 percent, and the treatment time is 8 hours.
2. Wet centrifugal separation
To separate the PET/cotton fiber flocculent mixture obtained by the dry state physical crushing processPure cotton fiber and regenerated PET fiber are obtained, and wet density is 1.38-1.41 g/cm by using wet horizontal centrifugal equipment by utilizing wet density difference of the PET fiber and the cotton fiber 3 The PET short fiber and wet state density of the polyester staple are 1.50-1.58 g/cm 3 Is separated from the cotton fibers of the (a).
3. Vertical gas cyclone separation
And drying the fiber flocculent mixture treated by the wet process, and further separating by a vertical gas cyclone separation device. The dried fiber wadding enters the equipment through an inlet at the left side of the equipment, is fine under the pushing of rotating air in the equipment, and uniformly dispersed fiber particles are directly output from the upper end of the equipment at a 90-degree angle, and large, coarse and unseparated fiber clusters, related metals and other impurities are discharged from the bottom of the equipment along with the two sides of the equipment. Fibers with a length of 1.5mm were selected for use.
4. Surface passivation modification treatment for regenerated polyester staple fibers
In order to further improve the performance of the subsequent polyester fiber modified polypropylene material, the PET short fiber carefully selected by the vertical gas cyclone separation process is etched by a NaOH solution with the surface of 3 percent, the treatment time is 90 minutes at 60 ℃, the surface alkali liquor is cleaned by clean water, and then the PET short fiber is dried, subjected to surface treatment passivation by hexadecyl trimethoxy silane at 50 ℃, and dried, so that the modified regenerated PET fiber with the surface polarity close to that of PP resin is prepared. Wherein the content of 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 parts by weight, the regenerated modified polyester staple fiber, the antioxidant, the toner and the polypropylene resin prepared in the step one are melted, extruded, cooled and pelletized through a double screw extruder to prepare the regenerated modified polyester staple fiber reinforced polypropylene compound modified material, and the performance of the related material is evaluated.
The processing set temperature of the I-X region of the double-screw extruder is 135 ℃,165 ℃,180 ℃,190 ℃,200 ℃,210 ℃,210 ℃,215 ℃,215 ℃ and 220 ℃ in sequence. The main screw speed was set at 400r/min and the water bath temperature was 40 ℃.
Example 3 preparation of Polypropylene composite Material
1. The preparation treatment process of the regenerated modified polyester staple fiber comprises the following steps:
1. dry physical crushing stage
And (3) cleaning the recovered terylene or polyester-cotton blended fabric, then transferring the cleaned terylene or polyester-cotton blended fabric into a sulfuric acid tank for acidizing treatment (impurity removal, fabric softening and convenient subsequent crushing), drying the terylene or polyester-cotton blended fabric after the treatment is finished, and then feeding the terylene or polyester-cotton blended fabric into a physical crusher for crushing treatment, wherein the crushing times are controlled during the treatment so that the length of the obtained fiber is between 0.5 and 5mm. The sulfuric acid pool is a dilute sulfuric acid solution with the concentration of 50 percent, and the treatment time is 4 hours.
2. Wet centrifugal separation
In order to separate the PET/cotton fiber flocculent mixture obtained after the dry physical crushing process treatment so as to obtain pure cotton fibers and regenerated PET fibers, wet density difference between the PET fibers and the cotton fibers is utilized, and wet horizontal centrifugal equipment is adopted to ensure that the wet density is 1.38-1.41 g/cm 3 The PET short fiber and wet state density of the polyester staple are 1.50-1.58 g/cm 3 Is separated from the cotton fibers of the (a).
3. Vertical gas cyclone separation
And drying the fiber flocculent mixture treated by the wet process, and further separating by a vertical gas cyclone separation device. The dried fiber wadding enters the equipment through an inlet at the left side of the equipment, is fine under the pushing of rotating air in the equipment, and uniformly dispersed fiber particles are directly output from the upper end of the equipment at a 90-degree angle, and large, coarse and unseparated fiber clusters, related metals and other impurities are discharged from the bottom of the equipment along with the two sides of the equipment. Fibers with a length of 2mm were selected for use.
