CN113480845B - Regenerated PA plastic particle prepared from waste cloth and method thereof - Google Patents

Regenerated PA plastic particle prepared from waste cloth and method thereof Download PDF

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CN113480845B
CN113480845B CN202110804381.9A CN202110804381A CN113480845B CN 113480845 B CN113480845 B CN 113480845B CN 202110804381 A CN202110804381 A CN 202110804381A CN 113480845 B CN113480845 B CN 113480845B
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calcium carbonate
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CN113480845A (en
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游义
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Jiangxi Mingxin Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2237—Oxides; Hydroxides of metals of titanium
    • C08K2003/2241—Titanium dioxide
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C08K2003/265—Calcium, strontium or barium carbonate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
    • C08L2205/16—Fibres; Fibrils
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2207/00—Properties characterising the ingredient of the composition
    • C08L2207/20—Recycled plastic
    • 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

Abstract

The invention discloses a regenerated PA plastic particle prepared by utilizing waste cloth and a method thereof, relating to the technical field of plastics and comprising the following raw materials in parts by weight: 50-70 parts of waste polyamide fabric, 10-20 parts of polyamide resin, 0.6-0.8 part of modified nano calcium carbonate, 1-3 parts of lignin fiber, 3-5 parts of modified polytetrafluoroethylene wax emulsion, 0.5-0.7 part of modified nano kaolin, 1-3 parts of calcium lignosulfonate, 2-4 parts of oxidized polyethylene wax, 2-4 parts of sorbitol and 2-5 parts of 2, 6-di-tert-butyl-4-methylphenol. The invention has the advantages that the waste cloth is recycled, the utilization rate of the waste textile is improved, the production cost is reduced, the mechanical strength, the toughness, the hydrophobicity and the like of the regenerated PA plastic particles are improved by adding other auxiliary agents into the raw materials, and the obtained PA plastic particles have excellent product performance and remarkable reprocessing capability.

Description

Regenerated PA plastic particle prepared from waste cloth and method thereof
Technical Field
The invention relates to the technical field of plastics, in particular to regenerated PA plastic particles prepared by utilizing waste cloth and a method thereof.
Background
As is well known, with the development of science and technology, the market share of clothes made of synthetic fibers is continuously expanded, and the economic productivity is increasingly increased. Meanwhile, because of the updating of the clothes, a large amount of waste clothes become solid waste every year, and the solid waste is difficult to completely degrade in a natural state, thereby bringing huge environmental burden. At present, the waste clothes are recycled mainly by processing the waste clothes to manufacture a mop for reuse or selling, but the mode has low productivity, narrow audience, low economic benefit and limited consumption of the waste clothes. Therefore, there is a need to expand the utilization of such waste clothes, enhance productivity, increase economic efficiency, and reduce environmental burden.
The plastic particles have wide application, low price and simple and convenient processing, are popular in the market, have ever-expanding market share, and cause great environmental pollution by plastic wastes along with ever-increasing plastic yield, so the plastic particles are particularly important for recycling the plastics. At present, the raw materials adopted for recycling the plastics are mainly various plastic products, such as agricultural films, woven bags, convenient bags, beverage bottles, plastic tubs, old sandals and the like, so as to prepare the plastic particles. The utilization rate of the huge amount of synthetic fiber clothing waste is still low despite that the synthetic fiber clothing waste is also a high polymer component such as PA, PC, PET and the like.
Chinese patent CN104928918A discloses a method for recovering waste cloth from clothing, which specifically comprises: selecting waste cloth, cutting into strips, soaking in disinfectant, and washing with clear water; soaking the waste cloth in a cleaning solution, and then cleaning the waste cloth with clean water; treating waste cloth at 105-110 ℃; soaking the cloth with the medicinal liquid; and (5) drying the cloth to prepare the mop. However, the method for utilizing waste cloth in the patent has low productivity, narrow audience, low economic benefit and limited consumption of waste clothes.
Chinese patent CN105643838A discloses a production process of recycled plastic particles, which comprises the steps of classifying waste plastics, crushing the waste plastics, and then removing iron; then washing the pretreated waste plastics in a subarea manner, and then drying; and finally, extruding, drawing, cooling and granulating to prepare a finished product of the regenerated plastic particles. However, the regenerated plastic particles prepared by the patent still traditionally adopt waste plastics as raw materials, the raw material source of the regenerated plastic particles is not increased, and the market homogenization phenomenon is obvious.
Chinese patent CN 106497025 a discloses a regenerated PA plastic particle prepared from waste cloth and a preparation method thereof, wherein the waste cloth of nylon material is sterilized, cut into pieces, and extruded with an auxiliary agent and new PA particles to prepare the regenerated PA plastic particle, but the prepared regenerated PA plastic particle has poor mechanical strength, toughness and hydrophobic property.
Disclosure of Invention
The invention aims to at least solve one of the technical problems in the prior art and provides a regenerated PA plastic particle prepared by using waste cloth and a method thereof.
The technical solution of the invention is as follows:
a regenerated PA plastic particle prepared by using waste cloth comprises the following raw materials in parts by weight: 50-70 parts of waste polyamide fabric, 10-20 parts of polyamide resin, 0.6-0.8 part of modified nano calcium carbonate, 1-3 parts of lignin fiber, 3-5 parts of modified polytetrafluoroethylene wax emulsion, 0.5-0.7 part of modified nano kaolin, 1-3 parts of calcium lignosulfonate, 2-4 parts of oxidized polyethylene wax, 2-4 parts of sorbitol and 2-5 parts of 2, 6-di-tert-butyl-4-methylphenol.
