CN106319929B - A kind of preparation method of ageing-resistant silk fiber - Google Patents
A kind of preparation method of ageing-resistant silk fiber Download PDFInfo
- Publication number
- CN106319929B CN106319929B CN201610686157.3A CN201610686157A CN106319929B CN 106319929 B CN106319929 B CN 106319929B CN 201610686157 A CN201610686157 A CN 201610686157A CN 106319929 B CN106319929 B CN 106319929B
- Authority
- CN
- China
- Prior art keywords
- silk fiber
- cellulose
- gamma
- fibroin
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000000835 fiber Substances 0.000 title claims abstract description 98
- 230000032683 aging Effects 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229920000858 Cyclodextrin Polymers 0.000 claims abstract description 57
- 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 57
- 229940080345 gamma-cyclodextrin Drugs 0.000 claims abstract description 57
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 claims abstract description 55
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 45
- 239000002245 particle Substances 0.000 claims abstract description 21
- 108010022355 Fibroins Proteins 0.000 claims abstract description 18
- 239000001913 cellulose Substances 0.000 claims abstract description 13
- 229920002678 cellulose Polymers 0.000 claims abstract description 13
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000004332 silver Substances 0.000 claims abstract description 9
- 229910052709 silver Inorganic materials 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 53
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 239000007788 liquid Substances 0.000 claims description 28
- 239000007787 solid Substances 0.000 claims description 25
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 20
- 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
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000011259 mixed solution Substances 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- 239000000706 filtrate Substances 0.000 claims description 13
- 239000000341 volatile oil Substances 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 235000019441 ethanol Nutrition 0.000 claims description 10
- 239000000017 hydrogel Substances 0.000 claims description 10
- 238000005470 impregnation Methods 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
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 8
- 238000005516 engineering process Methods 0.000 claims description 7
- 238000007598 dipping method Methods 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
- 238000000227 grinding Methods 0.000 claims description 5
- 239000003921 oil Substances 0.000 claims description 5
- IFPHDUVGLXEIOQ-UHFFFAOYSA-N ortho-iodosylbenzoic acid Chemical group OC(=O)C1=CC=CC=C1I=O IFPHDUVGLXEIOQ-UHFFFAOYSA-N 0.000 claims description 5
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 5
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 5
- 239000012279 sodium borohydride Substances 0.000 claims description 5
- -1 sodium cyanoborohydrides Chemical class 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 238000002604 ultrasonography Methods 0.000 claims description 5
- 244000178870 Lavandula angustifolia Species 0.000 claims description 4
- 235000010663 Lavandula angustifolia Nutrition 0.000 claims description 4
- 238000010790 dilution Methods 0.000 claims description 4
- 239000012895 dilution Substances 0.000 claims description 4
- 238000006073 displacement reaction Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 4
- 239000001102 lavandula vera Substances 0.000 claims description 4
- 235000018219 lavender Nutrition 0.000 claims description 4
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 4
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 claims description 3
- 241000255789 Bombyx mori Species 0.000 claims description 3
- 240000005636 Dryobalanops aromatica Species 0.000 claims description 3
- 244000246386 Mentha pulegium Species 0.000 claims description 3
- 235000016257 Mentha pulegium Nutrition 0.000 claims description 3
- 235000004357 Mentha x piperita Nutrition 0.000 claims description 3
- 229920013822 aminosilicone Polymers 0.000 claims description 3
- 235000001050 hortel pimenta Nutrition 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 239000000499 gel Substances 0.000 claims 1
- 230000001580 bacterial effect Effects 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 239000004753 textile Substances 0.000 abstract description 2
- 239000004744 fabric Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 230000000844 anti-bacterial effect Effects 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 229920001353 Dextrin Polymers 0.000 description 2
- 239000004375 Dextrin Substances 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 235000019425 dextrin Nutrition 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000000034 method Methods 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
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- BEOOHQFXGBMRKU-UHFFFAOYSA-N sodium cyanoborohydride Chemical compound [Na+].[B-]C#N BEOOHQFXGBMRKU-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- HSRJKNPTNIJEKV-UHFFFAOYSA-N Guaifenesin Chemical compound COC1=CC=CC=C1OCC(O)CO HSRJKNPTNIJEKV-UHFFFAOYSA-N 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- 241000282412 Homo Species 0.000 description 1
- 206010023126 Jaundice Diseases 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
- 229920002472 Starch Polymers 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 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
