CN105951434A - Biological enzyme method for water repellent finish of real silk fabric - Google Patents
Biological enzyme method for water repellent finish of real silk fabric Download PDFInfo
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- CN105951434A CN105951434A CN201610316380.9A CN201610316380A CN105951434A CN 105951434 A CN105951434 A CN 105951434A CN 201610316380 A CN201610316380 A CN 201610316380A CN 105951434 A CN105951434 A CN 105951434A
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- Prior art keywords
- real silk
- silk fabric
- fabric
- fluorinated acrylate
- water repellent
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
- D06M14/02—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of natural origin
- D06M14/06—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of natural origin of animal origin, e.g. wool or silk
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F289/00—Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds not provided for in groups C08F251/00 - C08F287/00
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/12—Aldehydes; Ketones
- D06M13/127—Mono-aldehydes, e.g. formaldehyde; Monoketones
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/10—Animal fibres
- D06M2101/12—Keratin fibres or silk
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Zoology (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a biological enzyme method for water repellent finish of real silk fabric. Tyrosine residues in fibroin of the real silk fabric are catalyzed by the aid of a horseradish peroxidase/hydrogen peroxide/diacetone system to generate phenoxy radicals, the phenoxy radicals and fluorinated acrylate monomers are subjected to graft copolymerization, the water repellent property of the real silk fabric is improved, and water repellent finish of the real silk fabric is realized with the biological enzyme method. The biological enzyme method comprises specific steps as follows: (1) preparation of a fluorinated acrylate emulsion; (2) treatment of the real silk fabric with horseradish peroxidase; (3) graft copolymerization of real silk and fluorinated acrylate; (4) after-treatment of the real silk fabric. Compared with a high-temperature padding and baking method and a traditional graft copolymerization method adopting ultraviolet light or microwave radiation, the method has higher graft copolymerization efficiency, the enzyme treatment condition is mild, the water repellent finish effect of the fabric is better, and the problems of reduction of strength of the fabric and yellowing of the surface of the fabric are solved.
Description
Technical field
A kind of method that the present invention relates to biological enzyme real silk fabric water repellent finish, particularly a kind of by means of horseradish peroxidase/
Hydrogen peroxide/acetylacetone,2,4-pentanedione system, catalysis fibroin produces activity Phenoxy radical, and fluorinated acrylate monomer generation graft copolymerization,
Improve the water repellency of real silk fabric, it is achieved biological enzyme real silk fabric water repellent finish, belong to field of textile biotechnology.
Background technology
Silkworm silk is made up of sericin and fibroin two parts, and in degumming process, sericin is dissolved by alkaline agent or protease hydrolysis, and chemistry is steady
Qualitative higher fibroin is effectively retained.Real silk fabric is soft, and gloss is graceful, absorbs excellent, has and well take
Comfortableness;But then, real silk fabric there is also some drawbacks, including as poor in wrinkle resistance, non-oxidizability is low, be easily generated
The phenomenons such as yellowing, it is therefore desirable to real silk is carried out the Final finishing processing of necessity.In recent years, new to silk like fabric along with consumer
Grain huskization, the requirement of functionalization, real silk fabric has been not limited to tradition boundary in season, has been not only used as frivolous summer clothing garment material,
It is also used for suit autumn and winter, tippet, high-grade wind coat and upholstery etc..Therefore, silk fabric is functional and product improving
Added value aspect, several functions finishing technique obtains research and development, whole including fire-retardant, antibacterial, radioprotective and water and oil repellant
Reason etc..Wherein, water repellent finish can improve the application category of real silk fabric, gives waterproof and moisture-inhibiting effect that ready-made clothes is good.Tradition
Water repellent finish of waterproof many employings fluorine-contained finishing agent, carry out rolling baking mode, but when being applied to real silk fabric water repellent finish, have one
Fixed problem, on the one hand, can affect real silk fabric feel or breathability, on the other hand, high temperature bakes (150~180 DEG C) pole
Easily making real silk fabric yellowing, make cloth cover color ligh modification, fabric strength declines.Therefore, how under more gentle process conditions
Carrying out real silk fabric water repellent finish is technical problem urgently to be resolved hurrily.
