CN110820081B - Method for manufacturing PLA fiber fabric containing coffee carbon - Google Patents
Method for manufacturing PLA fiber fabric containing coffee carbon Download PDFInfo
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- CN110820081B CN110820081B CN201911087671.5A CN201911087671A CN110820081B CN 110820081 B CN110820081 B CN 110820081B CN 201911087671 A CN201911087671 A CN 201911087671A CN 110820081 B CN110820081 B CN 110820081B
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
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- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/0032—Determining dye recipes and dyeing parameters; Colour matching or monitoring
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- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/445—Use of auxiliary substances before, during or after dyeing or printing
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- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/62—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing low-molecular-weight organic compounds with sulfate, sulfonate, sulfenic or sulfinic groups
- D06P1/621—Compounds without nitrogen
- D06P1/622—Sulfonic acids or their salts
- D06P1/623—Aliphatic, aralophatic or cycloaliphatic
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- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/64—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing low-molecular-weight organic compounds without sulfate or sulfonate groups
- D06P1/651—Compounds without nitrogen
- D06P1/65106—Oxygen-containing compounds
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- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/64—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing low-molecular-weight organic compounds without sulfate or sulfonate groups
- D06P1/651—Compounds without nitrogen
- D06P1/65106—Oxygen-containing compounds
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- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/673—Inorganic compounds
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- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/673—Inorganic compounds
- D06P1/67333—Salts or hydroxides
- D06P1/6735—Salts or hydroxides of alkaline or alkaline-earth metals with anions different from those provided for in D06P1/67341
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- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/673—Inorganic compounds
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- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/82—Textiles which contain different kinds of fibres
- D06P3/8204—Textiles which contain different kinds of fibres fibres of different chemical nature
- D06P3/8276—Textiles which contain different kinds of fibres fibres of different chemical nature mixtures of fibres containing ester groups
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- D06P5/02—After-treatment
- D06P5/10—After-treatment with compounds containing metal
Abstract
The invention provides a method for manufacturing a PLA fiber fabric containing coffee carbon, which belongs to the technical field of textile and comprises the following steps: spinning, pretreatment, dyeing, weaving, finishing and shaping; the fiber raw material for spinning is prepared by the following method: providing polylactic acid slices comprising poly-L-lactic acid and poly-D-lactic acid, providing coffee carbon polylactic acid master batches comprising a toughening agent and an antioxidant, taking the master batches and the polylactic acid slices to carry out melt spinning, and obtaining the PLA fiber containing coffee carbon after hot drawing and heat setting. The fiber manufacturing method can improve the heat resistance and high-temperature stability of the fiber, increase the tensile strength and elongation at break, and improve the resilience and crease resistance of the fiber and the fabric by increasing the crease recovery angle; the manufacturing method of the fabric can improve the fiber dye-uptake and dye-uptake rate, improve the color fastness to dyeing and washing, increase the color durability and shape retention of the fiber and the fabric, shorten the time consumption of the dyeing process and obviously reduce the production cost and energy consumption.
Description
Technical Field
The invention belongs to the technical field of textiles, and particularly relates to a method for manufacturing a PLA fiber fabric containing coffee carbon.
Background
Along with the improvement of living standard and the acceleration of work rhythm of people, the requirement on the protective function of the clothes is higher and higher. The attention of the textile industry to green and environment-friendly products has gradually become the standard for the research and development of new products, single-function textiles cannot meet the needs of people, and multifunctional finished textiles are receiving more and more attention and love of people due to the excellent performance of the textiles.
The polylactic acid fiber (PLA fiber) is prepared by fermenting renewable natural substances such as corn, potato, beet and the like to prepare lactic acid as a raw material, and then polymerizing and spinning the lactic acid. It can be completely biodegraded and can be recycled. The polylactic acid fabric also has excellent properties such as air permeability, moisture permeability, biocompatibility and bioabsorbability, as well as antibacterial property and flame retardance, and in the degradable thermoplastic polymer material, PLA has the best heat resistance, soft hand feeling and silky luster, but due to the defects of large brittleness, high hardness, poor heat resistance and the like of PLA, the prepared fiber has poor toughness, poor hand feeling, insufficient dimensional stability, poor wear resistance and poor water washing resistance, and the application of the polylactic acid fabric in the textile field, especially in the field of high-grade clothing is limited.
The coffee carbon fiber is produced by calcining waste coffee grounds at a high temperature of more than 1000 ℃ and then forming nano-scale particles added into spinning liquid, and the material and the performance of the coffee carbon fiber meet the current consumption trend. The main functions of the deodorant are functions and characteristics of bacteriostasis, deodorization, negative ion emission, ultraviolet resistance, heat storage, heat preservation, deodorization and environmental protection. However, the textile industry at home and abroad is basically applied to simple knitwear such as underwear, round-neck shirts, T-shirts, socks and the like, the research on the coffee carbon-containing garment fabric with a complex structure is less, and particularly, the coffee carbon-containing fiber fabric has the problems of low dye uptake, scratch and fuzz, poor color fastness and the like, so that the application of the coffee carbon-containing fiber fabric in the textile field is limited.