- 230000003712 anti-aging effect Effects 0.000 description 1
- 238000013475 authorization Methods 0.000 description 1
- 235000013871 bee wax Nutrition 0.000 description 1
- 239000012166 beeswax Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 210000005056 cell body Anatomy 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
- 230000003111 delayed effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000004615 ingredient Substances 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
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000001737 promoting effect Effects 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
- 239000000126 substance Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0009—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Glucans, e.g. polydextrose, alternan, glycogen; (alpha-1,4)(alpha-1,6)-D-Glucans; (alpha-1,3)(alpha-1,4)-D-Glucans, e.g. isolichenan or nigeran; (alpha-1,4)-D-Glucans; (alpha-1,3)-D-Glucans, e.g. pseudonigeran; Derivatives thereof
- C08B37/0012—Cyclodextrin [CD], e.g. cycle with 6 units (alpha), with 7 units (beta) and with 8 units (gamma), large-ring cyclodextrin or cycloamylose with 9 units or more; 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
- D06M11/32—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic Table; Titanates; Zirconates; Stannates; Plumbates
-
- 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
-
- 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
-
- 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
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
- D06M15/6436—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing amino groups
-
- 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
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
- D06M16/006—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic with wool-protecting agents; with anti-moth agents
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Biochemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Materials Engineering (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Cosmetics (AREA)
Abstract
The present invention relates to textile material fields, disclose a kind of preparation method of ageing-resistant silk fiber, including：Step 1：The preparation of γ cyclodextrin list aldehyde；Step 2：Carry the preparation of silver γ cyclodextrin list aldehyde；Step 3：The preparation of cellulose fibroin titanium dioxide xerogel particles；Step 4：Silk fiber is grafted；Step 5：Silk fiber dip finishing.Silk fiber produced by the present invention can effectively delay silk fiber aging and can avoid the generation of moth spot and bacterial plaque, and timeliness is long, additionally it is possible to keep the original compliance of silk and promote the tensile strength of silk, and it is environmentally friendly, human body will not be impacted.
Description
Technical field
The present invention relates to textile material fields, more particularly to silk fiber field.
Background technology
Silk is the secreted concretionary continuous fiber of silk liquid, also referred to as natural silk when matured silkworm cocoons, and is a kind of natural
Fiber is earliest one of the animal origin of human use.Silk is light and elongated, and fabric sheen is good, comfortable and easy to wear, and feel is smooth
Plentiful, poor heat conductivity, moisture absorption is ventilative, is widely used in and weaves various silks and satins and knitwear.But since silk main component is by moving
Object albumen, quality is more fragile, and jaundice is easy after long-time illumination, is hardened；On the other hand, silk fiber is vulnerable to micro- life
Object.The erosion of insects not only influences beautiful and feel, but also can make silk fiber accelerated ageing, and intensity declines, and is easy broken
Damage.
Authorization Notice No. is that the patent of invention of CN103741458A discloses a kind of silk fabric antibacterial moth proofing agent, it
It is to be grouped as by the group of following parts by weight：7-15 parts of Fructus Caryophylli powder, 7-14 parts of granatum powder, 5-9 parts of silicone oil, 2-7 parts of beeswax,
3-9 parts of alkylolamides, 2-6 parts of polyvinylpyrrolidone, 4-7 parts of xylene monosulfonic acid potassium, 2-7 parts of lactose, 3-7 parts of starch, wine
20-24 parts smart, 5-9 parts of phenyl salicylate, 5-9 parts of Span60.The silk fabric antibacterial of the invention is mothproof whole
Reason agent has effects that antibacterial is mothproof, excellent effect.(2) finish fabric has good washability and soft feel；(3) work is prepared
Skill is simple, non-toxic to humans, will not destroy the silk in silk fabric.
But the timeliness of above-mentioned silk fabric antibacterial moth proofing agent is poor, can not keep effect for a long time, and to silk
After fibre finish, the compliance of silk can be influenced.Also, the silk fabric antibacterial moth proofing agent does not have anti-aging function.
Invention content
In order to solve the above technical problem, the present invention provides a kind of preparation methods of ageing-resistant silk fiber.The present invention
Silk fiber obtained can effectively delay silk fiber aging and can avoid the generation of moth spot and bacterial plaque, and timeliness is long, this
Outside, additionally it is possible to keep the original compliance of silk and promote the tensile strength of silk, and is environmentally friendly, human body will not be made
At influence.