Preferably, the feed comprises the following raw materials in parts by weight: 55-65 parts of waste polyamide fabric, 12-18 parts of polyamide resin, 0.65-0.75 part of modified nano calcium carbonate, 1.5-2.5 parts of lignin fiber, 3.5-4.5 parts of modified polytetrafluoroethylene wax emulsion, 0.55-0.65 part of modified nano kaolin, 1.5-2.5 parts of calcium lignosulfonate, 2.5-3.5 parts of oxidized polyethylene wax, 2.5-3.5 parts of sorbitol and 3-4 parts of 2, 6-di-tert-butyl-4-methylphenol.
Preferably, the feed comprises the following raw materials in parts by weight: 60 parts of waste polyamide fabric, 15 parts of polyamide resin, 0.7 part of modified nano calcium carbonate, 2 parts of lignin fiber, 4 parts of modified polytetrafluoroethylene wax emulsion, 0.6 part of modified nano kaolin, 2 parts of calcium lignosulfonate, 3 parts of oxidized polyethylene wax, 3 parts of sorbitol and 3.5 parts of 2, 6-di-tert-butyl-4-methylphenol.
Preferably, the particle size of the modified nano kaolin and the modified nano calcium carbonate is less than 10 nm.
Preferably, the modified polytetrafluoroethylene wax emulsion comprises the following raw materials in parts by weight: 1-3 parts of 1H,1H,2H, 2H-perfluorooctyl trichlorosilane, 2-5 parts of difluoromethyltrimethylsilane, 0.1-0.5 part of polydimethylsiloxane and 20-40 parts of polytetrafluoroethylene wax emulsion.
Preferably, the preparation method of the modified polytetrafluoroethylene wax emulsion comprises the following steps: adding 1H,1H,2H, 2H-perfluoro octyl trichlorosilane, polydimethylsiloxane and difluoromethyl trimethylsilane into the polytetrafluoroethylene wax emulsion, dispersing for 6-10H at the temperature of 60-70 ℃, and naturally cooling.
Preferably, the preparation method of the modified nano kaolin comprises the following steps: adding 1g of nano kaolin into 50-55 ml of distilled water, placing the mixture in an ice water bath condition, adding 4-5 ml of concentrated hydrochloric acid while stirring, and dripping 9-10 ml of TiCl with the concentration of 1-2 mol/L 4 Adding the solution into the mixture, and then continuously adding 9-10 ml of the solution with the concentration of 1-2 molMixing and stirring an ammonium sulfate solution/L, heating the mixture to 90-100 ℃ in a water bath, and preserving heat for 30-60 min; and then dropwise adding ammonia water until the pH value is 7, filtering, washing and drying at 75-85 ℃ to obtain the modified nano kaolin.
Preferably, the preparation method of the modified nano calcium carbonate comprises the following steps: adding 1g of nano calcium carbonate and 8-9 g of urea into 50-55 ml of distilled water, adding a small amount of dispersant, dropwise adding 5-6 ml of titanium sulfate solution with the concentration of 0.2-0.3 mol/L under the condition of stirring at 80-85 ℃, continuing to react for 30-60 min after dropwise adding, cooling, carrying out suction filtration and washing, and drying at 75-80 ℃ to obtain composite powder; uniformly mixing 9-10 parts by mass of composite powder, 1-1.2 parts by mass of vinyltriethoxysilane, 1-3 parts by mass of acrylic monomer and 0.1-0.12 part by mass of initiator, and performing ball milling to uniformly mix the mixture to obtain the modified nano calcium carbonate.
A preparation method of regenerated PA plastic particles prepared by using waste cloth comprises the following steps:
s1, sterilizing and disinfecting the waste polyamide cloth, and then cutting the waste polyamide cloth into particles with the average particle size of 5-10 mm; adding the particles into water, adding a decoloring agent, heating until the water is boiled to fully decolor the particles, and drying the particles;
s2, dispersing the modified nano calcium carbonate and the modified nano kaolin in the modified polytetrafluoroethylene emulsion, soaking for 2-3 h, filtering to remove redundant emulsion, and dispersing and drying the treated modified nano calcium carbonate and the treated modified nano kaolin;
s3, adding the lignin fibers into ammonia water to be soaked for 40-60 min, taking out, washing with water, and drying; then adding the mixture into ester quaternary ammonium salt to be soaked for 10-20 min, and then dehydrating and drying;
s4, uniformly mixing the lignin fiber processed in the step S3 with the modified nano calcium carbonate and the modified nano kaolin processed in the step S2 to obtain a mixture;
and S5, uniformly mixing the particles obtained in the step S1 and the mixture obtained in the step S4 with polyamide resin, calcium lignosulfonate, oxidized polyethylene wax, sorbitol and 2, 6-di-tert-butyl-4-methylphenol, extruding and shearing for 20-30 min, and then extruding, cooling and granulating through a screw extrusion device to obtain the regenerated PA plastic particles.
The invention has at least one of the following beneficial effects:
1. the invention utilizes the waste cloth to prepare the regenerated plastic particles, thereby developing the recycling field of the waste cloth, improving the utilization rate of the waste textiles, reducing the production cost, relieving the contradiction between supply and demand of the textile product market and reducing the environmental pollution of the light textile industry.