Containing vinyl and carbon fluorine chain structure in fluorinated acrylate monomer, wherein, vinyl structure is in heating, microwave or ultraviolet
Under radiation parameter, initiator (such as persulfate, 2-hydroxyl-4-(2-hydroxy ethoxy)-2-methyl phenyl ketone etc.) can be passed through and promote list
It is polymerized between body, forms the organic fluorine water-refusing resin with low surface tension.Meanwhile, if fiber macromolecular surface contains
Reactive group, and this group can by initiator effect produce living radical, then can realize fluorinated acrylate monomer at fiber
The grafting on surface and copolymerization, give the water repellent finish effect of fibre washability.Containing about 30% in the fibroin macromole of real silk fabric
The polar amino acid residues of left and right, wherein the tyrosine residue of phenolic hydroxy group accounts for 10%, is urged under this phenolic hydroxyl group energy certain condition
Metaplasia becomes to have the Phenoxy radical of reactivity, can with vinyl monomer generation graft copolymerization, thus be based on graft copolymerization side
The real silk fabric functionalization of method arranges and provides possibility.
Horseradish peroxidase (HRP) has the strongest catalysis activity, at hydrogen peroxide (H2O2)/acetylacetone,2,4-pentanedione (ACAC) body
In system, acrylic acid or acrylate (including fluorinated acrylate) monomer copolymerization can be caused.Research shows, HRP is except for second
Outside the polymerization of thiazolinyl class monomer, moreover it is possible to cause the polymerization of phenols, phenyl amines, produce including tyrosine residue in catalysis fibroin and there is work
Property Phenoxy radical, it is achieved with acrylic acid or acrylic ester grafted copolymerization, give the functional requirement needed for real silk fabric.Very
In silk fabrics water repellent finish processing, according to this feature of HRP, following thinking is used to carry out real silk fabric water repellent finish:
The first step: with HRP/H2O2/ ACAC system, in catalysis real silk, tyrosine residue generates activity Phenoxy radical;
Second step: add the fluorinated acrylate monomer after emulsifying in system, by Phenoxy radical on catalysis fibroin with fluorine-containing
Acrylate monomer graft copolymerization, improves the water repellency of real silk fabric.
Summary of the invention
The technical problem to be solved is to provide a kind of method of biological enzyme real silk fabric water repellent finish, it is intended to realize slow
With carry out Silk Fabric Finishing under the conditions of low-temp reaction, improving while water repellency, it is to avoid real silk fabric generation yellowing in arrangement
And strength damage.
For solving above-mentioned technical problem, the technical solution used in the present invention: with horseradish peroxidase/hydrogen peroxide/acetylacetone,2,4-pentanedione system,
In the fibroin of catalysis real silk fabric, tyrosine residue generates Phenoxy radical, after adding the emulsion of fluorinated acrylate monomer, passes through
On fibroin, Phenoxy radical and fluorinated acrylate monomer graft copolymerization, improve the water repellency of real silk fabric, concrete technology and step
As follows:
(1) preparation of fluorinated acrylate emulsion: carry out fluorinated acrylate monomer emulsifying with emulsifying agent, prepare emulsion system;
Process technology preparation and condition: emulsifying agent 0.25~2.5%, fluorinated acrylate monomer 1~6%, stir at 20~30 DEG C
Mix emulsifying 0.5~2 hours, prepare fluorinated acrylate emulsion;
(2) horseradish peroxidase processes real silk fabric: real silk fabric is immersed in horseradish peroxidase and acetylacetone,2,4-pentanedione solution
In, in solution, it is added dropwise over hydrogen peroxide under nitrogen protection;
Process technology preparation and condition: horseradish peroxidase 2~20U/mL, acetylacetone,2,4-pentanedione 5~10g/L, hydrogen peroxide 5~
20g/L, treatment temperature 30~60 DEG C, pH 5~9, time 0.25~1 hour;
(3) real silk and fluorinated acrylate graft copolymerization: add fluorine-containing third prepared in step (1) in step (2) solution
Olefin(e) acid ester emulsion, is catalyzed it in real silk surface grafting and copolymerization;
Process technology preparation and condition: fluorinated acrylate monomer 0.5~3%, treatment temperature 30~60 DEG C, pH 5~9, time
Between 2~12 hours;
(4) real silk fabric post processing: the real silk fabric after step (3) processes is dried, with acetone under the conditions of 30~50 DEG C
Or butanone extraction processes 2~12 hours, dry under the conditions of 30~50 DEG C the most again.
