CN106319954A - Method for preparing mothproof silk fiber - Google Patents
Method for preparing mothproof silk fiber Download PDFInfo
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- CN106319954A CN106319954A CN201610682062.4A CN201610682062A CN106319954A CN 106319954 A CN106319954 A CN 106319954A CN 201610682062 A CN201610682062 A CN 201610682062A CN 106319954 A CN106319954 A CN 106319954A
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- China
- Prior art keywords
- silk fiber
- gamma
- fibroin
- mothproof
- cellulose
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- 239000000835 fiber Substances 0.000 title claims abstract description 94
- 238000000034 method Methods 0.000 title claims abstract description 11
- 229920000858 Cyclodextrin Polymers 0.000 claims abstract description 59
- GDSRMADSINPKSL-HSEONFRVSA-N gamma-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO GDSRMADSINPKSL-HSEONFRVSA-N 0.000 claims abstract description 59
- 229940080345 gamma-cyclodextrin Drugs 0.000 claims abstract description 59
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052709 silver Inorganic materials 0.000 claims abstract description 13
- 239000004332 silver Substances 0.000 claims abstract description 13
- 238000007598 dipping method Methods 0.000 claims abstract description 9
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 claims description 53
- 239000000243 solution Substances 0.000 claims description 46
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 239000007788 liquid Substances 0.000 claims description 29
- 239000002245 particle Substances 0.000 claims description 25
- 239000007787 solid Substances 0.000 claims description 25
- 239000011259 mixed solution Substances 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- 108010022355 Fibroins Proteins 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 241000255789 Bombyx mori Species 0.000 claims description 14
- 239000003921 oil Substances 0.000 claims description 14
- 239000001913 cellulose Substances 0.000 claims description 12
- 229920002678 cellulose Polymers 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 12
- 239000000017 hydrogel Substances 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 10
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000005470 impregnation Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- 241000218646 Cedrus deodara Species 0.000 claims description 6
- 238000005516 engineering process Methods 0.000 claims description 6
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 6
- 239000012279 sodium borohydride Substances 0.000 claims description 6
- UWFRVQVNYNPBEF-UHFFFAOYSA-N 1-(2,4-dimethylphenyl)propan-1-one Chemical compound CCC(=O)C1=CC=C(C)C=C1C UWFRVQVNYNPBEF-UHFFFAOYSA-N 0.000 claims description 5
- JBJAAHCMRSHTAO-UHFFFAOYSA-N [K].I(=O)(=O)C1=C(C(=O)O)C=CC=C1 Chemical compound [K].I(=O)(=O)C1=C(C(=O)O)C=CC=C1 JBJAAHCMRSHTAO-UHFFFAOYSA-N 0.000 claims description 5
- 238000006073 displacement reaction Methods 0.000 claims description 5
- 239000012530 fluid Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 5
- 239000000376 reactant Substances 0.000 claims description 5
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 5
- 230000008961 swelling Effects 0.000 claims description 5
- 238000002604 ultrasonography Methods 0.000 claims description 5
- -1 after stirring Substances 0.000 claims description 4
- 125000004093 cyano group Chemical group *C#N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 235000016257 Mentha pulegium Nutrition 0.000 claims description 3
- 235000004357 Mentha x piperita Nutrition 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 235000001050 hortel pimenta Nutrition 0.000 claims description 3
- 239000000341 volatile oil Substances 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 2
- 241001479543 Mentha x piperita Species 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 5
- 239000007863 gel particle Substances 0.000 abstract 1
- 238000009987 spinning Methods 0.000 abstract 1
- 239000004744 fabric Substances 0.000 description 11
- 230000000694 effects Effects 0.000 description 8
- 230000000844 anti-bacterial effect Effects 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 244000246386 Mentha pulegium Species 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 238000006197 hydroboration reaction Methods 0.000 description 2
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 2
- ZQBAKBUEJOMQEX-UHFFFAOYSA-N phenyl salicylate Chemical compound OC1=CC=CC=C1C(=O)OC1=CC=CC=C1 ZQBAKBUEJOMQEX-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 241001312402 Helvella corium Species 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 244000294611 Punica granatum Species 0.000 description 1
- 235000014360 Punica granatum Nutrition 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- HVUMOYIDDBPOLL-XGKPLOKHSA-N [2-[(2r,3r,4s)-3,4-dihydroxyoxolan-2-yl]-2-hydroxyethyl] octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XGKPLOKHSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000013475 authorization Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007766 cera flava Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 description 1