Disclosure of Invention
The invention aims to provide a preparation method of PLA fiber containing coffee carbon, which can improve heat resistance and high-temperature stability, increase tensile strength and elongation at break, and improve resilience and crease resistance of fiber and fabric by increasing crease recovery angle.
The invention also aims to provide a novel anti-wrinkle fabric which can increase the resilience and anti-wrinkle performance of the fabric so as to bear the deformation of the fabric caused by rubbing and twisting; the dye-uptake and dye-uptake rate of the fiber can be improved, the color fastness to dyeing and washing is improved, and the color durability and shape retention of the fiber and the fabric are improved; the method for manufacturing the PLA fiber fabric containing the coffee carbon can shorten the time consumption of the dyeing process and obviously reduce the production cost and the energy consumption.
The technical scheme adopted by the invention for realizing the purpose is as follows:
a method of making a PLA fiber containing coffee carbon, comprising: providing a polylactic acid slice, wherein the polylactic acid comprises poly-L-lactic acid (PLLA) and poly-D-lactic acid (PDLA); providing coffee carbon polylactic acid master batches, wherein the master batches comprise a toughening agent and an antioxidant; and taking the coffee carbon polylactic acid master batch and the polylactic acid slices for melt spinning, and preparing the PLA fiber containing coffee carbon after hot drawing and heat setting; the tensile strength of the PLA fiber containing the coffee carbon is 2.8-5.8cN/dtex, and the elongation at break is 25-45%. The PLA fiber containing the coffee carbon prepared by the method has the functions of heat storage and heat preservation, bacteriostasis and deodorization, negative ion emission, ultraviolet resistance and the like, has better heat resistance and high-temperature stability, good air permeability and moisture absorption and sweat releasing performance, obtains higher tensile strength and elongation at break, and improves the resilience and wrinkle resistance of the fiber and fabric by increasing the wrinkle recovery angle.
In one embodiment of the present invention, the viscosity average molecular weight of the poly (L-lactic acid) is 45 to 350kDa, wherein the molar content of the L-optical isomer is 97.5 to 99.9%; the viscosity average molecular weight of the poly-D-lactic acid is 15-80kDa, wherein the molar content of the D optical isomer is 97.5-99.9%. Preferably, the viscosity average molecular weight of PLLA is 80-230kDa and the viscosity average molecular weight of PDLA is 45-65 kDa. The addition of the poly-D-lactic acid can enable the left-handed structure and the right-handed structure to form complementation, so that molecular chains are tightly stacked, intermolecular force can be enhanced, the heat resistance and the high-temperature stability of the poly-lactic acid are improved, the hydrolysis reaction and the degradation reaction of the poly-lactic acid are avoided in the high-temperature drying or spinning process, and the beneficial influence on the fiber strength is further generated.
In a further embodiment, the polylactic acid contains poly-L-lactic acid and poly-D-lactic acid in a weight ratio of 1: 0.1-0.3.
According to one embodiment of the invention, the coffee carbon polylactic acid master batch comprises the following components in parts by weight: 10-35 parts of coffee carbon nano powder, 65-85 parts of polylactic acid slices, 0.05-0.5 part of toughening agent and 0.05-1.5 parts of antioxidant.
In one embodiment of the invention, the toughening agent is polymethyl methacrylate and phenylacetic acid-2-methyl propyl ester, and the weight ratio of the polymethyl methacrylate to the phenylacetic acid-2-methyl propyl ester is 1: 0.1-0.5. Under the high-temperature environment of melt granulation, the levolactic acid and the dextrolactic acid are easy to generate ester exchange action so as to generate a block copolymer in a stereo complex form, and the toughening agent, especially the phenylacetic acid-2-methylpropyl ester is added, can be complexed with the dextrolactic acid and is embedded into the stereo complex under thermal tension, so that the bound molecules between crystal layers in a crystal area of the stereo complex are elongated, and stronger local fluidity can be realized among the crystal layers to resist substantial breaking force when stress concentration is generated outside, so that the fiber has enhanced tensile strength and elongation at break; in addition, after complexation of phenylacetic acid-2-methyl propyl ester and D-lactic acid, the intermolecular van der Waals force effect of the stereocomplex is enhanced, so that fabrics formed by the fibers such as fabrics show larger wrinkle recovery angle, and the fibers and the fabrics have better resilience and wrinkle resistance.