2. The modified nano calcium carbonate is prepared by reacting urea and titanium sulfate to generate titanium dioxide, the surface of the titanium dioxide is modified with nano calcium carbonate to generate calcium carbonate/titanium dioxide composite powder, and further, the surface of the calcium carbonate/titanium dioxide composite powder is subjected to surface grafting modification treatment through an acrylic acid monomer, so that the binding force between the calcium carbonate/titanium dioxide composite powder and polyamide can be enhanced, and the agglomeration among the nano calcium carbonate is reduced. The modified nano kaolin of the invention adopts TiCl 4 Treating kaolin with ammonium sulfate, TiCl 4 And ammonium sulfate to produce titanium dioxide, and the titanium dioxide and kaolin react to produce the kaolin/titanium dioxide composite material. The kaolin has good plasticity and fire resistance, and the nano calcium carbonate can improve the plastic particle rheology and improve the moldability; the composite material has the functions of toughening and reinforcing, can improve the bending strength, the bending elastic modulus, the thermal deformation temperature and the dimensional stability of plastics, and has the advantages of good glossiness, strong dispersibility, large covering power, weather resistance and antibacterial effect of titanium dioxide.
3. The modified polytetrafluoroethylene wax emulsion is modified by 1H,1H,2H, 2H-perfluorooctyltrichlorosilane, difluoromethyltrimethylsilane and cyclomethicone, and has strong hydrophobicity, so that the hydrophobicity of PA plastic particles can be improved when the modified polytetrafluoroethylene wax emulsion is added in raw materials.
4. The preparation method comprises the steps of dispersing the modified nano calcium carbonate and the modified nano kaolin in the modified polytetrafluoroethylene emulsion, so that the polytetrafluoroethylene emulsion is attached to the surfaces of the modified nano calcium carbonate and the modified nano kaolin, and is mixed with other raw materials together with the modified nano calcium carbonate and the modified nano kaolin, so that the polytetrafluoroethylene emulsion can be uniformly dispersed in the polyamide resin, the dispersion effect of the polytetrafluoroethylene emulsion is improved, and the improvement of the hydrophobicity of the PA plastic particles is facilitated finally.
5. According to the preparation method, the lignin fiber is soaked in the ammonia water, so that the toughness of the lignin fiber can be improved, and the tensile property of the plastic particles is improved; furthermore, the lignin fiber is added into the esterquat, so that the compatibility of the lignin fiber with other raw materials is improved, the lignin fiber can be uniformly dispersed in other raw materials, and the agglomeration of the lignin fiber is reduced.
Detailed Description
The present invention will be described in further detail with reference to the following examples, but the present invention is not limited to the following examples.
The waste and old polyamide fabrics used in the following examples and comparative examples are the same batch of fabric with the same components.
Example 1
A regenerated PA plastic particle prepared by utilizing waste cloth comprises the following raw materials in parts by weight: 50 parts of waste polyamide fabric, 10 parts of polyamide resin, 0.6 part of modified nano calcium carbonate, 1 part of lignin fiber, 3 parts of modified polytetrafluoroethylene wax emulsion, 0.5 part of modified nano kaolin, 1 part of calcium lignosulfonate, 2 parts of oxidized polyethylene wax, 2 parts of sorbitol and 2 parts of 2, 6-di-tert-butyl-4-methylphenol.
Wherein the particle size of the modified nano kaolin and the modified nano calcium carbonate is less than 10 nm.
The modified polytetrafluoroethylene wax emulsion comprises the following raw materials in parts by weight: 1 part of 1H,1H,2H, 2H-perfluorooctyl trichlorosilane, 2 parts of difluoromethyltrimethylsilane, 0.1 part of polydimethylsiloxane and 20 parts of polytetrafluoroethylene wax emulsion. The preparation method comprises the following steps: adding 1H,1H,2H, 2H-perfluorooctyl trichlorosilane, polydimethylsiloxane and difluoromethyltrimethylsilane into the polytetrafluoroethylene wax emulsion, dispersing for 10H at the temperature of 60 ℃, and naturally cooling.
The preparation method of the modified nano kaolin comprises the following steps: adding 1g of nano kaolin into 50ml of distilled water, adding 4ml of concentrated hydrochloric acid while stirring under the condition of ice-water bath, and dripping 9ml of TiCl with the concentration of 1mol/L 4 Continuing adding 9ml of ammonium sulfate solution with the concentration of 1mol/L, mixing and stirring, heating the mixture to 90 ℃ in a water bath, and preserving heat for 60 min; then ammonia water is dripped until the pH value is 7, and the modified nano kaolin is obtained after filtration, washing and drying at the temperature of 75 ℃.
The preparation method of the modified nano calcium carbonate comprises the following steps: adding 1g of nano calcium carbonate and 8g of urea into 50ml of distilled water, adding a small amount of dispersant sodium dodecyl benzene sulfonate, dropwise adding 5ml of titanium sulfate solution with the concentration of 0.2mol/L under the condition of stirring at 80 ℃, continuing to react for 60min after the dropwise adding is finished, cooling, carrying out suction filtration, washing, and drying at 75 ℃ to obtain composite powder; and (2) uniformly mixing 9 parts by mass of the composite powder, 1 part by mass of vinyltriethoxysilane, 1 part by mass of acrylic acid monomer and 0.1 part by mass of initiator peroxyglutaric acid, and performing ball milling and uniform mixing to obtain the modified nano calcium carbonate.