The specific technical solution of the present invention is：A kind of preparation method of ageing-resistant silk fiber, carries out according to the following steps：
Step 1：By gamma-cyclodextrin, adjacent iodosobenzoic acid, dimethyl sulfoxide (DMSO) 5-10 in mass ratio:3-5:100 mixing,
Solution is reacted into 8-16h in 40-50 DEG C of ultrasound bath after being completely dissolved；It is filtered after reaction, takes filtrate, will filtered with acetone
40-50 times of liquid agitation and dilution, is filtered again, takes solid, and the water of 30-35 times of solid masses is used in combination to be dissolved, and then carries out
It filters three times, takes filtrate, gamma-cyclodextrin list aldehyde is made after dry, it is spare.
Step 2：Gamma-cyclodextrin list aldehyde in part obtained above 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 into gamma-cyclodextrin list aldehyde solution, stirs evenly
Afterwards, solution ph is controlled in 4-6, under the conditions of being protected from light, is heated to 50-60 DEG C and keeps the temperature 2-3h, be then centrifuged for isolated
Solid, solid is cleaned, after drying, is dissolved in sodium hydroxide solution, and it is solid 0.5- that quality is added into sodium hydroxide solution
1.5% sodium borohydride adjusts pH to 7-8, is then stirred, and is made after centrifuging and drying again and carries silver γ-ring paste
Smart list aldehyde.
Step 3：It is a concentration of that cellulose, fibroin albumen are formulated as a concentration of 2-4% of cellulose quality, fibroin albumen quality
The mixed solution of 1-3% successively adds the load silver gamma-cyclodextrin list aldehyde of mixed solution quality 0.5-1.5% into mixed solution
With the ethylene glycol diglycidylether of mixed solution quality 0.1-0.3%, mixed sols is made after being uniformly dispersed, by mixed sols
With titania hydrosol 4-6 in mass ratio:1 mixing, is transferred in -10 DEG C to -6 DEG C of environment after stirring evenly and freezes 2-3
It, thaws after frost, and cellulose-fibroin-titanium dioxide hydrogel is made；With ethyl alcohol to cellulose-fibroin-titanium dioxide
After hydrogel carries out solvent displacement for several times, cellulose-fibroin-titanium dioxide alcogel is made；To cellulose-fibroin-titanium dioxide
Titanium alcogel carries out supercritical fluid drying, eventually passes through grinding and cellulose-fibroin-titanium dioxide xerogel particles are made.
Step 4：Silk fiber, gamma-cyclodextrin list aldehyde and fiber are successively added into the aqueous hydrochloric acid solution that pH value is 5-6
Element-fibroin-titanium dioxide xerogel particles is heated to 38-42 DEG C of reaction 2-3h, wherein silk fiber, γ-ring after stirring evenly
The mass ratio of dextrin list aldehyde, cellulose-fibroin-titanium dioxide xerogel particles and aqueous hydrochloric acid solution is 2-3:3-5:1-3:100；
Then enough sodium cyanoborohydrides are added, reacts 3-5 days, reaction solution is finally adjusted to neutrality, silk fiber is taken out and washed
Only.
Step 5：By step 4 treated silk fiber impregnation in dressing liquid, takes out and is dried after dipping,
Ageing-resistant silk fiber is made；The dressing liquid include the mothproof essential oil of 5-15wt%, 1-3wt% hydrophilic amino silicone oil,
The ethyl alcohol of 10-30wt% and the water of surplus.
First gamma-cyclodextrin list aldehyde is made with gamma-cyclodextrin in step 1 of the present invention, and gamma-cyclodextrin list aldehyde can be grafted to silk
On fiber.In step 2, a part of gamma-cyclodextrin list aldehyde is taken, carries out carrying silver using the suction-operated of gamma-cyclodextrin list aldehyde, it can
So that silk fiber has antibacterial effect.Cellulose-is made in cellulose, fibroin albumen, the silver-colored gamma-cyclodextrin list aldehyde of load by step 3
Fibroin-titanium dioxide xerogel particles has extra specific surface area and outstanding suction-operated, and selects cellulose, fibroin albumen
As main material, the tensile strength of silk fiber, homologous substance of the fibroin albumen as silk fiber, compatibility can be promoted
More preferably, titanium dioxide has outstanding anti-light aging, and silk fiber can be delayed to be illuminated by the light yellow, aging；Ethylene glycol two contracts
Water glycerin 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, fiber
Element-fibroin-titanium dioxide xerogel particles are grafted on silk fiber.Silk fiber after grafting is impregnated in arrangement by step 5
In liquid, there are gamma-cyclodextrin list aldehyde molecule micro-cavities, cellulose-fibroin-titanium dioxide xerogel particles to have complicated three
Pore passage structure is tieed up, the two mutual cooperation can fully adsorb mothproof ingredient in dressing liquid, and absorption fastness is good, and with slow
Effect is released, to keep the mothproof timeliness of silk fiber good.