4. Surface passivation modification treatment for regenerated polyester staple fibers
In order to further improve the performance of the subsequent polyester fiber modified polypropylene material, the PET short fiber carefully selected by the vertical gas cyclone separation process is etched by a NaOH solution with the surface of 5 percent, the treatment time is 40 minutes at 90 ℃, the surface alkali liquor is cleaned by clear water, and then the PET short fiber is dried, subjected to surface treatment passivation by dodecyl trimethoxy silane at 60 ℃, and dried, so that the modified regenerated PET fiber with the surface polarity close to that of PP resin is prepared.
Wherein the content of terylene/cotton fiber is 97.1/2.9%, and the modified fiber prepared by the method is modified terylene short fiber with 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 parts by weight, the regenerated modified polyester staple fiber, the antioxidant, the toner and the polypropylene resin prepared in the step one are melted, extruded, cooled and pelletized through a double screw extruder to prepare the regenerated modified polyester staple fiber reinforced polypropylene compound modified material, and the performance of the related material is evaluated.
The processing set temperature of the I-X region of the double-screw extruder is 135 ℃,165 ℃,180 ℃,190 ℃,200 ℃,210 ℃,210 ℃,215 ℃,215 ℃ and 220 ℃ in sequence. The main screw speed was set at 400r/min and the water bath temperature was 40 ℃.
Example 4 preparation of Polypropylene composite Material
1. The preparation treatment process of the regenerated modified polyester staple fiber comprises the following steps:
cleaning the recovered terylene or polyester-cotton blended fabric, then transferring the cleaned terylene or polyester-cotton blended fabric into a sulfuric acid tank for acidizing treatment (impurity removal, fabric softening is convenient for subsequent crushing), drying the terylene or cotton blended fabric after the treatment is finished, then feeding the terylene or cotton blended fabric into a physical crusher for crushing treatment, controlling the crushing times during the treatment to ensure that the length of the obtained fiber is between 0.5 and 5mm, then carrying out wet centrifugation and air cyclone separation on the obtained fiber, and selecting the fiber with the length of 2.5mm for treatment by hexadecyl trimethoxy silane for later use, wherein the content of terylene/cotton fiber is 96.6/3.4 percent, and the modified fiber prepared by the method is modified terylene short 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 parts by weight, the regenerated modified polyester staple fiber, the antioxidant, the toner and the polypropylene resin prepared in the step one are melted, extruded, cooled and pelletized through a double screw extruder to prepare the regenerated modified polyester staple fiber reinforced polypropylene compound modified material, and the performance of the related material is evaluated.
The processing set temperature of the I-X region of the double-screw extruder is 135 ℃,165 ℃,180 ℃,190 ℃,200 ℃,210 ℃,210 ℃,215 ℃,215 ℃ and 220 ℃ in sequence. The main screw speed was set at 400r/min and the water bath temperature was 40 ℃.
Example 5 preparation of Polypropylene composite Material
1. The preparation treatment process of the regenerated modified polyester staple fiber comprises the following steps:
cleaning the recovered terylene or polyester-cotton blended fabric, then transferring the cleaned terylene or polyester-cotton blended fabric into a sulfuric acid tank for acidizing treatment (impurity removal, fabric softening is convenient for subsequent crushing), drying the terylene or cotton blended fabric after the treatment is finished, then feeding the terylene or cotton blended fabric into a physical crusher for crushing treatment, controlling the crushing times during the treatment to ensure that the length of the obtained fiber is between 0.5 and 5mm, then carrying out wet centrifugation and air cyclone separation on the obtained fiber, and selecting the fiber with the length of 3.0mm for treatment by hexadecyl trimethoxy silane for later use, wherein the content of terylene/cotton fiber is 94.6/5.4 percent, and the modified fiber prepared by the method is modified terylene short 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:
according to the parts by weight, the regenerated modified polyester staple fiber, the antioxidant, the toner and the polypropylene resin prepared in the step one are melted by a double-screw extruder, extruded, cooled and pelletized to prepare the regenerated modified polyester staple fiber reinforced polypropylene compound modified material, and the performance of the related material is evaluated.