In one embodiment of the invention, the polylactic acid slices are used after being subjected to pre-drying treatment; the pre-drying treatment conditions are as follows: the drying temperature is 90-110 ℃, the drying time is 3-16h, and the final water content of the slices is controlled to be less than or equal to 50 ppm.
According to one embodiment of the invention, the granulation temperature of the coffee carbon polylactic acid master batch is 170-250 ℃; the processing temperature of the melt spinning is 200-250 ℃, and the speed is 500-2000 m/min.
In one embodiment of the invention, the weight ratio of the coffee carbon polylactic acid master batch to the polylactic acid slices used in the preparation of the PLA fiber containing coffee carbon is 0.5-1.5: 10.
In one embodiment of the invention, the hot-drawing temperature is 85-120 ℃ and the multiple is 2-5; the heat setting temperature is 100-110 ℃, and the time is 2-24 h.
The invention also provides a preparation method of the PLA fiber fabric containing coffee carbon, which comprises the following steps: spinning, pretreating, dyeing, weaving, finishing and shaping, wherein the fiber raw material for spinning is the PLA fiber containing the coffee carbon prepared by the preparation method. The method greatly improves the dye-uptake and dye-uptake rate of the fiber, improves the color fastness to dyeing and washing, shortens the time consumption of the dyeing process, saves the time cost and the energy consumption, and the prepared fiber fabric has the advantages of the coffee carbon fiber and the polylactic acid fiber, is soft and comfortable in hand feeling, has good air permeability and moisture absorption and perspiration property, is good in heat resistance and high-temperature stability, excellent in rebound resilience and crease resistance, can bear washing and twisting without deformation, and is good in color persistence and shape retention of the fiber and the fabric.
In one embodiment of the invention, the yarn obtained by spinning is a PLA fiber twisted yarn containing coffee carbon, and the specification of the yarn is 100D/45F-180D/75F.
In one embodiment of the invention, the pre-treatment comprises degreasing and refining, and the preparation comprises the following components: 1.5-6g/L of sodium carbonate, 2-8.5g/L of sodium silicate, 3-13g/L of hydrogen peroxide and 0.1-0.5g/L of penetrating agent. Preferably, the penetrant is sodium sulfosuccinate.
In a further embodiment, the pretreatment step is: adding penetrant to react for 30-60min, adding soda ash and sodium silicate, heating to 55-75 deg.C, adding hydrogen peroxide, maintaining the temperature for 5-10min, heating to 85-95 deg.C, maintaining the temperature for 30-60min, cooling, and washing with water.
In one embodiment of the present invention, the dyeing bath ratio is 1: 25-35; the dyeing preparation comprises the following components in percentage by weight: leveling agent, salt and sodium carbonate in the weight ratio of 1 to 2.5-5 to 2.5-3; the dye concentration in the dye bath used for dyeing is 1.5-3.0 wt%.
In a further embodiment, the dyeing step is: adding a leveling agent, a dye and salt at the temperature of 35-45 ℃, heating to 85-105 ℃ at the heating rate of 1.5 ℃/min, preserving heat for 30-60min, adding soda for fixation for 20-30min, then cooling to 60 ℃ at the temperature of 1.5 ℃/min, discharging liquid, adding water, preserving heat for 20-30min at the temperature of 80-90 ℃, and repeatedly washing for 2-3 times.
Other steps in the method for manufacturing the PLA fiber fabric containing the coffee carbon provided by the invention can be completed by adopting the prior art, and are not repeated herein.
The invention has the beneficial effects that:
1) according to the invention, the coffee carbon is added into the polylactic acid raw material to prepare the PLA fiber containing the coffee carbon, so that the fiber has the functions of heat storage and heat preservation, bacteriostasis and deodorization, negative ion emission, ultraviolet resistance and the like, the preparation method improves the heat resistance and high-temperature stability of the fiber, increases the tensile strength and elongation at break of the fiber, and improves the resilience and crease resistance of the fiber and the fabric by increasing the crease recovery angle;
2) the fiber fabric prepared by the preparation method of the fabric has the advantages of the coffee carbon fiber and the polylactic acid fiber, has good heat resistance and high-temperature stability, excellent resilience and crease resistance, can bear washing and twisting without deformation, improves the dye uptake and dye uptake of the fiber, has high color fastness to washing and washing, has excellent color durability and shape retention of the fiber and the fabric, has short time consumption of a dyeing process, and obviously reduces the production cost and energy consumption.
The invention adopts the technical scheme to provide the method for manufacturing the PLA fiber fabric containing the coffee carbon, so that the defects of the prior art are overcome, the design is reasonable, and the operation is convenient.
Drawings
FIG. 1 is a graph showing the dye uptake rate of weakly acidic red G.