A preparation method of regenerated PA plastic particles prepared by using waste cloth comprises the following steps:
s1, sterilizing and disinfecting the waste polyamide cloth, and then cutting the waste polyamide cloth into particles with the average particle size of 5-10 mm; adding the particles into water, adding a decoloring agent, heating until the water is boiled to fully decolor the particles, and drying the particles;
s2, dispersing the modified nano calcium carbonate and the modified nano kaolin into the modified polytetrafluoroethylene emulsion, soaking for 2 hours, then filtering to remove redundant emulsion, and dispersing and drying the treated modified nano calcium carbonate and the modified nano kaolin;
s3, adding the lignin fibers into ammonia water to be soaked for 40min, taking out, washing with water, and drying; then adding into ester quaternary ammonium salt to soak for 10min, then dehydrating and drying;
s4, uniformly mixing the lignin fiber processed in the step S3 with the modified nano calcium carbonate and the modified nano kaolin processed in the step S2 to obtain a mixture;
s5, uniformly mixing the granules obtained in the step S1 and the mixture obtained in the step S4 with polyamide resin, calcium lignosulfonate, oxidized polyethylene wax, sorbitol and 2, 6-di-tert-butyl-4-methylphenol, extruding and shearing for 20min, and then extruding, cooling and granulating through a screw extrusion device to obtain the regenerated PA plastic granules.
Example 2
The regenerated PA plastic particle prepared by using waste cloth preferably comprises the following raw materials in parts by weight: 55 parts of waste polyamide fabric, 12 parts of polyamide resin, 0.65 part of modified nano calcium carbonate, 1.5 parts of lignin fiber, 3.5 parts of modified polytetrafluoroethylene wax emulsion, 0.55 part of modified nano kaolin, 1.5 parts of calcium lignosulfonate, 2.5 parts of oxidized polyethylene wax, 2.5 parts of sorbitol and 3 parts of 2, 6-di-tert-butyl-4-methylphenol.
Wherein the particle size of the modified nano kaolin and the modified nano calcium carbonate is less than 10 nm.
The modified polytetrafluoroethylene wax emulsion comprises the following raw materials in parts by weight: 2 parts of 1H,1H,2H, 2H-perfluorooctyl trichlorosilane, 3 parts of difluoromethyltrimethylsilane, 0.2 part of polydimethylsiloxane and 25 parts of polytetrafluoroethylene wax emulsion. The preparation method comprises the following steps: adding 1H,1H,2H, 2H-perfluorooctyl trichlorosilane, polydimethylsiloxane and difluoromethyltrimethylsilane into the polytetrafluoroethylene wax emulsion, dispersing for 9H at the temperature of 62 ℃, and naturally cooling.
The preparation method of the modified nano kaolin comprises the following steps: mixing 1g of nano kaolinAdding soil into 52ml distilled water, placing in ice water bath, adding 4.5ml concentrated hydrochloric acid while stirring, and adding dropwise 9.2ml TiCl with concentration of 1.5mol/L 4 Continuously adding 9.2ml of ammonium sulfate solution with the concentration of 1-2 mol/L into the solution, mixing and stirring, heating the mixture to 92 ℃ in a water bath, and preserving the heat for 40 min; then ammonia water is dripped until the pH value is 7, and the modified nano kaolin is obtained after filtration, washing and drying at 78 ℃.
The preparation method of the modified nano calcium carbonate comprises the following steps: adding 1g of nano calcium carbonate and 8.2g of urea into 51ml of distilled water, adding a small amount of dispersant sodium dodecyl benzene sulfonate, dropwise adding 5.2ml of titanium sulfate solution with the concentration of 0.25mol/L under the condition of stirring at 81 ℃, continuing to react for 40min after the dropwise addition is finished, cooling, performing suction filtration, washing, and drying at 76 ℃ to obtain composite powder; uniformly mixing 9.2 parts by mass of composite powder, 1 part by mass of vinyltriethoxysilane, 1.5 parts by mass of acrylic monomer and 0.1 part by mass of initiator peroxyglutaric acid, and performing ball milling to uniformly mix the mixture to obtain the modified nano calcium carbonate.
A preparation method of regenerated PA plastic particles prepared by using waste cloth comprises the following steps:
s1, sterilizing and disinfecting the waste polyamide cloth, and then cutting the waste polyamide cloth into particles with the average particle size of 5-10 mm; adding the particles into water, adding a decoloring agent, heating until the water is boiled to decolor the particles fully, and drying the particles;
s2, dispersing the modified nano calcium carbonate and the modified nano kaolin into the modified polytetrafluoroethylene emulsion, soaking for 2.5 hours, then filtering to remove redundant emulsion, and dispersing and drying the treated modified nano calcium carbonate and the modified nano kaolin;
s3, adding the lignin fibers into ammonia water to be soaked for 50min, taking out, washing with water and drying; then adding into ester quaternary ammonium salt to soak for 15min, then dehydrating and drying;
s4, uniformly mixing the lignin fiber processed in the step S3 with the modified nano calcium carbonate and the modified nano kaolin processed in the step S2 to obtain a mixture;
s5, uniformly mixing the granules obtained in the step S1 and the mixture obtained in the step S4 with polyamide resin, calcium lignosulfonate, oxidized polyethylene wax, sorbitol and 2, 6-di-tert-butyl-4-methylphenol, extruding and shearing for 25min, and then extruding, cooling and granulating through a screw extrusion device to obtain the regenerated PA plastic granules.