Further, the grain size of the cellulose-fibroin-titanium dioxide xerogel particles is less than or equal to 1 micron.
Further, the silk fiber passes through pretreatment before step 4：By silk fiber temperature be 35-45 DEG C
Water in be swollen 1-3h, then take out in mass ratio 1:Silk fiber is impregnated in the carbon that mass concentration is 0.2-0.4% by 60-80
In sour potassium solution, 0.5-1h is boiled；Finally silk fiber taking-up is dried spare.
Pretreated silk fiber can be preferably grafted with gamma-cyclodextrin list aldehyde.
Further, the impregnation technology of silk fiber is in step 5：The mass ratio of silk fiber and dressing liquid is 1:100-
200；Dressing liquid temperature is 45-55 DEG C；Dip time is 8-10h.
Further, mothproof essential oil described in step 5 is cedarwood essential oil, Lavender, Peppermint essential oil, cinnamomum camphora essential oil
In one or more mixtures.
It is compared with the prior art, the beneficial effects of the invention are as follows：Silk fiber produced by the present invention can effectively delay silkworm
Silk fiber aging and the generation that moth spot and bacterial plaque can be avoided, and timeliness is long, additionally it is possible to keep the original compliance of silk
It is and environmentally friendly with the tensile strength for promoting silk, human body will not be impacted.When the mothproof effect of silk fiber becomes
When poor, it can be impregnated in dressing liquid again.
Specific implementation mode
With reference to embodiment, the invention will be further described.
Embodiment 1
A kind of preparation method of ageing-resistant silk fiber, carries out according to the following steps：
Step 1：By gamma-cyclodextrin, adjacent iodosobenzoic acid, dimethyl sulfoxide (DMSO) in mass ratio 7.5:4:100 mixing, completely
Solution is reacted into 12h in 45 DEG C of ultrasound bath after dissolving；It is filtered after reaction, takes filtrate, stirred filtrate with acetone dilute
45 times are released, is filtered again, solid is taken, the water of 32 times of solid masses is used in combination to be dissolved, third time filtering is then carried out, takes filter
Gamma-cyclodextrin list aldehyde is made in liquid after dry, spare.
Step 2：Gamma-cyclodextrin list aldehyde in part obtained above 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 into gamma-cyclodextrin list aldehyde solution, will after stirring evenly
Solution ph is controlled 5, under the conditions of being protected from light, is heated to 55 DEG C and is kept the temperature 2.5h, be then centrifuged for isolated solid, by solid
It cleans, after drying, is dissolved in sodium hydroxide solution, the sodium borohydride that quality is solid 1% is added into sodium hydroxide solution, is adjusted
PH to 7.5 is saved, is then stirred, is made after centrifuging and drying again and carries silver-colored gamma-cyclodextrin list aldehyde.
Step 3：Cellulose, fibroin albumen be formulated as to cellulose quality is a concentration of 3%, fibroin albumen quality is a concentration of
2% mixed solution successively adds the load silver gamma-cyclodextrin list aldehyde of mixed solution quality 1% into mixed solution and mixes molten
Mixed sols is made, by mixed sols and titanium dioxide water in the ethylene glycol diglycidylether of liquid quality 0.2% after being uniformly dispersed
Colloidal sol in mass ratio 56:1 mixing, is transferred in -8 DEG C of environment after stirring evenly and freezes 2.5 days, thaw after frost, makes
Obtain cellulose-fibroin-titanium dioxide hydrogel；Solvent for several times is carried out with ethyl alcohol to cellulose-fibroin-titanium dioxide hydrogel to set
After changing, cellulose-fibroin-titanium dioxide alcogel is made；Shooting flow is carried out to cellulose-fibroin-titanium dioxide alcogel
Soma is dry, eventually passes through grinding and cellulose-fibroin-titanium dioxide xerogel particles that grain size is less than 1 micron are made.