- 239000008101 lactose Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229960000969 phenyl salicylate Drugs 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
-
- 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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
-
- 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
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/76—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon oxides or carbonates
-
- 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
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
-
- 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
- D06M13/005—Compositions containing perfumes; Compositions containing deodorants
-
- 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
- D06M13/11—Compounds containing epoxy groups or precursors thereof
-
- 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
- D06M13/144—Alcohols; Metal alcoholates
-
- 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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
- D06M15/05—Cellulose or derivatives thereof
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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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/15—Proteins or derivatives thereof
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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
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention relates to the field of spinning materials and discloses a method for preparing mothproof silk fiber. The method includes the steps that firstly, gamma-cyclodextrin monoacetal is prepared; secondly, silver-loaded gamma-cyclodextrin monoacetal is prepared; thirdly, cellulose-fibroin dried gel particles are prepared; fourthly, silk fiber is grafted; fifthly, the silk fiber is subjected to dipping. The prepared silk fiber is long in mothproof time, the original smoothness of silk can be kept, tensile strength of silk can be improved, and the mothproof silk fiber is environmentally friendly and free of harm and does not influence human bodies.
Description
Technical field
The present invention relates to textile material field, particularly relate to silk fiber field.
Background technology
Silkworm silk is the matured silkworm secreted concretionary continuous fiber of silk liquid, also referred to as natural silk when cocooing, and is a kind of natural
Fiber, is one of human use's animal fiber the earliest.Silkworm silk light weight and elongated, fabric sheen is good, comfortable and easy to wear, and feel is smooth
Plentiful, poor heat conductivity, moisture absorption is breathed freely, and is widely used in and knits the various silks and satins of system and knitwear.But owing to silkworm silk main component is by moving
Thing albumen, quality is the most fragile, is subject to insects and corrodes, and forms moth speckle, not only affects attractive in appearance, but also can make silk fiber
Intensity decline, easily damaged.
Authorization Notice No. is that the patent of invention of CN103741458A discloses a kind of antibacterial moth proofing agent of silk fabric, it
Be made up of the component of following parts by weight: Fructus Caryophylli powder 7-15 part, Punica granatum L. corium farinosum 7-14 part, silicone oil 5-9 part, Cera Flava 2-7 part,
Alkylolamides 3-9 part, polyvinylpyrrolidone 2-6 part, xylene monosulfonic acid potassium 4-7 part, lactose 2-7 part, starch 3-7 part, wine
Essence 20-24 part, phenyl salicylate 5-9 part, Span60 5-9 part.The silk fabric of this invention is antibacterial mothproof whole
Reason agent has antibacterial mothproof effect, excellent effect.(2) finish fabric has good washability and soft feel；(3) work is prepared
Skill is simple, harmless to human non-toxic, will not destroy the silkworm silk in silk fabric.
But the antibacterial moth proofing agent of above-mentioned silk fabric is ageing poor, it is impossible to keep effect for a long time, and to silkworm silk
After fibre finish, the compliance of silkworm silk can be affected.
Summary of the invention
In order to solve above-mentioned technical problem, the invention provides the preparation method of a kind of mothproof silk fiber.System of the present invention
The mothproof timeliness of silk fiber obtained is long, it is possible to keep the original compliance of silkworm silk, but also the stretch-proof that can promote silkworm silk is strong
Degree, and environmentally friendly, human body is not resulted in impact.
The concrete technical scheme of the present invention is: the preparation method of a kind of mothproof silk fiber, sequentially includes the following steps:
Step 1: by gamma-cyclodextrin, o-iodoxy benzoic acid potassium, dimethyl sulfoxide 5-10:3-5:100 in mass ratio mixing,
After being completely dissolved, solution is reacted in the ultrasound bath of 40-50 DEG C 8-16h；Filter after reaction, take filtrate, will filter with acetone
Liquid agitation and dilution 40-50 times, filters again, takes solid, and is dissolved with the water of solid masses 30-35 times, then carries out
Filter, take filtrate for three times, the dried gamma-cyclodextrin list aldehyde for preparing, standby.