A kind of method of biological enzyme real silk fabric water repellent finish, described emulsifying agent includes polyoxyethylene nonionic surfactant,
Polyalcohols nonionic surfactant, or non-ion fluorin carbon surface active agent;Described fluorinated acrylate includes acrylic acid trifluoro
Ethyl ester, trifluoroethyl methacrylate, hexafluorobutyl acrylate, Hexafluorobutyl mathacrylate, acrylic acid octafluoro pentyl ester, first
Base acrylic acid octafluoro pentyl ester, dodecafluorhe-ptylacrylate, dodecafluoroheptyl methacrylate, or methacrylic acid ten trifluoro monooctyl ester;
Described horseradish peroxidase derives from animal, plant or microorganism.
The present invention is by means of horseradish peroxidase/hydrogen peroxide/acetylacetone,2,4-pentanedione system, by tyrosine residue in the fibroin of catalysis real silk
Producing Phenoxy radical, it is achieved Phenoxy radical and fluorinated acrylate monomer graft copolymerization, preparation has the real silk of water repellency and knits
Thing.Compared with padding the method for baking, ultraviolet light or microwave exposure conventional propylene acid esters graft copolymerization with employing high temperature, the present invention adopts
Biological enzyme water repellent finish have the advantage that
(1) graft copolymerization efficiency is higher, and it is residual that horseradish peroxidase/hydrogen peroxide/acetylacetone,2,4-pentanedione system can be catalyzed tyrosine in fibroin
Base generates Phenoxy radical, and by carrying out graft copolymerization with fluorinated acrylate monomer, gives real silk fabric water repellency, it is thus achieved that
Preferable finishing effect;
(2) ferment treatment condition relaxes, and under low temperature and near-neutral sulfite deinking, carries out in real silk fabric by means of horseradish peroxidase
Fibroin and fluorinated acrylate monomer graft copolymerization, have the advantage that energy consumption is low, process process safety;
(3), after real silk fabric water repellent finish, not only mechanical strength is improved, it also avoid high temperature pad bake, ultraviolet light and microwave
The problem that irradiation method graft copolymerization is easily generated fabric yellowing.
Detailed description of the invention
Use horseradish peroxidase/hydrogen peroxide/acetylacetone,2,4-pentanedione system catalysis real silk fabric and fluorinated acrylate monomer graft copolymerization,
Realize real silk fabric water repellent finish, measure fabric face wetting contact angle, fabric face moisture resistance (spray rating 1~5 grades, its
In 5 grades the highest), finished tensile strength and whiteness value, specific embodiment is as follows:
Embodiment 1
Use the real silk fabric (70g/m after degumming2), carrying out water repellent finish with the method that the present invention addresses, processing step is as follows:
(1) preparation of hexafluorobutyl acrylate emulsion: with 0.25%Tween 80 (polyoxyethylene nonionic surfactant)
It is emulsifying agent with 0.25% non-ion fluorin carbon surface active agent, carries out hexafluorobutyl acrylate high-speed stirred, emulsifying 0.5 at 25 DEG C
The hexafluorobutyl acrylate emulsion that concentration is 5% is obtained after hour;
(2) horseradish peroxidase processes real silk fabric: real silk fabric is immersed in horseradish peroxidase and acetylacetone,2,4-pentanedione solution
In, in solution, it is added dropwise over hydrogen peroxide under nitrogen protection;Wherein horseradish peroxidase 5U/mL, acetylacetone,2,4-pentanedione 5g/L,
Hydrogen peroxide 8g/L, treatment temperature 50 DEG C, pH 7,0.25 hour time;
(3) real silk and fluorinated acrylate graft copolymerization: add the emulsion of preparation in step (1) in step (2) solution,
Hexafluorobutyl acrylate 3% in reaction system, temperature 50 C, pH 7,6 hours time;
(4) real silk fabric post processing: the real silk fabric after step (3) processes is dried, with acetone extract under the conditions of 45 DEG C
Process 10 hours, dry under the conditions of 45 DEG C the most again.
Sample 1: untrimmed real silk fabric
Sample 2: the real silk fabric processed through step (1), (2), (3) and (4);
After above-mentioned PROCESS FOR TREATMENT, respectively measure the moistened surface contact angle of sample 1~2, fabric face moisture resistance (spray rating),
Finished tensile strength and fabric whiteness value;Wherein the surface contact angle of sample 1 is 0 °, and moisture resistance is 1 grade, and fracture strength is
440N, whiteness value 80%;The surface contact angle of sample 2 is 134 °, and moisture resistance is 4 grades, and fracture strength is 452N, in vain
Angle value 79%.