Detailed Description
The technical solution of the present invention is further described in detail below with reference to the following detailed description and the accompanying drawings:
a method of making a PLA fiber containing coffee carbon, comprising: providing a polylactic acid slice, wherein the polylactic acid comprises poly-L-lactic acid (PLLA) and poly-D-lactic acid (PDLA); providing coffee carbon polylactic acid master batches, wherein the master batches comprise a toughening agent and an antioxidant; and taking the coffee carbon polylactic acid master batch and the polylactic acid slices for melt spinning, and preparing the PLA fiber containing coffee carbon after hot drawing and heat setting; the tensile strength of the PLA fiber containing the coffee carbon is 2.8-5.8cN/dtex, and the elongation at break is 25-45%. The PLA fiber containing the coffee carbon prepared by the method has the functions of heat storage and heat preservation, bacteriostasis and deodorization, negative ion emission, ultraviolet resistance and the like, has better heat resistance and high-temperature stability, good air permeability and moisture absorption and sweat releasing performance, obtains higher tensile strength and elongation at break, and improves the resilience and wrinkle resistance of the fiber and fabric by increasing the wrinkle recovery angle.
In one embodiment of the present invention, the viscosity average molecular weight of the poly (L-lactic acid) is 45 to 350kDa, wherein the molar content of the L-optical isomer is 97.5 to 99.9%; the viscosity average molecular weight of the poly-D-lactic acid is 15-80kDa, wherein the molar content of the D optical isomer is 97.5-99.9%. Preferably, the viscosity average molecular weight of PLLA is 80-230kDa and the viscosity average molecular weight of PDLA is 45-65 kDa. More preferably, the viscosity average molecular weight of PLLA is 100-180kDa and the viscosity average molecular weight of PDLA is 50-60 kDa. The addition of the poly-D-lactic acid can enable the left-handed structure and the right-handed structure to form complementation, so that molecular chains are tightly stacked, intermolecular force can be enhanced, the heat resistance and the high-temperature stability of the poly-lactic acid are improved, the hydrolysis reaction and the degradation reaction of the poly-lactic acid are avoided in the high-temperature drying or spinning process, and the beneficial influence on the fiber strength is further generated.
In a further embodiment, the polylactic acid comprises poly-L-lactic acid and poly-D-lactic acid in a weight ratio of 1:0.1 to 0.3 (e.g., 1:0.1 or 1:0.15 or 1:0.2 or 1:0.25 or 1: 0.3).
According to one embodiment of the invention, the coffee carbon polylactic acid master batch comprises the following components in parts by weight: 10-35 parts of coffee carbon nano powder, 65-85 parts of polylactic acid slices, 0.05-0.5 part of toughening agent and 0.05-1.5 parts of antioxidant.
In one embodiment of the invention, the toughening agent is polymethyl methacrylate and 2-methylpropyl phenylacetate in a weight ratio of 1:0.1 to 0.5 (e.g., 1:0.1 or 1:0.15 or 1:0.2 or 1:0.3 or 1:0.4 or 1: 0.5). Under the high-temperature environment of melt granulation, the levolactic acid and the dextrolactic acid are easy to generate ester exchange action so as to generate a block copolymer in a stereo complex form, and the toughening agent, especially the phenylacetic acid-2-methylpropyl ester is added, can be complexed with the dextrolactic acid and is embedded into the stereo complex under thermal tension, so that the bound molecules between crystal layers in a crystal area of the stereo complex are elongated, and stronger local fluidity can be realized among the crystal layers to resist substantial breaking force when stress concentration is generated outside, so that the fiber has enhanced tensile strength and elongation at break; in addition, after complexation of phenylacetic acid-2-methyl propyl ester and D-lactic acid, the intermolecular van der Waals force effect of the stereocomplex is enhanced, so that fabrics formed by the fibers such as fabrics show larger wrinkle recovery angle, and the fibers and the fabrics have better resilience and wrinkle resistance.
In one embodiment of the invention, the antioxidant is one or more of antioxidant 1010, antioxidant BHT, antioxidant 264, antioxidant 2112, antioxidant AO-60, didodecyl alcohol ester, ditetradecyl alcohol ester, tributyl phosphite and triphenyl phosphite.
In one embodiment of the invention, the polylactic acid slices are used after being subjected to pre-drying treatment; the pre-drying treatment conditions are as follows: the drying temperature is 90-110 ℃, the drying time is 3-16h, and the final water content of the slices is controlled to be less than or equal to 50 ppm.
According to one embodiment of the invention, the granulation temperature of the coffee carbon polylactic acid master batch is 170-250 ℃; the processing temperature of the melt spinning is 200-250 ℃, and the speed is 500-2000 m/min.
In a further embodiment, the coffee carbon polylactic acid masterbatch is prepared by the following steps: adding the plasticizer into the polylactic acid slices, uniformly stirring and crushing the polylactic acid slices into powder, then adding the coffee carbon nano powder and the antioxidant, fully and uniformly mixing, and then melting and granulating the mixture at the temperature of 170-250 ℃ to obtain the polylactic acid.