Example 3
A regenerated PA plastic particle prepared by using waste cloth comprises the following raw materials in parts by weight: 60 parts of waste polyamide fabric, 15 parts of polyamide resin, 0.7 part of modified nano calcium carbonate, 2 parts of lignin fiber, 4 parts of modified polytetrafluoroethylene wax emulsion, 0.6 part of modified nano kaolin, 2 parts of calcium lignosulfonate, 3 parts of oxidized polyethylene wax, 3 parts of sorbitol and 3.5 parts of 2, 6-di-tert-butyl-4-methylphenol.
Wherein the particle size of the modified nano kaolin and the modified nano calcium carbonate is less than 10 nm.
The modified polytetrafluoroethylene wax emulsion comprises the following raw materials in parts by weight: 1.5 parts of 1H,1H,2H, 2H-perfluorooctyl trichlorosilane, 4 parts of difluoromethyltrimethylsilane, 0.3 part of polydimethylsiloxane and 30 parts of polytetrafluoroethylene wax emulsion. The preparation method comprises the following steps: adding 1H,1H,2H, 2H-perfluorooctyl trichlorosilane, polydimethylsiloxane and difluoromethyltrimethylsilane into the polytetrafluoroethylene wax emulsion, dispersing for 8H at the temperature of 65 ℃, and naturally cooling.
The preparation method of the modified nano kaolin comprises the following steps: adding 1g of nano kaolin into 53ml of distilled water, placing the mixture in an ice-water bath condition, adding 4.5ml of concentrated hydrochloric acid while stirring, and dripping 9.5ml of TiCl with the concentration of 1.5mol/L 4 Continuously adding 9.5ml of ammonium sulfate solution with the concentration of 1.5mol/L, mixing and stirring, heating the mixture to 95 ℃ in a water bath, and preserving the heat for 45 min; then ammonia water is dripped until the pH value is 7, and the modified nano kaolin is obtained after filtration, washing and drying at the temperature of 80 ℃.
The preparation method of the modified nano calcium carbonate comprises the following steps: adding 1g of nano calcium carbonate and 8.5g of urea into 53ml of distilled water, adding a small amount of dispersant sodium dodecyl benzene sulfonate, dropwise adding 5.5ml of titanium sulfate solution with the concentration of 0.25mol/L under the condition of stirring at 83 ℃, continuing to react for 45min after the dropwise addition is finished, cooling, performing suction filtration, washing, and drying at 77 ℃ to obtain composite powder; uniformly mixing 9.5 parts by mass of composite powder, 1.1 parts by mass of vinyltriethoxysilane, 2 parts by mass of acrylic monomer and 0.11 part by mass of initiator peroxyglutaric acid, and performing ball milling to uniformly mix the mixture to obtain the modified nano calcium carbonate.
A preparation method of regenerated PA plastic particles prepared by using waste cloth comprises the following steps:
s1, sterilizing and disinfecting the waste polyamide cloth, and then cutting the waste polyamide cloth into particles with the average particle size of 5-10 mm; adding the particles into water, adding a decoloring agent, heating until the water is boiled to decolor the particles fully, and drying the particles;
s2, dispersing the modified nano calcium carbonate and the modified nano kaolin in the modified polytetrafluoroethylene emulsion, soaking for 3 hours, filtering to remove redundant emulsion, and dispersing and drying the treated modified nano calcium carbonate and the treated modified nano kaolin;
s3, adding the lignin fibers into ammonia water to be soaked for 60min, taking out, washing with water and drying; then adding into ester quaternary ammonium salt to soak for 20min, then dehydrating and drying;
s4, uniformly mixing the lignin fiber treated in the step S3 with the modified nano calcium carbonate and the modified nano kaolin treated in the step S2 to obtain a mixture;
s5, uniformly mixing the granules obtained in the step S1 and the mixture obtained in the step S4 with polyamide resin, calcium lignosulfonate, oxidized polyethylene wax, sorbitol and 2, 6-di-tert-butyl-4-methylphenol, extruding and shearing for 30min, and then extruding, cooling and granulating through a screw extrusion device to obtain the regenerated PA plastic granules.
Example 4
A regenerated PA plastic particle prepared by utilizing waste cloth comprises the following raw materials in parts by weight: 65 parts of waste polyamide fabric, 18 parts of polyamide resin, 0.75 part of modified nano calcium carbonate, 2.5 parts of lignin fiber, 4.5 parts of modified polytetrafluoroethylene wax emulsion, 0.65 part of modified nano kaolin, 2.5 parts of calcium lignosulfonate, 3.5 parts of oxidized polyethylene wax, 3.5 parts of sorbitol and 4 parts of 2, 6-di-tert-butyl-4-methylphenol.
Wherein the particle size of the modified nano kaolin and the modified nano calcium carbonate is less than 10 nm.
The modified polytetrafluoroethylene wax emulsion comprises the following raw materials in parts by weight: 1-3 parts of 1H,1H,2H, 2H-perfluorooctyl trichlorosilane, 2-5 parts of difluoromethyltrimethylsilane, 0.1-0.5 part of polydimethylsiloxane and 20-40 parts of polytetrafluoroethylene wax emulsion. The preparation method comprises the following steps: adding 1H,1H,2H, 2H-perfluorooctyl trichlorosilane, polydimethylsiloxane and difluoromethyltrimethylsilane into the polytetrafluoroethylene wax emulsion, dispersing for 7H at the temperature of 68 ℃, and naturally cooling.