Embodiment 2
Use the real silk fabric (63g/m after degumming2), carrying out water repellent finish with the method that the present invention addresses, processing step is as follows:
(1) preparation of Hexafluorobutyl mathacrylate emulsion: with 0.5%Tween 80 (polyoxyethylene non-ionic surface active
Agent) and 0.5% non-ion fluorin carbon surface active agent be emulsifying agent, carry out Hexafluorobutyl mathacrylate high-speed stirred at 25 DEG C, breast
The Hexafluorobutyl mathacrylate emulsion that concentration is 4.5% is obtained after changing 1 hour;
(2) horseradish peroxidase processes real silk fabric: real silk fabric is immersed in horseradish peroxidase and acetylacetone,2,4-pentanedione solution
In, in solution, it is added dropwise over hydrogen peroxide under nitrogen protection;Wherein horseradish peroxidase 10U/mL, acetylacetone,2,4-pentanedione 5g/L,
Hydrogen peroxide 9g/L, treatment temperature 50 DEG C, pH 7,0.5 hour time;
(3) real silk and fluorinated acrylate graft copolymerization: add the emulsion of preparation in step (1) in step (2) solution,
Hexafluorobutyl mathacrylate 2.5% in reaction system, temperature 50 C, pH 7,6 hours time;
(4) real silk fabric post processing: the real silk fabric after step (3) processes is dried under the conditions of 50 DEG C, extracts with butanone
Process 8 hours, dry under the conditions of 50 DEG C the most again.
Sample 3: untrimmed real silk fabric
Sample 4: the real silk fabric processed through step (1), (2), (3) and (4);
After above-mentioned PROCESS FOR TREATMENT, respectively measure the moistened surface contact angle of sample 3~4, fabric face moisture resistance (spray rating),
Finished tensile strength and fabric whiteness value;Wherein the surface contact angle of sample 3 is 0 °, and moisture resistance is 1 grade, and fracture strength is
432N, whiteness value 82%;The surface contact angle of sample 4 is 153 °, and moisture resistance is 5 grades, and fracture strength is 449N, in vain
Angle value 80%.
Although the present invention is open the most as above with preferred embodiment, but it is not limited to the present invention, any person skilled in the art,
Without departing from the spirit and scope of the present invention, all can do various changes and modification, therefore protection scope of the present invention should be with
What claims were defined is as the criterion.
Claims (2)
1. a method for biological enzyme real silk fabric water repellent finish, particularly a kind of by means of horseradish peroxidase/hydrogen peroxide/
Acetylacetone,2,4-pentanedione system, in the fibroin of catalysis real silk fabric, tyrosine residue generates Phenoxy radical, sends out with fluorinated acrylate monomer
Raw graft copolymerization, improves the water repellency of real silk fabric, it is achieved biological enzyme real silk fabric water repellent finish, and concrete technology is with step such as
Under:
(1) preparation of fluorinated acrylate emulsion: carry out fluorinated acrylate monomer emulsifying, wherein emulsifying agent with emulsifying agent
0.25~2.5%, fluorinated acrylate monomer 1~6%, 20~30 DEG C of stirring and emulsifying 0.5~2 hours, prepare fluorine-containing propene
Acid esters emulsion;
(2) horseradish peroxidase processes real silk fabric: real silk fabric is immersed in horseradish peroxidase and acetylacetone,2,4-pentanedione solution
In, in solution, be added dropwise over hydrogen peroxide, wherein horseradish peroxidase 2~20U/mL under nitrogen protection, acetylacetone,2,4-pentanedione 5~
10g/L, hydrogen peroxide 5~20g/L, treatment temperature 30~60 DEG C, pH 5~9, time 0.25~1 hour;
(3) real silk and fluorinated acrylate graft copolymerization: add fluorine-containing third prepared in step (1) in step (2) solution
Olefin(e) acid ester emulsion, be catalyzed its in real silk surface grafting and copolymerization, wherein fluorinated acrylate monomer 0.5~3%, treatment temperature 30~
60 DEG C, pH 5~9, time 2~12 hours;
(4) real silk fabric post processing: the real silk fabric after step (3) processes is dried, with acetone under the conditions of 30~50 DEG C
Or butanone extraction processes 2~12 hours, dry under the conditions of 30~50 DEG C the most again.