In one embodiment of the present invention, the weight ratio of the coffee carbon polylactic acid master batch to the polylactic acid chip used in the preparation of the PLA fiber containing coffee carbon is 0.5-1.5:10 (e.g., 0.8:10 or 1:10 or 1.1:10 or 1.3: 10).
In one embodiment of the invention, the hot-drawing temperature is 85-120 ℃ and the multiple is 2-5; the heat setting temperature is 100-110 ℃, and the time is 2-24 h.
In a further embodiment, the coffee carbon-containing PLA fibers are prepared by the steps of: spinning the master batch and the polylactic acid slices, collecting nascent fiber at the temperature of 200-120 ℃ and the speed of 500-2000m/min, performing hot drawing at the temperature of 85-120 ℃ and the multiple of 2-5 times, and performing heat setting at the temperature of 100-110 ℃ for 2-24 hours to obtain the polylactic acid fiber.
The invention also provides a preparation method of the PLA fiber fabric containing coffee carbon, which comprises the following steps: spinning, pretreating, dyeing, weaving, finishing and shaping, wherein the fiber raw material for spinning is the PLA fiber containing the coffee carbon prepared by the preparation method. The method greatly improves the dye-uptake and dye-uptake rate of the fiber, improves the color fastness to dyeing and washing, shortens the time consumption of the dyeing process, saves the time cost and the energy consumption, and the prepared fiber fabric has the advantages of the coffee carbon fiber and the polylactic acid fiber, is soft and comfortable in hand feeling, has good air permeability and moisture absorption and perspiration property, is good in heat resistance and high-temperature stability, excellent in rebound resilience and crease resistance, can bear washing and twisting without deformation, and is good in color persistence and shape retention of the fiber and the fabric.
In one embodiment of the invention, the yarn obtained by spinning is a PLA fiber twisted yarn containing coffee carbon, and the specification of the yarn is 100D/45F-180D/75F.
In one embodiment of the invention, the pre-treatment comprises degreasing and refining, and the preparation comprises the following components: 1.5-6g/L of sodium carbonate, 2-8.5g/L of sodium silicate, 3-13g/L of hydrogen peroxide and 0.1-0.5g/L of penetrating agent. Preferably, the penetrant is sodium sulfosuccinate.
In a further embodiment, the pretreatment step is: adding penetrant to react for 30-60min, adding soda ash and sodium silicate, heating to 55-75 deg.C, adding hydrogen peroxide, maintaining the temperature for 5-10min, heating to 85-95 deg.C, maintaining the temperature for 30-60min, cooling, and washing with water.
In one embodiment of the present invention, the dyeing bath ratio is 1: 25-35; the dyeing preparation comprises the following components in percentage by weight: leveling agent, salt and sodium carbonate in the weight ratio of 1 to 2.5-5 to 2.5-3; the dye concentration in the dye bath used for dyeing is 1.5-3.0 wt%.
In a further embodiment, the dyeing step is: adding a leveling agent, a dye and salt at the temperature of 35-45 ℃, heating to 85-105 ℃ at the heating rate of 1.5 ℃/min, preserving heat for 30-60min, adding soda for fixation for 20-30min, then cooling to 60 ℃ at the temperature of 1.5 ℃/min, discharging liquid, adding water, preserving heat for 20-30min at the temperature of 80-90 ℃, and repeatedly washing for 2-3 times.
Other steps in the method for manufacturing the PLA fiber fabric containing the coffee carbon provided by the invention can be completed by adopting the prior art, and are not repeated herein.
It is to be understood that the foregoing description is to be considered illustrative or exemplary and not restrictive, and that changes and modifications may be made by those skilled in the art within the scope and spirit of the appended claims. In particular, the present invention covers other embodiments having any combination of features from the different embodiments described above and below, without the scope of the invention being limited to the specific examples below.
Example 1:
a method for making a PLA fiber containing coffee carbon, comprising the steps of:
(1) mixing poly-L-lactic acid and poly-D-lactic acid according to the weight ratio of 1:0.1 to form a poly-lactic acid raw material slice, and then drying at the temperature of 95 ℃ for 8 hours until the final water content is controlled to be less than or equal to 50ppm, wherein the viscosity average molecular weight of PLLA is 130kDa, the molar content of L optical isomer is 98.9 percent, the viscosity average molecular weight of PDLA is 55kDa, and the molar content of D optical isomer is 99.1 percent;
(2) adding 0.15 weight part of plasticizer into 68 weight parts of polylactic acid slices, uniformly stirring and crushing the mixture into powder, then adding 18 weight parts of coffee carbon nano powder and 0.5 weight part of antioxidant 1010, fully and uniformly mixing the mixture, and performing melt granulation at the temperature of 250 ℃ under 170-plus-one conditions to obtain coffee carbon polylactic acid master batches, wherein the toughening agents are polymethyl methacrylate and 2-methylpropyl phenylacetate in a weight ratio of 1: 0.15;
(3) and (2) spinning the master batches and the polylactic acid slices according to the weight ratio of 1.1:10, collecting nascent fibers at 235 ℃ and the speed of 800m/min, performing hot drawing at 110 ℃ and the multiple of 5, and performing hot setting at 105 ℃ for 12 hours to obtain the PLA fiber containing the coffee carbon.