Step 2: above-mentioned prepared part gamma-cyclodextrin list aldehyde is formulated as the gamma-cyclodextrin list that mass concentration is 4-6%
Aldehyde solution, adds the silver nitrate that quality is 0.3-0.5 times of gamma-cyclodextrin list aldehyde in gamma-cyclodextrin list aldehyde solution, stirs
After, solution ph is controlled at 4-6, under the conditions of lucifuge, be heated to 50-60 DEG C and be incubated 2-3h, being then centrifuged for isolated
Solid, solid is clean, dried, it is dissolved in sodium hydroxide solution, adding quality in sodium hydroxide solution is solid 0.5-
The sodium borohydride of 1.5%, regulates pH to 7-8, is then stirred, and recentrifuge separates and prepares after drying load silver γ-ring and sticks with paste
The single aldehyde of essence.
Step 3: cellulose, fibroin albumen are formulated as cellulose mass concentration be 2-4%, fibroin albumen quality concentration be
The mixed solution of 1-3%, successively adds the load silver gamma-cyclodextrin list aldehyde of mixed solution quality 0.5-1.5% in mixed solution
With the Ethylene glycol diglycidyl ether of mixed solution quality 0.1-0.3%, after being uniformly dispersed, mixed solution is transferred to-10 DEG C
Freeze 2-3 days to the environment of-6 DEG C, thaw after frost, prepare cellulose-fibroin hydrogel, with ethanol to cellulose-
After fibroin hydrogel carries out solvent displacement for several times, prepare cellulose-fibroin alcogel；Cellulose-fibroin alcogel is surpassed
Supercritical fluid drying, eventually passes through grinding and prepares cellulose-fibroin xerogel particles.
Step 4: successively add silk fiber, gamma-cyclodextrin list aldehyde and fiber in the aqueous hydrochloric acid solution that pH value is 5-6
Element-fibroin xerogel particles, stir post-heating to 38-42 DEG C reaction 2-3h, wherein silk fiber, gamma-cyclodextrin list aldehyde,
The mass ratio of cellulose-fibroin xerogel particles and aqueous hydrochloric acid solution is 2-3:3-5:1-3:100；Then to adding enough cyanogen
Base sodium borohydride, reacts 3-5 days, finally reactant liquor is adjusted to neutrality, is taken out by silk fiber and clean.
Step 5: the impregnation process in dressing liquid of the silk fiber after step 4 being processed, takes out after dipping and is dried,
Prepare mothproof silk fiber；Described dressing liquid includes the mothproof quintessence oil of 5-15wt%, the ethanol of 10-30wt% and the water of surplus.
Step 1 of the present invention first prepares gamma-cyclodextrin list aldehyde with gamma-cyclodextrin, and gamma-cyclodextrin list aldehyde can be grafted to silkworm silk
On fiber.In step 2, take a part of gamma-cyclodextrin list aldehyde, utilize the adsorption of gamma-cyclodextrin list aldehyde to carry out carrying silver, it is possible to
Silk fiber is made to have antibacterial effect.Step 3 cellulose, fibroin albumen, load silver gamma-cyclodextrin list aldehyde are prepared cellulose-
Fibroin xerogel particles, has extra specific surface area and outstanding adsorption, and selects cellulose, fibroin albumen as main material
Material, it is possible to promote the tensile strength of silk fiber, fibroin albumen is as the homology material of silk fiber, and affinity is more preferable, second two
Alcohol diglycidyl ether can improve the degree of cross linking in hydrogel forming process, and stability is more preferable.Step 4 is by gamma-cyclodextrin list
Aldehyde, cellulose-fibroin xerogel particles is grafted on silk fiber.Silk fiber after grafting be impregnated in dressing liquid by step 5
In, gamma-cyclodextrin list aldehyde molecule has micro-cavities, and cellulose-fibroin xerogel particles has the three-dimensional open-framework of complexity,
Both cooperate and can fully adsorb composition mothproof in dressing liquid, and absorption fastness is good, and has slow release effect, thus
Make the mothproof ageing good of silk fiber.
Further, the particle diameter of described cellulose-fibroin xerogel particles is less than or equal to 1 micron.
Further, described silk fiber before step 4 through pretreatment: silk fiber is 35-45 DEG C in temperature
Water in swelling 1-3h, by silk fiber and to impregnated in mass concentration be 0.2-0.4%'s to then take out 1:60-80 in mass ratio
In solution of potassium carbonate, boil 0.5-1h；Finally silk fiber taking-up is dried standby.