Step 4：Silk fiber is swollen 2h in the water that temperature is 40 DEG C, then takes out in mass ratio 1:70 by silk fibroin
Dimension is impregnated in the solution of potassium carbonate that mass concentration is 0.3%, boils 45min；Finally silk fiber taking-up is dried spare.
Pretreated silk fiber, gamma-cyclodextrin list aldehyde and fibre are successively added in the aqueous hydrochloric acid solution for being 5.5 to pH value
Element-fibroin-titanium dioxide xerogel particles are tieed up, 40 DEG C of reaction 2.5h, wherein silk fiber, γ-ring are heated to after stirring evenly
The mass ratio of dextrin list aldehyde, cellulose-fibroin-titanium dioxide xerogel particles and aqueous hydrochloric acid solution is
2.5:4:2:100；Then enough sodium cyanoborohydrides are added, reacts 4 days, reaction solution is finally adjusted to neutrality,
Silk fiber is taken out and cleaned.
Step 5：By step 4 treated silk fiber impregnation in dressing liquid, takes out and is dried after dipping,
Ageing-resistant silk fiber is made；The dressing liquid includes the parent of the cedarwood essential oil of 5wt%, the cinnamomum camphora essential oil of 5wt%, 2wt%
The water of aqueous amido silicon oil, the ethyl alcohol of 20wt% and surplus.Impregnation technology is：The mass ratio of silk fiber and dressing liquid is 1:
150；Dressing liquid temperature is 50 DEG C；Dip time is 9h.
Embodiment 2
A kind of preparation method of ageing-resistant silk fiber, carries out according to the following steps：
Step 1：By gamma-cyclodextrin, adjacent iodosobenzoic acid, dimethyl sulfoxide (DMSO) in mass ratio 5:3:100 mixing, it is completely molten
Solution is reacted into 16h in 40 DEG C of ultrasound bath after solution；It is filtered after reaction, takes filtrate, with acetone by filtrate agitation and dilution
It 40 times, filters again, takes solid, the water of 30 times of solid masses is used in combination to be dissolved, then carry out third time filtering, take filtrate,
Gamma-cyclodextrin list aldehyde is made after drying, it is spare.
Step 2：Gamma-cyclodextrin list aldehyde in part obtained above 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 into gamma-cyclodextrin list aldehyde solution, will after stirring evenly
Solution ph is controlled 4, under the conditions of being protected from light, is heated to 50 DEG C and is kept the temperature 3h, be then centrifuged for isolated solid, solid is washed
Only it, after dry, is dissolved in sodium hydroxide solution, the sodium borohydride that quality is solid 0.5% is added into sodium hydroxide solution, is adjusted
PH to 7 is saved, is then stirred, is made after centrifuging and drying again and carries silver-colored gamma-cyclodextrin list aldehyde.
Step 3：Cellulose, fibroin albumen be formulated as to cellulose quality is a concentration of 2%, fibroin albumen quality is a concentration of
1% mixed solution successively adds load silver gamma-cyclodextrin list aldehyde and the mixing of mixed solution quality 0.5% into mixed solution
Mixed sols is made, by mixed sols and titanium dioxide in the ethylene glycol diglycidylether of solution quality 0.1% after being uniformly dispersed
The hydrosol in mass ratio 4:1 mixing, is transferred in -10 environment after stirring evenly and freezes 2 days, thaw after frost, is made
Cellulose-fibroin-titanium dioxide hydrogel；Solvent displacement for several times is carried out to cellulose-fibroin-titanium dioxide hydrogel with ethyl alcohol
Afterwards, cellulose-fibroin-titanium dioxide alcogel is made；Supercritical fluid is carried out to cellulose-fibroin-titanium dioxide alcogel
It is dry, it eventually passes through grinding and cellulose-fibroin-titanium dioxide xerogel particles that grain size is less than 1 micron is made.
Step 4：Silk fiber is swollen 3h in the water that temperature is 35 DEG C, then takes out in mass ratio 1:60 by silk fibroin
Dimension is impregnated in the solution of potassium carbonate that mass concentration is 0.2%, boils 1h；Finally silk fiber taking-up is dried spare.
Pretreated silk fiber, gamma-cyclodextrin list aldehyde and fiber are successively added in the aqueous hydrochloric acid solution for being 5 to pH value
Element-fibroin-titanium dioxide xerogel particles is heated to 38 DEG C of reaction 3h, wherein silk fiber, gamma-cyclodextrin after stirring evenly
The mass ratio of single aldehyde, cellulose-fibroin-titanium dioxide xerogel particles and aqueous hydrochloric acid solution is 2:3:1:100；Then addition foot
The sodium cyanoborohydride of amount reacts 3 days, reaction solution is finally adjusted to neutrality, silk fiber is taken out and cleaned.