Example 2:
a method for manufacturing a PLA fiber fabric containing coffee carbon comprises the following specific steps:
(1) spinning: spinning the fiber prepared in the example 1, wherein the yarn is PLA fiber twisted yarn containing coffee carbon, and the specification of the yarn is 100D/45F-180D/75F;
(2) pretreatment: putting the yarn into a dye vat, feeding water, adding a penetrant sodium alkyl succinate sulfonate according to the amount of 0.15g/L, reacting for 30min, adding soda ash and sodium silicate according to the amounts of 5g/L and 6.5g/L respectively, heating to 75 ℃, adding hydrogen peroxide according to the amount of 5g/L, preserving heat for 10min, heating to 90 ℃, preserving heat for 35min, cooling, and washing with water;
(3) dyeing: feeding water according to a bath ratio of 1:33, adding a leveling agent triethanolamine, a dye and salt at 40 ℃, heating to 105 ℃ at a heating rate of 1.5 ℃/min, preserving heat for 45min, adding soda ash for fixation for 30min, cooling to 60 ℃ at 1.5 ℃/min, discharging liquid, adding water, preserving heat for 30min at 90 ℃, and repeatedly washing for 3 times, wherein the weight ratio of the preparation is as follows: a leveling agent, namely common salt and sodium carbonate, wherein the ratio of the sodium carbonate to the sodium carbonate is 1:3.5:2.5, and the concentration of the dye in a dye bath is 2.5 wt%;
(4) weaving: weaving by adopting plain weave;
(5) finishing: washing the woven grey cloth with water at a bath ratio of 1:25 at 60 ℃ for 30 min;
(6) shaping: adding 20g/L of organic silicon softening agent on a setting machine, tentering 154cm on the machine, finishing at 160 ℃, carrying out the speed of 25m/min, inspecting, rolling and packaging.
Example 3:
this embodiment differs from embodiment 2 only in that: the penetrant used in the step (2) contains 0.03 wt% of tetraisopropyl titanate and 0.05 wt% of pentaerythritol, the tetraisopropyl titanate and the pentaerythritol are added into the penetrant to achieve a synergistic effect on the permeated yarns and can also permeate into gaps inside the yarns, the tolerance of the fibers to water is improved by utilizing hydrophilic groups, so that the surface wettability of the internal fibers is increased, the dye-uptake rate and the dye-uptake rate of the dye in the subsequent dyeing process are improved, the time consumption of the dyeing process is shortened, the time cost and the energy consumption are saved, in addition, the dye is fixed on the surfaces of the fibers by the tetraisopropyl titanate and the pentaerythritol, the dye-uptake rate and the dye-uptake rate of the fibers are increased, the dye-uptake rate and the dye-uptake rate of the dye in the subsequent dyeing process are.
Example 4:
this embodiment differs from embodiment 1 only in that: the polylactic acid raw material is only poly-L-lactic acid, the viscosity average molecular weight of PLLA is 130kDa, and the molar content of L optical isomer is 98.9 percent.
Example 5:
this embodiment differs from embodiment 2 only in that: the PLA fiber containing the coffee carbon prepared in example 4 was used to prepare a PLA fiber fabric containing coffee carbon.
Example 6:
this embodiment differs from embodiment 1 only in that: the toughening agent in the step (2) is polymethyl methacrylate, and phenylacetic acid-2-methylpropyl ester is not added.
Example 7:
this embodiment differs from embodiment 2 only in that: the PLA fiber containing the coffee carbon prepared in example 6 was used to prepare a PLA fiber fabric containing coffee carbon.
Example 8:
this embodiment differs from embodiment 1 only in that: the polylactic acid raw material is only poly-L-lactic acid, the viscosity average molecular weight of PLLA is 130kDa, and the molar content of L optical isomer is 98.9 percent; meanwhile, the toughening agent in the step (2) is polymethyl methacrylate, and phenylacetic acid-2-methylpropyl ester is not added.
Example 9:
this embodiment differs from embodiment 2 only in that: the PLA fiber containing the coffee carbon prepared in example 8 was used to prepare a PLA fiber fabric containing coffee carbon.