Pretreated silk fiber can preferably be grafted with gamma-cyclodextrin list aldehyde.
Further, in step 5, the impregnation technology of silk fiber is: silk fiber is 1:100-with the mass ratio of dressing liquid
200；Dressing liquid temperature is 45-55 DEG C；Dip time is 8-10h.
Further, mothproof quintessence oil described in step 5 is Deodar Cedar (Himalayan Cedar) quintessence oil, Herba Lysimachiae foenum-graeci quintessence oil, Peppermint essential oil, Radix Cinnamomi porrecti quintessence oil
In one or more mixture.
It is compared with the prior art, the invention has the beneficial effects as follows: the mothproof timeliness of silk fiber that the present invention prepares is long, it is possible to
Keep the original compliance of silkworm silk, but also the tensile strength of silkworm silk can be promoted, and environmentally friendly, human body will not be made
Become impact.Additionally, when the mothproof effect of silk fiber is deteriorated, can again be impregnated in dressing liquid.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
The preparation method of a kind of mothproof silk fiber, sequentially includes the following steps:
Step 1: by gamma-cyclodextrin, o-iodoxy benzoic acid potassium, dimethyl sulfoxide 7.5:4:100 in mass ratio mixing, complete
After CL, solution is reacted in the ultrasound bath of 45 DEG C 12h；Filter after reaction, take filtrate, with acetone, filtrate is stirred
Dilute 45 times, again filter, take solid, and dissolved with the water of solid masses 32 times, then carry out third time and filter, take filter
Liquid, the dried gamma-cyclodextrin list aldehyde for preparing, standby.
Step 2: above-mentioned prepared part gamma-cyclodextrin list aldehyde is formulated as the gamma-cyclodextrin list aldehyde that mass concentration is 5%
Solution, adds the silver nitrate that quality is 0.4 times of gamma-cyclodextrin list aldehyde in gamma-cyclodextrin list aldehyde solution, after stirring, and will
Solution ph controls 5, under the conditions of lucifuge, is heated to 55 DEG C and is incubated 2.5h, being then centrifuged for isolated solid, by solid
Clean, dried, it is dissolved in sodium hydroxide solution, in sodium hydroxide solution, adds the sodium borohydride that quality is solid 1%, adjust
Joint pH to 7.5, is then stirred, and recentrifuge separates and prepares after drying and carries silver gamma-cyclodextrin list aldehyde.
Step 3: cellulose, fibroin albumen are formulated as cellulose mass concentration be 3%, fibroin albumen quality concentration be
The mixed solution of 2%, load silver gamma-cyclodextrin list aldehyde and the mixing of successively adding mixed solution quality 1% in mixed solution are molten
The Ethylene glycol diglycidyl ether of liquid quality 0.2%, after being uniformly dispersed, is transferred in the environment of-8 DEG C frost by mixed solution
2.5 days, thaw after frost, prepare cellulose-fibroin hydrogel, with ethanol, cellulose-fibroin hydrogel is carried out for several times
After solvent displacement, prepare cellulose-fibroin alcogel；Cellulose-fibroin alcogel is carried out supercritical fluid drying, final warp
Cross and grind the cellulose-fibroin xerogel particles preparing particle diameter less than 1 micron.
Step 4: by silk fiber swelling 2h in the water that temperature is 40 DEG C, then take out 1:70 in mass ratio by silk fibroin
Tie up and impregnated in the solution of potassium carbonate that mass concentration is 0.3%, boil 45min；Finally silk fiber taking-up is dried standby.
Successively pretreated silk fiber, gamma-cyclodextrin list aldehyde and fibre is added in the aqueous hydrochloric acid solution that pH value is 5.5
Dimension element-fibroin xerogel particles, stir post-heating to 40 DEG C reaction 2.5h, wherein silk fiber, gamma-cyclodextrin list aldehyde,
The mass ratio of cellulose-fibroin xerogel particles and aqueous hydrochloric acid solution is 2.5:4:2:100；Then to adding enough cyano group boron
Sodium hydride, reacts 4 days, finally reactant liquor is adjusted to neutrality, is taken out by silk fiber and clean.