The processing set temperature of the I-X region of the double-screw extruder is 135 ℃,165 ℃,180 ℃,190 ℃,200 ℃,210 ℃,210 ℃,215 ℃,215 ℃ and 220 ℃ in sequence. The main screw speed was set at 400r/min and the water bath temperature was 40 ℃.
Example 6 preparation of Polypropylene composite Material
1. The preparation treatment process of the regenerated modified polyester staple fiber comprises the following steps:
cleaning the recovered terylene or polyester-cotton blended fabric, then transferring the cleaned terylene or polyester-cotton blended fabric into a sulfuric acid tank for acidizing treatment (impurity removal, fabric softening is convenient for subsequent crushing), drying the terylene or cotton blended fabric after the treatment is finished, then feeding the terylene or cotton blended fabric into a physical crusher for crushing treatment, controlling the crushing times during the treatment to ensure that the length of the obtained fiber is between 0.5 and 5mm, then carrying out wet centrifugation and air cyclone separation on the obtained fiber, and selecting the fiber with the length of 4.0mm for treatment by hexadecyl trimethoxy silane for later use, wherein the content of terylene/cotton fiber is 93.5/6.5 percent, and the modified fiber prepared by the method is modified terylene short 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 parts by weight, the regenerated modified polyester staple fiber, the antioxidant, the toner and the polypropylene resin prepared in the step one are melted, extruded, cooled and pelletized through a double screw extruder to prepare the regenerated modified polyester staple fiber reinforced polypropylene compound modified material, and the performance of the related material is evaluated.
The processing set temperature of the I-X region of the double-screw extruder is 135 ℃,165 ℃,180 ℃,190 ℃,200 ℃,210 ℃,210 ℃,215 ℃,215 ℃ and 220 ℃ in sequence. The main screw speed was set at 400r/min and the water bath temperature was 40 ℃.
Example 7 preparation of Polypropylene composite Material
1. The preparation treatment process of the regenerated modified polyester staple fiber comprises the following steps:
the recovered terylene or polyester-cotton blended fabric is cleaned, then the cleaned terylene or polyester-cotton blended fabric is moved into a sulfuric acid tank for acidification treatment (impurity removal, fabric softening is convenient for subsequent crushing), the terylene or polyester-cotton blended fabric is dried after the treatment is finished, then the terylene or cotton blended fabric is fed into a physical crusher for crushing treatment, the crushing times are controlled during the treatment so that the length of the obtained fiber is between 0.5 and 5mm, the obtained fiber is subjected to wet centrifugation and air cyclone separation, and the fiber with the length of 4.5mm is selected and treated by hexadecyl trimethoxy silane for standby, wherein the content of terylene/cotton fiber is 93.1/6.9 percent, and the modified fiber prepared by the method is modified terylene short 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 parts by weight, the regenerated modified polyester staple fiber, the antioxidant, the toner and the polypropylene resin prepared in the step one are melted, extruded, cooled and pelletized through a double screw extruder to prepare the regenerated modified polyester staple fiber reinforced polypropylene compound modified material, and the performance of the related material is evaluated.
The processing set temperature of the I-X region of the double-screw extruder is 135 ℃,165 ℃,180 ℃,190 ℃,200 ℃,210 ℃,210 ℃,215 ℃,215 ℃ and 220 ℃ in sequence. The main screw speed was set at 400r/min and the water bath temperature was 40 ℃.