Test example 1:
tensile Property test of PLA fibers containing Coffea carbon
The test method comprises the following steps: the rupture strength and the rupture elongation of the biomass graphene modified polylactic acid fiber were measured by an LLY-06E type electronic single fiber strength tester using PLA fibers containing coffee carbon prepared in examples 1, 4, 6 and 8, wherein the tensile speed was set to 20mm/min, the grip distance was set to 10mm, and each sample was measured for 20 times, and the results were averaged. The test results are shown in table 1 below.
TABLE 1 tensile Property test results for coffee carbon-containing PLA fibers
As can be seen from the above table, the tensile strength and elongation at break of the coffee carbon-containing PLA fiber in the wet state are superior to those in the dry state; the tensile strength and elongation at break of example 1 are optimal; examples 4 and 6 both exhibited a reduced tendency in tensile strength and elongation at break compared to example 1, but the reduction in example 6 was more pronounced than in example 4; the tensile strength and elongation at break of example 8 are the worst; in conclusion, the phenylacetic acid-2-methyl propyl ester and the poly-D-lactic acid in the toughening agent have obvious gain effect on the improvement of the tensile strength and the elongation at break of the fiber, and the effect is not as good as the synergistic effect of the two when the toughening agent is used singly.
Test example 2:
crease elasticity test of PLA fiber fabric containing coffee carbon
The test method comprises the following steps: the fiber fabrics prepared in examples 2, 5, 7 and 9 were used as test samples, and the wrinkle recovery angle of the fabrics was tested by using YG541 type fabric wrinkle elasticity tester, with reference to GB/T3819-1997 test method for measuring recovery angle of fabric crease recovery. The results are shown in table 2 below.
TABLE 2 wrinkle elasticity test results for PLA fiber fabrics containing coffee carbon
The larger the wrinkle recovery angle, the better the wrinkle resistance. As can be seen from the above table, the wrinkle recovery angle of example 2 is the largest, and both the wrinkle recovery angles of example 5 and example 7 show a decreasing trend compared to example 2, but the decrease of example 7 is more significant than that of example 5; the crease recovery angle of example 9 was minimal; in conclusion, the phenylacetic acid-2-methyl propyl ester and the poly-D-lactic acid in the toughening agent have a remarkable effect of improving the wrinkle recovery angle of the fiber and the fabric, the effect is not as good as the synergistic effect of the two when the toughening agent is used singly, and the two are beneficial to enabling the fiber and the fabric to show better rebound resilience and wrinkle resistance.
Test example 3:
dyeing effect and dyeing quality test of PLA fiber and fabric containing coffee carbon
The test method comprises the following steps: (1) in the dyeing methods of examples 2 and 3, the dyeing time and the dye uptake in the dyeing process were measured and the dye uptake rate was plotted according to GB/T23976.1-2009 method for measuring dye uptake rate curve, wherein the dye is weakly acidic red G, the dyeing temperature is 105 ℃. As shown in fig. 1.
(2) Using the fiber fabrics produced in example 2 and example 3 as samples, with reference to GB/T3921-2008C (3)' color fastness to soaping color fastness of textile, sample size: 4cm × 10cm, lining fabric: 1 piece of wool fiber white cloth and 1 piece of cotton fiber white cloth. Soaping temperature: (60. + -.2) ℃ and soaping time: and (4) 45 min. Evaluation criteria: GB/T250-2008 'Gray sample card for evaluating color change in textile color fastness test'; GB/T251-2008 'Grey sample card for evaluating textile color fastness test'. The results are shown in table 3 below.
FIG. 1 is a graph showing the dye uptake rate of weakly acidic red G. As can be seen from the figure, the final dye-uptake of example 2 is 97.6%, the final dye-uptake of example 3 is 99.3%, and the dye-uptake of example 2 is substantially stable after 45min, while the dye-uptake of example 3 is substantially stable after 38min, and the dye-uptake rate are remarkably improved; compared with the penetrant in the embodiment 2, the penetrant in the embodiment 3 can obviously improve the dye-uptake rate and the dye-uptake rate of the dye in the subsequent dyeing process, shorten the time consumption of the dyeing process, save the time cost and the energy consumption, and achieve the beneficial effect of enhancing the dyeing effect.
TABLE 3 color fastness to washing test results for PLA fiber fabrics containing coffee carbon
As can be seen from the above table, the color fastness to washing of the fiber fabric is good, but the example 3 is more excellent in color change and staining than the example 2, which shows that the manufacturing method of the example 3 can significantly increase the color fastness to washing compared with the example 2, thereby achieving the beneficial effect of improving the dyeing quality.
Conventional techniques in the above embodiments are known to those skilled in the art, and therefore, will not be described in detail herein.
The above embodiments are merely illustrative, and not restrictive, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention. Therefore, all equivalent technical solutions also belong to the scope of the present invention, and the protection scope of the present invention should be defined by the claims.