Step 5: the impregnation process in dressing liquid of the silk fiber after step 4 being processed, takes out after dipping and is dried,
Prepare mothproof silk fiber；Described dressing liquid includes the Deodar Cedar (Himalayan Cedar) quintessence oil of 5wt%, the Radix Cinnamomi porrecti quintessence oil of 5wt%, the ethanol of 20wt%
Water with surplus.Impregnation technology is: silk fiber is 1:150 with the mass ratio of dressing liquid；Dressing liquid temperature is 50 DEG C；During dipping
Between be 9h.
Embodiment 2
The preparation method of a kind of mothproof silk fiber, sequentially includes the following steps:
Step 1: by gamma-cyclodextrin, o-iodoxy benzoic acid potassium, dimethyl sulfoxide 5:3:100 in mass ratio mixing, completely
After dissolving, solution is reacted in the ultrasound bath of 40 DEG C 16h；Filter after reaction, take filtrate, filtrate is stirred dilute with acetone
Release 40 times, again filter, take solid, and dissolved with the water of solid masses 30 times, then carry out third time and filter, take filter
Liquid, the dried gamma-cyclodextrin list aldehyde for preparing, standby.
Step 2: above-mentioned prepared part gamma-cyclodextrin list aldehyde is formulated as the gamma-cyclodextrin list aldehyde that mass concentration is 4%
Solution, adds the silver nitrate that quality is 0.3 times of gamma-cyclodextrin list aldehyde in gamma-cyclodextrin list aldehyde solution, after stirring, and will
Solution ph controls 4, under the conditions of lucifuge, is heated to 50 DEG C and is incubated 3h, being then centrifuged for isolated solid, washed by solid
Only, after drying, it is dissolved in sodium hydroxide solution, in sodium hydroxide solution, adds the sodium borohydride that quality is solid 0.5%, adjust
Joint pH to 7, is then stirred, and recentrifuge separates and prepares after drying and carries silver gamma-cyclodextrin list aldehyde.
Step 3: cellulose, fibroin albumen are formulated as cellulose mass concentration be 2%, fibroin albumen quality concentration be
The mixed solution of 1%, successively adds load silver gamma-cyclodextrin list aldehyde and the mixing of mixed solution quality 0.5% in mixed solution
The Ethylene glycol diglycidyl ether of solution quality 0.1%, after being uniformly dispersed, is transferred to ice in the environment of-10 DEG C by mixed solution
Freeze 2 days, thaw after frost, prepare cellulose-fibroin hydrogel, with ethanol, cellulose-fibroin hydrogel is carried out for several times
After solvent displacement, prepare cellulose-fibroin alcogel；Cellulose-fibroin alcogel is carried out supercritical fluid drying, final warp
Cross and grind the cellulose-fibroin xerogel particles preparing particle diameter less than 1 micron.
Step 4: by silk fiber swelling 3h in the water that temperature is 35 DEG C, then take out 1:60 in mass ratio by silk fibroin
Tie up and impregnated in the solution of potassium carbonate that mass concentration is 0.2%, boil 1h；Finally silk fiber taking-up is dried standby.
Successively pretreated silk fiber, gamma-cyclodextrin list aldehyde and fiber is added in the aqueous hydrochloric acid solution that pH value is 5
Element-fibroin xerogel particles, the post-heating that stirs is to 38 DEG C of reactions 3h, wherein silk fiber, gamma-cyclodextrin list aldehyde, fibers
The mass ratio of element-fibroin xerogel particles and aqueous hydrochloric acid solution is 2:3:1:100；Then to adding enough cyano group hydroborations
Sodium, reacts 3 days, finally reactant liquor is adjusted to neutrality, is taken out by silk fiber and clean.
Step 5: the impregnation process in dressing liquid of the silk fiber after step 4 being processed, takes out after dipping and is dried,
Prepare mothproof silk fiber；Described dressing liquid includes the Herba Lysimachiae foenum-graeci quintessence oil of 5wt%, the ethanol of 10wt% and the water of surplus.Dipping
Technique is: silk fiber is 1:100 with the mass ratio of dressing liquid；Dressing liquid temperature is 45 DEG C；Dip time is 10h.