Comparative example 1
In order to contrast with the embodiment 2, the invention better embodies the improvement effect of the wet centrifugal separation process of the polyester-cotton staple fibers on the performance of the polyester-staple fiber reinforced polypropylene composite in the preparation method of the regenerated modified polyester-staple fiber reinforced polypropylene composite, and the corresponding comparative example 1 directly adopts the broken fiber floc to directly fill and modify the polypropylene material, and mainly comprises the following concrete implementation steps:
according to the parts by weight, the fiber floccules, the antioxidant, the toner and the polypropylene resin which are subjected to the first physical crushing treatment are directly adopted in the steps, melted by a double screw extruder, extruded, cooled and pelletized, and the regenerated modified polyester staple fiber reinforced polypropylene composite modified material is prepared, and the performance of the related material is evaluated.
The processing set temperature of the I-X regions of the double-screw extruder is 135 ℃,165 ℃,180 ℃,190 ℃,200 ℃,210 ℃,215 ℃ and 220 ℃ in sequence. The main screw speed was set at 400r/min and the water bath temperature was 40 ℃.
Comparative example 2
In order to contrast with the embodiment 2, the invention better embodies the improvement effect of the vertical gas cyclone separation process of the polyester-cotton staple fibers on the performance of the polyester-staple-fiber reinforced polyolefin composite in the preparation method of the regenerated modified polyester-staple-fiber reinforced polyolefin composite, and the corresponding comparative embodiment 2 directly adopts the fiber floc treated by physical crushing and wet centrifugal separation process to directly carry out filling modification on the polypropylene material, and mainly comprises the following specific implementation steps:
according to the parts by weight, the steps are directly and directly adopted to prepare the regenerated modified polyester staple fiber reinforced polypropylene compound modified material by melting, extruding, cooling and granulating the fiber floccule, the antioxidant, the toner and the polypropylene resin which are treated by the first physical crushing part and the second wet centrifugal separation process through a double-screw extruder, and the performance of the modified material is evaluated.
The processing set temperature of the I-X region of the double-screw extruder is 135 ℃,165 ℃,180 ℃,190 ℃,200 ℃,210 ℃,210 ℃,215 ℃,215 ℃ and 220 ℃ in sequence. The main screw speed was set at 400r/min and the water bath temperature was 40 ℃.
Comparative example 3
In order to contrast with the embodiment 2, the method for preparing the regenerated modified polyester staple fiber reinforced polypropylene composite better embodies the improvement effect of the surface passivation modification treatment of the polyester staple fiber on the performance of the reinforced polyester staple fiber composite, and the corresponding comparative example 3 directly adopts the fiber floccule which is crushed and subjected to wet centrifugal separation process and vertical gas cyclone separation process to directly carry out filling modification on the polypropylene material, and mainly comprises the following specific implementation steps:
according to parts by weight, the steps are directly adopted in comparative example 3, and fiber flocculent fiber, antioxidant, toner and polypropylene resin treated by a wet centrifugal separation process and a vertical gas cyclone separation process are directly adopted, melted by a double screw extruder, extruded, cooled and pelletized, so that the regenerated modified polyester staple fiber reinforced polypropylene compound modified material is prepared, and related material performance evaluation is carried out.
The processing set temperature of the I-X region of the double-screw extruder is 135 ℃,165 ℃,180 ℃,190 ℃,200 ℃,210 ℃,210 ℃,215 ℃,215 ℃ and 220 ℃ in sequence. The main screw speed was set at 400r/min and the water bath temperature was 40 ℃.
Comparative example 4
In order to better embody the performance advantages of the regenerated modified polyester staple fiber reinforced polypropylene compound in comparison with the embodiment 2, the corresponding comparative example 4 directly adopts talcum powder commonly used in the field of the current automobile modified material industry to directly carry out filling modification on a polypropylene material, and mainly comprises the following specific implementation steps:
according to the parts by weight, the steps are directly adopted for talcum powder, antioxidant, toner and polypropylene resin with the mesh number of 3000 which are commonly used in the automobile industry, melted by a double screw extruder, extruded, cooled and pelletized, so as to prepare the talcum powder reinforced polypropylene composite modified material, and the performance of the relevant material is evaluated.