Claims (9)
1. A method of making a PLA fiber containing coffee carbon, comprising:
providing a polylactic acid slice, wherein the polylactic acid comprises poly-L-lactic acid and poly-D-lactic acid;
providing coffee carbon-polylactic acid master batches, wherein the master batches comprise a toughening agent and an antioxidant, and the toughening agent is polymethyl methacrylate and phenylacetic acid-2-methylpropyl ester;
and taking the coffee carbon-polylactic acid master batch and the polylactic acid slices for melt spinning, and preparing the PLA fiber containing coffee carbon after hot drafting and hot setting;
the tensile strength of the PLA fiber containing the coffee carbon is 2.8-5.8cN/dtex, and the elongation at break is 25-45%;
the weight ratio of poly-L-lactic acid and poly-D-lactic acid contained in the polylactic acid is 1: 0.1-0.3; the weight ratio of polymethyl methacrylate to phenylacetic acid-2-methyl propyl ester in the toughening agent is 1: 0.1-0.5;
the coffee carbon polylactic acid master batch comprises the following components in parts by weight: 10-35 parts of coffee carbon nano powder, 65-85 parts of polylactic acid slices, 0.05-0.5 part of toughening agent and 0.05-1.5 parts of antioxidant.
2. The method of claim 1, wherein the PLA fiber containing coffee carbon is prepared by: the viscosity average molecular weight of the poly-L-lactic acid is 80-230kDa, and the viscosity average molecular weight of the poly-D-lactic acid is 45-65 kDa.
3. The method of claim 1, wherein the PLA fiber containing coffee carbon is prepared by: the polylactic acid slices are used after being pre-dried; the pre-drying treatment conditions are as follows: the drying temperature is 90-110 ℃, the drying time is 3-16h, and the final water content of the slices is controlled to be less than or equal to 50 ppm.
4. The method of claim 1, wherein the PLA fiber containing coffee carbon is prepared by: the granulation temperature of the coffee carbon-polylactic acid master batch is 170-250 ℃; the processing temperature of the melt spinning is 200-250 ℃ and the speed is 500-2000 m/min.
5. The method of claim 1, wherein the PLA fiber containing coffee carbon is prepared by: the weight ratio of the coffee carbon-polylactic acid master batch to the polylactic acid slices used in the preparation of the PLA fiber containing coffee carbon is 0.5-1.5: 10; the hot drawing temperature is 85-120 ℃, and the multiple is 2-5 times; the heat setting temperature is 100-110 ℃, and the time is 2-24 h.
6. A method for manufacturing a PLA fiber fabric containing coffee carbon comprises the following steps: a step of spinning, pretreatment, dyeing, weaving, finishing and shaping, wherein the fiber raw material for spinning is the PLA fiber containing the coffee carbon prepared by the preparation method of any one of claims 1 to 5;
the pretreatment steps are as follows: adding penetrant to react for 30-60min, adding soda ash and sodium silicate, heating to 55-75 deg.C, adding hydrogen peroxide, maintaining the temperature for 5-10min, heating to 85-95 deg.C, maintaining the temperature for 30-60min, cooling, and washing with water; the penetrant is sodium alkyl sulfosuccinate;
the concentrations of the reagents in the pretreatment step are as follows: 1.5-6g/L of sodium carbonate, 2-8.5g/L of sodium silicate, 3-13g/L of hydrogen peroxide and 0.1-0.5g/L of penetrating agent.
7. The method for manufacturing the PLA fiber fabric containing coffee carbon as claimed in claim 6, wherein: the yarn obtained by spinning is a PLA fiber twisted yarn containing coffee carbon, and the specification of the yarn is 100D/45F-180D/75F.
8. The method for manufacturing the PLA fiber fabric containing coffee carbon as claimed in claim 6, wherein: the dyeing bath ratio is 1: 25-35; the dyeing preparation comprises the following components in percentage by weight: a leveling agent, namely common salt and soda ash =1:2.5-5: 2.5-3; the dye concentration of the dye bath used for dyeing is 1.5-3.0 wt%.
9. The method for manufacturing the PLA fiber fabric containing coffee carbon as claimed in claim 6, wherein: the dyeing steps are as follows: adding a leveling agent, a dye and salt at the temperature of 35-45 ℃, heating to 85-105 ℃ at the heating rate of 1.5 ℃/min, preserving heat for 30-60min, adding soda for fixation for 20-30min, then cooling to 60 ℃ at the temperature of 1.5 ℃/min, discharging liquid, adding water, preserving heat for 20-30min at the temperature of 80-90 ℃, and repeatedly washing for 2-3 times.
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Inventor after: Jiang Qiquan Inventor after: Li Yunzi Inventor after: Yu Jian Inventor before: Jiang Qiquan Inventor before: Li Yunzi Inventor before: Yu Jian |