Embodiment 3
The preparation method of a kind of mothproof silk fiber, sequentially includes the following steps:
Step 1: by gamma-cyclodextrin, o-iodoxy benzoic acid potassium, dimethyl sulfoxide 10:5:100 in mass ratio mixing, completely
After dissolving, solution is reacted in the ultrasound bath of 50 DEG C 8h；Filter after reaction, take filtrate, with acetone by filtrate agitation and dilution
50 times, again filter, take solid, and dissolved with the water of solid masses 35 times, then carry out third time and filter, take filtrate,
The dried gamma-cyclodextrin list aldehyde for preparing, standby.
Step 2: above-mentioned prepared part gamma-cyclodextrin list aldehyde is formulated as the gamma-cyclodextrin list aldehyde that mass concentration is 6%
Solution, adds the silver nitrate that quality is 0.5 times of gamma-cyclodextrin list aldehyde in gamma-cyclodextrin list aldehyde solution, after stirring, and will
Solution ph controls 6, under the conditions of lucifuge, is heated to 60 DEG C and is incubated 2h, being then centrifuged for isolated solid, washed by solid
Only, after drying, it is dissolved in sodium hydroxide solution, in sodium hydroxide solution, adds the sodium borohydride that quality is solid 1.5%, adjust
Joint pH to 8, is then stirred, and recentrifuge separates and prepares after drying and carries silver gamma-cyclodextrin list aldehyde.
Step 3: cellulose, fibroin albumen are formulated as cellulose mass concentration be 4%, fibroin albumen quality concentration be
The mixed solution of 3%, successively adds load silver gamma-cyclodextrin list aldehyde and the mixing of mixed solution quality 1.5% in mixed solution
The Ethylene glycol diglycidyl ether of solution quality 0.3%, after being uniformly dispersed, is transferred in the environment of-6 DEG C frost by mixed solution
3 days, thaw after frost, prepare cellulose-fibroin hydrogel, with ethanol, cellulose-fibroin hydrogel is carried out the most molten
After agent displacement, prepare cellulose-fibroin alcogel；Cellulose-fibroin alcogel is carried out supercritical fluid drying, eventually passes through
Grind the cellulose-fibroin xerogel particles preparing particle diameter less than 1 micron.
Step 4: by silk fiber swelling 1h in the water that temperature is 45 DEG C, then take out 1:80 in mass ratio by silk fibroin
Tie up and impregnated in the solution of potassium carbonate that mass concentration is 0.4%, boil 0.5h；Finally silk fiber taking-up is dried standby.
Successively pretreated silk fiber, gamma-cyclodextrin list aldehyde and fiber is added in the aqueous hydrochloric acid solution that pH value is 6
Element-fibroin xerogel particles, the post-heating that stirs is to 42 DEG C of reactions 2h, wherein silk fiber, gamma-cyclodextrin list aldehyde, fibers
The mass ratio of element-fibroin xerogel particles and aqueous hydrochloric acid solution is 3:5:3:100；Then to adding enough cyano group hydroborations
Sodium, reacts 5 days, finally reactant liquor is adjusted to neutrality, is taken out by silk fiber and clean.
Step 5: the impregnation process in dressing liquid of the silk fiber after step 4 being processed, takes out after dipping and is dried,
Prepare mothproof silk fiber；Described dressing liquid includes the Herba Lysimachiae foenum-graeci quintessence oil of 10wt%, the Peppermint essential oil of 5wt%, the second of 30wt%
Alcohol and the water of surplus.Impregnation technology is: silk fiber is 1:200 with the mass ratio of dressing liquid；Dressing liquid temperature is 55 DEG C；Dipping
Time is 8h.
Carrying out mothproof effect through the prepared mothproof silk fiber of the embodiment of the present invention 1 to test, mothproof effect can be grown
Reach 1-2, and after repeatedly washing, still can keep better effects.Additionally to mothproof silk fiber fabric and with kind silkworm silk
Fabric carries out stiffness test, and mothproof silk fiber boardness is to declining about 3-5%, therefore to silk fiber
Pliability impact is little；To mothproof silk fiber fabric and carry out fracture strength and extension at break with kind silk fiber fabric
Rate is tested, and mothproof silk fiber fabric breaking strength rises 10-20%, and elongation at break improves 14-18%.
Raw materials used, equipment in the present invention, unless otherwise noted, is the conventional raw material of this area, equipment；In the present invention
Method therefor, unless otherwise noted, is the conventional method of this area.