The processing set temperature of the I-X region of the double-screw extruder is 135 ℃,165 ℃,180 ℃,190 ℃,200 ℃,210 ℃,210 ℃,215 ℃,215 ℃ and 220 ℃ in sequence. The main screw speed was set at 400r/min and the water bath temperature was 40 ℃.
Comparative example 5
In order to better embody the performance advantages of the regenerated modified polyester staple fiber reinforced polypropylene composite of the invention in comparison with the embodiment 2, the corresponding comparative example 4 directly adopts glass fiber commonly used in the field of the current automobile modified material industry to directly carry out filling modification on a polypropylene material, and mainly comprises the following specific implementation steps:
according to the parts by weight, the steps are directly and directly adopted for glass fiber with the fiber diameter of 13um, an antioxidant, toner and polypropylene resin which are commonly used in the automobile industry, and the glass fiber reinforced polypropylene compound modified material is prepared through melting, extruding, cooling and granulating by a double screw extruder, and the performance of the related material is evaluated.
The processing set temperature of the I-X region of the double-screw extruder is 135 ℃,165 ℃,180 ℃,190 ℃,200 ℃,210 ℃,210 ℃,215 ℃,215 ℃ and 220 ℃ in sequence. The main screw speed was set at 400r/min and the water bath temperature was 40 ℃.
The reinforced modified polypropylene composite materials prepared in examples 1 to 7 and the corresponding comparative examples 1 to 5 were subjected to performance tests according to the test standards and conditions shown in Table 3 below, the treatment process and formulation information of the reinforced modified polypropylene products in examples 1 to 7 and comparative examples 1 to 5 are shown in Table 4, the test performance of the reinforced modified polypropylene products in examples 1 to 7 and comparative examples 1 to 5 are shown in Table 5, and the performance-versus-properties of the modified polypropylene materials prepared in examples 2 and comparative examples 1 to 5 are shown in Table 6.
Performance test criteria and conditions for the reinforced polypropylene composites prepared in Table 3
| Sequence number | Inspection index | Inspection method | Unit (B) | 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 examples 1 to 7 and comparative examples 1 to 5 reinforced modified polypropylene products treatment process and formulation information
TABLE 5 influence of average length of PET fibers on the Properties of modified Polypropylene materials in examples 1 to 7
Remarks: for screening out the appropriate modified fiber length.
TABLE 6 comparison of Properties of the modified Polypropylene materials prepared in example 2 and comparative examples 1 to 5
Table 4 shows the treatment process and formulation information of the reinforced modified polypropylene products of examples 1 to 7 and comparative examples 1 to 5, and Table 5 shows the influence of the average length of the PET fibers on the performance of the modified polypropylene material of examples 1 to 7, and 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 fibers, mainly because on one hand, the reinforcing effect of the PET fibers on the polypropylene resin is increased along with the increase of the average length of the regenerated PET fibers, the tensile strength and the impact strength of the final modified polypropylene product are increased, but when the average length of the PET fibers is increased to 1.5mm, the own purity of the PET fibers/cotton fibers is reduced, the compatibility of the PET fibers and the polypropylene matrix resin is influenced, and finally the impact performance of the product is obviously reduced, so that it is important how to balance the average length of the PET fibers and the final mechanical performance of the final modified polypropylene product.
To further verify the inventive effects of the present invention, the inventive effects of the present invention patent were fully verified by comparing the properties of the modified polypropylene materials prepared in example 2 and comparative examples 1 to 5 of table 6, and as shown in table 6, the wet centrifugation and suspension air flow separation process in the present technical scheme is advantageous to increase the purity of the PET staple fibers prepared by the dry crushing process, reduce the content of cotton fibers and related impurities affecting the properties of the final modified polypropylene product, and thus improve the mechanical properties, particularly the improvement in impact properties, of the final modified product. In addition, as shown in the test data in table 6, the compatibility of the PET fiber and the polypropylene resin is improved by introducing the fiber surface passivation treatment process, and the impact performance of the final product is obviously improved.