The preparation method of the modified nano kaolin comprises the following steps: adding 1g of nano kaolin into 54ml of distilled water, placing the mixture in an ice-water bath condition, adding 4.8ml of concentrated hydrochloric acid while stirring, and dripping 9.8ml of TiCl with the concentration of 1.5mol/L 4 Continuously adding 9.5ml of ammonium sulfate solution with the concentration of 1-2 mol/L into the solution, mixing and stirring, heating the mixture to 98 ℃ in a water bath, and preserving the temperature for 45 min; then ammonia water is dripped until the pH value is 7, and the modified nano kaolin is obtained after filtration, washing and drying at 82 ℃.
The preparation method of the modified nano calcium carbonate comprises the following steps: adding 1g of nano calcium carbonate and 8.8g of urea into 54ml of distilled water, adding a small amount of dispersant sodium dodecyl benzene sulfonate, dropwise adding 5.8ml of titanium sulfate solution with the concentration of 0.25mol/L under the condition of stirring at 84 ℃, continuously reacting for 50min after dropwise adding, cooling, carrying out suction filtration and washing, and drying at 79 ℃ to obtain composite powder; uniformly mixing 9.8 parts by mass of composite powder, 1.2 parts by mass of vinyltriethoxysilane, 2 parts by mass of acrylic monomer and 0.12 part by mass of initiator peroxyglutaric acid, and performing ball milling to uniformly mix the mixture to obtain the modified nano calcium carbonate.
A method for preparing regenerated PA plastic particles using waste cloth is the same as in example 1.
Example 5
A regenerated PA plastic particle prepared by utilizing waste cloth comprises the following raw materials in parts by weight: 70 parts of waste polyamide fabric, 20 parts of polyamide resin, 0.8 part of modified nano calcium carbonate, 3 parts of lignin fiber, 5 parts of modified polytetrafluoroethylene wax emulsion, 0.7 part of modified nano kaolin, 3 parts of calcium lignosulfonate, 4 parts of oxidized polyethylene wax, 4 parts of sorbitol and 5 parts of 2, 6-di-tert-butyl-4-methylphenol.
Wherein the particle size of the modified nano kaolin and the modified nano calcium carbonate is less than 10 nm.
The modified polytetrafluoroethylene wax emulsion comprises the following raw materials in parts by weight: 3 parts of 1H,1H,2H, 2H-perfluorooctyl trichlorosilane, 5 parts of difluoromethyltrimethylsilane, 0.5 part of polydimethylsiloxane and 40 parts of polytetrafluoroethylene wax emulsion.
The preparation method of the modified polytetrafluoroethylene wax emulsion comprises the following steps: adding 1H,1H,2H, 2H-perfluorooctyl trichlorosilane, polydimethylsiloxane and difluoromethyltrimethylsilane into the polytetrafluoroethylene wax emulsion, dispersing for 10H at the temperature of 70 ℃, and naturally cooling.
The preparation method of the modified nano kaolin comprises the following steps: adding 1g of nano kaolin into 55ml of distilled water, placing the mixture in an ice water bath condition, adding 5ml of concentrated hydrochloric acid while stirring, and dripping 10ml of TiCl with the concentration of 2mol/L 4 Continuously adding 10ml of ammonium sulfate solution with the concentration of 2mol/L, mixing and stirring, heating the mixture to 100 ℃ in a water bath, and preserving the heat for 60 min; then ammonia water is dripped until the pH value is 7, and the modified nano kaolin is obtained after filtration, washing and drying at the temperature of 85 ℃.
The preparation method of the modified nano calcium carbonate comprises the following steps: adding 1g of nano calcium carbonate and 9g of urea into 55ml of distilled water, adding a small amount of dispersant sodium dodecyl benzene sulfonate, dropwise adding 6ml of titanium sulfate solution with the concentration of 0.2mol/L under the condition of stirring at 85 ℃, continuing to react for 60min after the dropwise adding is finished, cooling, carrying out suction filtration, washing, and drying at 80 ℃ to obtain composite powder; uniformly mixing 10 parts by mass of composite powder, 1.2 parts by mass of vinyltriethoxysilane, 3 parts by mass of acrylic acid monomer and 0.12 part by mass of initiator peroxyglutaric acid, and performing ball milling to uniformly mix the mixture to obtain the modified nano calcium carbonate.
A method for preparing regenerated PA plastic particles using waste cloth is the same as in example 1.
Comparative example 1
The difference from example 1 is that: the raw materials are not added with modified nano calcium carbonate, lignin fiber, modified polytetrafluoroethylene wax emulsion and modified nano kaolin, and the rest is the same as the example 1.
Comparative example 2
The difference from example 1 is that: the raw material modified nano calcium carbonate, modified nano kaolin and modified polytetrafluoroethylene wax emulsion are not modified, that is, the raw material modified nano calcium carbonate, modified nano kaolin and modified polytetrafluoroethylene wax emulsion are respectively modified into nano calcium carbonate, nano kaolin and polytetrafluoroethylene wax emulsion, and the rest is the same as that in example 1.