The above, be only presently preferred embodiments of the present invention, not impose any restrictions the present invention, every according to the present invention
Any simple modification, change and the equivalent transformation that above example is made by technical spirit, all still falls within the technology of the present invention side
The protection domain of case.
Claims (5)
1. the preparation method of a mothproof silk fiber, it is characterised in that sequentially include the following steps:
Step 1: by gamma-cyclodextrin, o-iodoxy benzoic acid potassium, dimethyl sulfoxide 5-10:3-5:100 in mass ratio mixing, completely
After dissolving, solution is reacted in the ultrasound bath of 40-50 DEG C 8-16h；Filter after reaction, take filtrate, with acetone, filtrate is stirred
Mix dilution 40-50 times, again filter, take solid, and dissolved with the water of solid masses 30-35 times, then carry out third time
Filter, take filtrate, the dried gamma-cyclodextrin list aldehyde for preparing, standby；
Step 2: above-mentioned prepared part gamma-cyclodextrin list aldehyde is formulated as the gamma-cyclodextrin list aldehyde that mass concentration is 4-6% molten
Liquid, adds the silver nitrate that quality is 0.3-0.5 times of gamma-cyclodextrin list aldehyde in gamma-cyclodextrin list aldehyde solution, after stirring,
Solution ph is controlled at 4-6, under the conditions of lucifuge, be heated to 50-60 DEG C and be incubated 2-3h, be then centrifuged for isolated solid
Body, solid is clean, dried, it is dissolved in sodium hydroxide solution, adding quality in sodium hydroxide solution is solid 0.5-
The sodium borohydride of 1.5%, regulates pH to 7-8, is then stirred, and recentrifuge separates and prepares after drying load silver γ-ring and sticks with paste
The single aldehyde of essence；
Step 3: cellulose, fibroin albumen are formulated as cellulose mass concentration be 2-4%, fibroin albumen quality concentration be 1-
The mixed solution of 3%, successively add in mixed solution mixed solution quality 0.5-1.5% load silver gamma-cyclodextrin list aldehyde and
The Ethylene glycol diglycidyl ether of mixed solution quality 0.1-0.3%, after being uniformly dispersed, mixed solution is transferred to-10 DEG C to-
The environment of 6 DEG C freezes 2-3 days, thaws after frost, prepare cellulose-fibroin hydrogel, with ethanol to cellulose-fibroin
After hydrogel carries out solvent displacement for several times, prepare cellulose-fibroin alcogel；Cellulose-fibroin alcogel is carried out supercritical
Fluid drying, eventually passes through grinding and prepares cellulose-fibroin xerogel particles；
Step 4: successively add silk fiber, gamma-cyclodextrin list aldehyde and cellulose-silk in the aqueous hydrochloric acid solution that pH value is 5-6
Element xerogel particles, the post-heating that stirs is to 38-42 DEG C of reaction 2-3h, wherein silk fiber, gamma-cyclodextrin list aldehyde, fiber
The mass ratio of element-fibroin xerogel particles and aqueous hydrochloric acid solution is 2-3:3-5:1-3:100；Then to adding enough cyano group boron
Sodium hydride, reacts 3-5 days, finally reactant liquor is adjusted to neutrality, is taken out by silk fiber and clean；
Step 5: the impregnation process in dressing liquid of the silk fiber after step 4 being processed, takes out after dipping and is dried, and prepares
Mothproof silk fiber；Described dressing liquid includes the mothproof quintessence oil of 5-15wt%, the ethanol of 10-30wt% and the water of surplus.
The preparation method of a kind of mothproof silk fiber the most as claimed in claim 1, it is characterised in that described cellulose-fibroin
The particle diameter of xerogel particles is less than or equal to 1 micron.
The preparation method of a kind of mothproof silk fiber the most as claimed in claim 1, it is characterised in that described silk fiber is in step
Through pretreatment before rapid 4: by silk fiber swelling 1-3h in the water that temperature is 35-45 DEG C, then take out in mass ratio 1:
60-80 is by silk fiber and impregnated in the solution of potassium carbonate that mass concentration is 0.2-0.4%, boils 0.5-1h；Finally by silkworm
Silk fiber taking-up is dried standby.