Method the most according to claim 1, it is characterised in that: described emulsifying agent includes that polyoxyethylene non-ionic surface is lived
Property agent, polyalcohols nonionic surfactant, or non-ion fluorin carbon surface active agent;Described fluorinated acrylate includes propylene
Acid trifluoro ethyl ester, trifluoroethyl methacrylate, hexafluorobutyl acrylate, Hexafluorobutyl mathacrylate, acrylic acid octafluoro penta
Ester, methacrylic acid octafluoro pentyl ester, dodecafluorhe-ptylacrylate, dodecafluoroheptyl methacrylate, or methacrylic acid 13
Fluorine monooctyl ester;Described horseradish peroxidase derives from animal, plant or microorganism.
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106702738A (en) * | 2016-12-09 | 2017-05-24 | 南通纺织丝绸产业技术研究院 | Preparation method of functional real silk fabric |
CN107059406A (en) * | 2017-04-19 | 2017-08-18 | 江苏腾盛纺织科技集团有限公司 | The preparation method of super-hydrophobic terylene |
CN108589289A (en) * | 2018-04-13 | 2018-09-28 | 江南大学 | A method of protein fibre antibiotic finish is carried out based on coupling and enzymatic polymerization |
CN109183412A (en) * | 2018-09-13 | 2019-01-11 | 江苏大同宝富纺织科技有限公司 | A kind of dacron water-repellent finishing method based on graft copolymerization |
CN109183417A (en) * | 2018-08-23 | 2019-01-11 | 贵州凯里经济开发区鑫田民族服饰工艺品发展有限公司 | Miao ethnic group's needlework and preparation method thereof |
CN110156924A (en) * | 2019-05-31 | 2019-08-23 | 东华大学 | A kind of method that microwave irradiation prepares fluorine-containing fabric water-refusing oil-refusing finishing agent |
CN111501341A (en) * | 2020-04-10 | 2020-08-07 | 蚌埠学院 | Preparation method of hydrophobic modified silk fiber material |
CN116240725A (en) * | 2023-04-28 | 2023-06-09 | 潮州市丹辉婚纱礼服有限公司 | Preparation process of polyester fabric |
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CN103526543A (en) * | 2012-08-29 | 2014-01-22 | 江南大学 | Flame-proof treatment method of real silk fabrics by biological enzyme method |
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LEO SIMMONS ETAL: ""Chemoenzymatic modification of silk fibroin with poly(2,6-dimethyl-1,5-phenylene ether) using horseradish peroxidase"", 《RSC ADVANCES》 * |
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Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106702738A (en) * | 2016-12-09 | 2017-05-24 | 南通纺织丝绸产业技术研究院 | Preparation method of functional real silk fabric |
CN106702738B (en) * | 2016-12-09 | 2019-04-05 | 南通纺织丝绸产业技术研究院 | The preparation method of functional real silk fabric |
CN107059406A (en) * | 2017-04-19 | 2017-08-18 | 江苏腾盛纺织科技集团有限公司 | The preparation method of super-hydrophobic terylene |
CN108589289A (en) * | 2018-04-13 | 2018-09-28 | 江南大学 | A method of protein fibre antibiotic finish is carried out based on coupling and enzymatic polymerization |
CN109183417A (en) * | 2018-08-23 | 2019-01-11 | 贵州凯里经济开发区鑫田民族服饰工艺品发展有限公司 | Miao ethnic group's needlework and preparation method thereof |
CN109183412A (en) * | 2018-09-13 | 2019-01-11 | 江苏大同宝富纺织科技有限公司 | A kind of dacron water-repellent finishing method based on graft copolymerization |
CN109183412B (en) * | 2018-09-13 | 2021-04-20 | 江苏大同宝富纺织科技有限公司 | Polyester fabric water repellent finishing method based on graft copolymerization |
CN110156924A (en) * | 2019-05-31 | 2019-08-23 | 东华大学 | A kind of method that microwave irradiation prepares fluorine-containing fabric water-refusing oil-refusing finishing agent |
CN111501341A (en) * | 2020-04-10 | 2020-08-07 | 蚌埠学院 | Preparation method of hydrophobic modified silk fiber material |
CN116240725A (en) * | 2023-04-28 | 2023-06-09 | 潮州市丹辉婚纱礼服有限公司 | Preparation process of polyester fabric |
CN116240725B (en) * | 2023-04-28 | 2023-11-03 | 普宁市荣煌织造有限公司 | Preparation process of polyester fabric |
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