Comparative example 3
The difference from example 1 is that: the raw material ratio is the same as that of example 1, and the preparation method of the regenerated PA plastic particles comprises the following steps:
steps S1 to S2 are the same as those in example 1, and modifications of S3 to S5 are:
and (3) uniformly mixing the particles obtained in the step (S1), the modified nano calcium carbonate and the modified nano kaolin which are treated in the step (S2), polyamide resin, lignin fiber, calcium lignosulfonate, oxidized polyethylene wax, sorbitol and 2, 6-di-tert-butyl-4-methylphenol, extruding and shearing for 20min, and then extruding, cooling and granulating by using a screw extrusion device to obtain the regenerated PA plastic particles.
Comparative example 4
The difference from example 1 is that: the raw material ratio is the same as that of example 1, and the preparation method of the regenerated PA plastic particles comprises the following steps:
steps S1 and S3 were modified from embodiments 1, S2 and S4 to S5 as follows:
and (3) uniformly mixing the particles obtained in the step (S1), the lignin fiber treated in the step (S3), polyamide resin, modified nano calcium carbonate, modified polytetrafluoroethylene emulsion, modified nano kaolin, calcium lignosulfonate, oxidized polyethylene wax, sorbitol and 2, 6-di-tert-butyl-4-methylphenol, extruding and shearing for 20min, and then extruding, cooling and granulating by using a screw extrusion device to obtain the regenerated PA plastic particles.
And (3) testing:
respectively carrying out injection molding on the regenerated plastic particles prepared in the examples 1-5 and the comparative examples 1-3 to obtain plastic sample strips with the same size, and testing the main mechanical properties and the hydrophobicity of the plastic sample strips, wherein the testing method and the standard are as follows: the test method comprises the following steps of (1) testing 5 plastic sample bars of each group of test samples by using a tensile strength GB/T1040-2006, a breaking elongation GB/T1040-2006, an impact strength GB/T1843-2008 and a bending strength GB/T9341-2000, and finally taking an average value as a final test result; hydrophobicity the contact angle CA was measured using a contact angle measuring instrument. The test results are shown in table 1:
TABLE 1
Figure BDA0003165839950000101
Figure BDA0003165839950000111
As can be seen from Table 1, the plastic sample bars prepared in examples 1-5 all have good tensile strength, elongation at break, impact strength, bending strength and hydrophobicity; as can be seen by comparing examples 1 to 5 with comparative examples 1 to 3, the tensile strength, elongation at break, impact strength and bending strength of the plastic sample strips prepared in examples 1 to 5 are significantly better than those of comparative example 1 (no modified nano calcium carbonate, lignin fiber, modified polytetrafluoroethylene wax emulsion and modified nano kaolin are added to the raw materials), comparative example 2 (no modified nano calcium carbonate, polytetrafluoroethylene wax emulsion and nano kaolin are used), comparative example 3 (different preparation methods) and comparative example 4 (different preparation methods), thereby indicating whether the nano calcium carbonate, lignin fiber, modified polytetrafluoroethylene wax emulsion and modified nano kaolin are added to the raw materials and whether the nano calcium carbonate, polytetrafluoroethylene wax emulsion and nano kaolin and the preparation methods affect the tensile strength, elongation at break, impact strength, tensile strength, bending strength and bending strength of the plastic sample strips, And (3) bending strength. The water contact angle CA of the plastic sample strips prepared in the examples 1-5 is also larger than that of the comparative examples 1-3, so that whether the modified polytetrafluoroethylene wax emulsion and the like are added into the raw materials or not and the mixing mode of the modified polytetrafluoroethylene wax emulsion and other raw materials in the preparation method can also influence the hydrophobicity of the plastic sample strips.
The above are merely characteristic embodiments of the present invention, and do not limit the scope of the present invention in any way. All technical solutions formed by equivalent exchanges or equivalent substitutions fall within the protection scope of the present invention.

Claims (5)

1. The regenerated PA plastic particles prepared from waste cloth are characterized by comprising the following raw materials in parts by weight: 50-70 parts of waste polyamide fabric, 10-20 parts of polyamide resin, 0.6-0.8 part of modified nano calcium carbonate, 1-3 parts of lignin fiber, 3-5 parts of modified polytetrafluoroethylene wax emulsion, 0.5-0.7 part of modified nano kaolin, 1-3 parts of calcium lignosulfonate, 2-4 parts of oxidized polyethylene wax, 2-4 parts of sorbitol and 2-5 parts of 2, 6-di-tert-butyl-4-methylphenol;
the modified polytetrafluoroethylene wax emulsion comprises the following raw materials in parts by weight: 1 to 3 parts of 1H,1H,2H, 2H-perfluorooctyl trichlorosilane, 2 to 5 parts of difluoromethyltrimethylsilane, 0.1 to 0.5 part of polydimethylsiloxane and 20 to 40 parts of polytetrafluoroethylene wax emulsion; the preparation method of the modified polytetrafluoroethylene wax emulsion comprises the following steps: adding 1H,1H,2H, 2H-perfluorooctyl trichlorosilane, polydimethylsiloxane and difluoromethyltrimethylsilane into the polytetrafluoroethylene wax emulsion, dispersing at the temperature of 60-70 ℃ for 6-10H, and naturally cooling;