The preparation method of a kind of mothproof silk fiber the most as claimed in claim 1, it is characterised in that silk fiber in step 5
Impregnation technology be: the mass ratio of silk fiber and dressing liquid is 1:100-200；Dressing liquid temperature is 45-55 DEG C；Dip time
For 8-10h.
5. the preparation method of a kind of mothproof silk fiber as described in claim 1 or 4, it is characterised in that anti-described in step 5
Moth quintessence oil is one or more mixture in Deodar Cedar (Himalayan Cedar) quintessence oil, Herba Lysimachiae foenum-graeci quintessence oil, Peppermint essential oil, Radix Cinnamomi porrecti quintessence oil.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107022826A (en) * | 2017-06-08 | 2017-08-08 | 太仓市鑫泰针织有限公司 | A kind of anti-insect type silk |
| CN110685153A (en) * | 2019-09-24 | 2020-01-14 | 江苏烨天羊绒科技有限公司 | Mothproof pure cashmere fabric and manufacturing method thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0359178A (en) * | 1989-07-28 | 1991-03-14 | Mitsubishi Rayon Co Ltd | Moth-proofing fiber |
| JPH05311509A (en) * | 1992-05-07 | 1993-11-22 | Kanebo Ltd | Insecticidal acrylic synthetic yarn and its production |
| CN101187159A (en) * | 2007-12-06 | 2008-05-28 | 浙江理工大学 | Silk fragrant fiber preparation method |
| CN101187156A (en) * | 2007-12-06 | 2008-05-28 | 浙江理工大学 | Gum-containing silk functional fiber preparation method |
| CN101187161A (en) * | 2007-12-06 | 2008-05-28 | 浙江理工大学 | Antibiotic and anti-infectious fiber preparation method |
| DE102009025190A1 (en) * | 2009-06-12 | 2010-12-16 | Call, Krimhild | Enzyme-based method for coupling- and/or crosslinking reactions of e.g. textiles, comprises coating surfaces of products, modifying suitable compounds, and coupling and/or crosslinking suitable compounds as coupling agents to the compounds |
| CN103710965A (en) * | 2013-12-28 | 2014-04-09 | 杭州泛林科技有限公司 | Preparation method of natural silk functional textile |
| CN105220479A (en) * | 2015-09-21 | 2016-01-06 | 中国丝绸博物馆 | A kind of preparation method being applicable to the silk fiber of textiles historical relic's protection |
-
2016
- 2016-08-17 CN CN201610682062.4A patent/CN106319954B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0359178A (en) * | 1989-07-28 | 1991-03-14 | Mitsubishi Rayon Co Ltd | Moth-proofing fiber |
| JPH05311509A (en) * | 1992-05-07 | 1993-11-22 | Kanebo Ltd | Insecticidal acrylic synthetic yarn and its production |
| CN101187159A (en) * | 2007-12-06 | 2008-05-28 | 浙江理工大学 | Silk fragrant fiber preparation method |
| CN101187156A (en) * | 2007-12-06 | 2008-05-28 | 浙江理工大学 | Gum-containing silk functional fiber preparation method |
| CN101187161A (en) * | 2007-12-06 | 2008-05-28 | 浙江理工大学 | Antibiotic and anti-infectious fiber preparation method |
| DE102009025190A1 (en) * | 2009-06-12 | 2010-12-16 | Call, Krimhild | Enzyme-based method for coupling- and/or crosslinking reactions of e.g. textiles, comprises coating surfaces of products, modifying suitable compounds, and coupling and/or crosslinking suitable compounds as coupling agents to the compounds |
| CN103710965A (en) * | 2013-12-28 | 2014-04-09 | 杭州泛林科技有限公司 | Preparation method of natural silk functional textile |
| CN105220479A (en) * | 2015-09-21 | 2016-01-06 | 中国丝绸博物馆 | A kind of preparation method being applicable to the silk fiber of textiles historical relic's protection |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107022826A (en) * | 2017-06-08 | 2017-08-08 | 太仓市鑫泰针织有限公司 | A kind of anti-insect type silk |
| CN110685153A (en) * | 2019-09-24 | 2020-01-14 | 江苏烨天羊绒科技有限公司 | Mothproof pure cashmere fabric and manufacturing method thereof |
| CN110685153B (en) * | 2019-09-24 | 2022-04-29 | 江苏烨天羊绒科技有限公司 | Mothproof pure cashmere fabric and manufacturing method thereof |
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