The regenerated modified polyester staple fiber reinforced polypropylene compound prepared by the method shown in the example 2 and the comparative examples 4 and 5-6 in the table 6 achieves low carbon and green circulation industry appeal, and has better material strength and lower material density advantage compared with mineral talcum powder filling commonly used in the automobile industry, and compared with the conventional short glass fiber reinforced polypropylene material, the regenerated modified polyester staple fiber reinforced polypropylene compound prepared by the method has lower material density when the material strength is close, can be used for completely or partially replacing glass fibers or mineral reinforced polypropylene materials, and provides a brand new innovative application for realizing the recycling of waste clothes in the application fields of the automobile modified polypropylene materials and related modified materials.
Claims (8)
1. The preparation method of the waste polyester cotton fabric modified reinforced polypropylene composite material is characterized by comprising the following raw materials in parts by weight: 10 to 40 parts of regenerated modified polyester staple fiber, 0.1 to 3.0 parts of antioxidant and toner, and 60 to 90 parts of polypropylene resin; the polypropylene resin refers to polypropylene with the material flow speed of 0.5-120 g/10min under the condition of 230 ℃ and 2.16 Kg; the antioxidant is at least one of antioxidant 1010 (tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] 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%, and the average length of the fiber is 0.5 mm-5.0 mm;
the preparation method 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 recycled polyester-cotton blended fabric to obtain regenerated modified polyester staple fibers;
the wet centrifugation operation 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 PET short fiber and wet state density of the polyester staple are 1.50-1.58 g/cm 3 Cotton fibers of (a);
coarsening PET short fibers subjected to vertical gas cyclone separation, carrying out surface treatment passivation through a solution containing alkylsilane, and drying to prepare modified regenerated PET fibers; the alkali solution for roughening treatment is 1-5% NaOH solution, the treatment temperature is 50-90 ℃, and the treatment time is 40-120 minutes.
2. The method of manufacturing of claim 1, further comprising the steps of:
step s2, preparation of a polypropylene compound: melting 10-40 parts of regenerated modified polyester staple fibers obtained in the step s1, 0.1-3.0 parts of antioxidant and toner, and the balance of polypropylene PP resin raw materials through 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 region of the double-screw extruder is 135 ℃,165 ℃,180 ℃,190 ℃,200 ℃,210 ℃,215 ℃,220 ℃ and the main screw rotating speed is 300-500 r/min, and the water tank temperature is 23-50 ℃.
3. The method of claim 2, wherein in step s1, the dry physical disruption is performed as follows: and (3) cleaning the recovered pure polyester or polyester-cotton blended fabric through a clear water tank, acidizing the fabric in a sulfuric acid tank, drying the fabric, and crushing the fabric for a plurality of times through a crusher to obtain a PET/cotton fiber flocculent mixture with the fiber length of 0.5-5.0 mm.
4. The preparation method of claim 3, wherein the sulfuric acid tank is a dilute sulfuric acid solution with a sulfuric acid solution concentration of 20% -50%, and the treatment time is generally 4-12 hours.
5. A method of making as claimed in claim 3 wherein the PET/cotton fiber batt blend has a fiber length of 0.5mm to 1.5mm.
6. The process according to claim 3, wherein in step s1, a PET/cotton fiber flocculent mixture having a PET purity of 93% or more is obtained by vertical gas cyclone separation.
7. The method of claim 1, wherein the alkylsiloxane is a dodecane to octadecyltrimethoxysilane.
8. The method of claim 1, wherein the passivation temperature is between 30 ℃ and 60 ℃.
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