the preparation method of the modified nano kaolin comprises the following steps: adding 1g of nano kaolin into 50-55 ml of distilled water, placing the mixture in an ice-water bath condition, adding 4-5 ml of concentrated hydrochloric acid while stirring, and dripping 9-10 ml of 1-2 mol/L TiCl 4 Continuously adding 9-10 ml of ammonium sulfate solution with the concentration of 1-2 mol/L, mixing and stirring, heating the mixture to 90-100 ℃ in a water bath, and preserving heat for 30-60 min; then, dropwise adding ammonia water until the pH value is 7, filtering, washing, and drying at 75-85 ℃ to obtain modified nano kaolin;
the preparation method of the modified nano calcium carbonate comprises the following steps: adding 1g of nano calcium carbonate and 8-9 g of urea into 50-55 ml of distilled water, adding a small amount of dispersing agent, dropwise adding 5-6 ml of titanium sulfate solution with the concentration of 0.2-0.3 mol/L under the condition of stirring at 80-85 ℃, continuing to react for 30-60 min after dropwise adding is finished, cooling, carrying out suction filtration, washing, and drying at 75-80 ℃ to obtain composite powder; uniformly mixing 9-10 parts by mass of composite powder, 1-1.2 parts by mass of vinyltriethoxysilane, 1-3 parts by mass of acrylic monomer and 0.1-0.12 part by mass of initiator, and performing ball milling to uniformly mix the mixture to obtain modified nano calcium carbonate;
the preparation method comprises the following steps:
s1, sterilizing and disinfecting the waste polyamide cloth, and then cutting the waste polyamide cloth into particles with the average particle size of 5-10 mm; adding the particles into water, adding a decoloring agent, heating until the water is boiled to decolor the particles fully, and drying the particles;
s2, dispersing the modified nano calcium carbonate and the modified nano kaolin into the modified polytetrafluoroethylene emulsion, soaking for 2-3 h, then filtering to remove redundant emulsion, and dispersing and drying the treated modified nano calcium carbonate and the modified nano kaolin;
s3, adding the lignin fibers into ammonia water to be soaked for 40-60 min, taking out, washing with water, and drying; then adding the mixture into ester quaternary ammonium salt to be soaked for 10-20 min, and then dehydrating and drying;
s4, uniformly mixing the lignin fiber treated in the step S3 with the modified nano calcium carbonate and the modified nano kaolin treated in the step S2 to obtain a mixture;
s5, uniformly mixing the particles obtained in the step S1 and the mixture obtained in the step S4 with polyamide resin, calcium lignosulfonate, oxidized polyethylene wax, sorbitol and 2, 6-di-tert-butyl-4-methylphenol, extruding and shearing for 20-30 min, and then extruding, cooling and granulating through a screw extrusion device to obtain the regenerated PA plastic particles.
2. The recycled PA plastic particle prepared from waste cloth according to claim 1, which comprises the following raw materials in parts by weight: 55-65 parts of waste polyamide fabric, 12-18 parts of polyamide resin, 0.65-0.75 part of modified nano calcium carbonate, 1.5-2.5 parts of lignin fiber, 3.5-4.5 parts of modified polytetrafluoroethylene wax emulsion, 0.55-0.65 part of modified nano kaolin, 1.5-2.5 parts of calcium lignosulfonate, 2.5-3.5 parts of oxidized polyethylene wax, 2.5-3.5 parts of sorbitol and 3-4 parts of 2, 6-di-tert-butyl-4-methylphenol.
3. The recycled PA plastic particle prepared from waste cloth according to claim 1, which is characterized by comprising the following raw materials in parts by weight: 60 parts of waste polyamide fabric, 15 parts of polyamide resin, 0.7 part of modified nano calcium carbonate, 2 parts of lignin fiber, 4 parts of modified polytetrafluoroethylene wax emulsion, 0.6 part of modified nano kaolin, 2 parts of calcium lignosulfonate, 3 parts of oxidized polyethylene wax, 3 parts of sorbitol and 3.5 parts of 2, 6-di-tert-butyl-4-methylphenol.
4. The recycled PA plastic particle prepared from waste cloth according to claim 1, wherein the particle size of the modified nano kaolin and the modified nano calcium carbonate is less than 10 nm.
5. The method for preparing the regenerated PA plastic particles by using the waste cloth as claimed in any one of claims 1 to 4, which is characterized by comprising the following steps:
s1, sterilizing and disinfecting the waste polyamide cloth, and then cutting the waste polyamide cloth into particles with the average particle size of 5-10 mm; adding the particles into water, adding a decoloring agent, heating until the water is boiled to decolor the particles fully, and drying the particles;
s2, dispersing the modified nano calcium carbonate and the modified nano kaolin in the modified polytetrafluoroethylene emulsion, soaking for 2-3 h, filtering to remove redundant emulsion, and dispersing and drying the treated modified nano calcium carbonate and the treated modified nano kaolin;
s3, adding the lignin fibers into ammonia water to be soaked for 40-60 min, taking out, washing with water, and drying; then adding the mixture into ester quaternary ammonium salt to be soaked for 10-20 min, and then dehydrating and drying;
s4, uniformly mixing the lignin fiber treated in the step S3 with the modified nano calcium carbonate and the modified nano kaolin treated in the step S2 to obtain a mixture;
s5, uniformly mixing the particles obtained in the step S1 and the mixture obtained in the step S4 with polyamide resin, calcium lignosulfonate, oxidized polyethylene wax, sorbitol and 2, 6-di-tert-butyl-4-methylphenol, extruding and shearing for 20-30 min, and then extruding, cooling and granulating through a screw extrusion device to obtain the regenerated PA plastic particles.
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