Step 5：By step 4 treated silk fiber impregnation in dressing liquid, takes out and is dried after dipping,
Ageing-resistant silk fiber is made；The dressing liquid include the Lavender of 5wt%, 1wt% hydrophilic amino silicone oil,
The ethyl alcohol of 10wt% and the water of surplus.Impregnation technology is：The mass ratio of silk fiber and dressing liquid is 1:100；Dressing liquid temperature
It is 45 DEG C；Dip time is 10h.
Embodiment 3
A kind of preparation method of ageing-resistant silk fiber, carries out according to the following steps：
Step 1：By gamma-cyclodextrin, adjacent iodosobenzoic acid, dimethyl sulfoxide (DMSO) in mass ratio 10:5:100 mixing, completely
Solution is reacted into 8h in 50 DEG C of ultrasound bath after dissolving；It is filtered after reaction, takes filtrate, with acetone by filtrate agitation and dilution
It 50 times, filters again, takes solid, the water of 35 times of solid masses is used in combination to be dissolved, then carry out third time filtering, take filtrate,
Gamma-cyclodextrin list aldehyde is made after drying, it is spare.
Step 2：Gamma-cyclodextrin list aldehyde in part obtained above 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 into gamma-cyclodextrin list aldehyde solution, will after stirring evenly
Solution ph is controlled 6, under the conditions of being protected from light, is heated to 60 DEG C and is kept the temperature 2h, be then centrifuged for isolated solid, solid is washed
Only it, after dry, is dissolved in sodium hydroxide solution, the sodium borohydride that quality is solid 1.5% is added into sodium hydroxide solution, is adjusted
PH to 8 is saved, is then stirred, is made after centrifuging and drying again and carries silver-colored gamma-cyclodextrin list aldehyde.
Step 3：Cellulose, fibroin albumen be formulated as to cellulose quality is a concentration of 4%, fibroin albumen quality is a concentration of
3% mixed solution successively adds load silver gamma-cyclodextrin list aldehyde and the mixing of mixed solution quality 1.5% into mixed solution
Mixed sols is made, by mixed sols and titanium dioxide in the ethylene glycol diglycidylether of solution quality 0.3% after being uniformly dispersed
The hydrosol in mass ratio 6:1 mixing, is transferred in -6 DEG C of environment after stirring evenly and freezes 3 days, thaw after frost, is made
Cellulose-fibroin-titanium dioxide hydrogel；Solvent displacement for several times is carried out to cellulose-fibroin-titanium dioxide hydrogel with ethyl alcohol
Afterwards, cellulose-fibroin-titanium dioxide alcogel is made；Supercritical fluid is carried out to cellulose-fibroin-titanium dioxide alcogel
It is dry, it eventually passes through grinding and cellulose-fibroin-titanium dioxide xerogel particles that grain size is less than 1 micron is made.
Step 4：Silk fiber is swollen 1h in the water that temperature is 45 DEG C, then takes out in mass ratio 1:80 by silk fibroin
Dimension is impregnated in the solution of potassium carbonate that mass concentration is 0.4%, boils 0.5h；Finally silk fiber taking-up is dried spare.
Pretreated silk fiber, gamma-cyclodextrin list aldehyde and fiber are successively added in the aqueous hydrochloric acid solution for being 6 to pH value
Element-fibroin-titanium dioxide xerogel particles is heated to 42 DEG C of reaction 2h, wherein silk fiber, gamma-cyclodextrin after stirring evenly
The mass ratio of single aldehyde, cellulose-fibroin-titanium dioxide xerogel particles and aqueous hydrochloric acid solution is 3:5:3:100；Then addition foot
The sodium cyanoborohydride of amount reacts 5 days, reaction solution is finally adjusted to neutrality, silk fiber is taken out and cleaned.
Step 5：By step 4 treated silk fiber impregnation in dressing liquid, takes out and is dried after dipping,
Ageing-resistant silk fiber is made；The dressing liquid include the Lavender of 10wt%, the Peppermint essential oil of 5wt%, 3wt% parent
The water of aqueous amido silicon oil, the ethyl alcohol of 30wt% and surplus.Impregnation technology is：The mass ratio of silk fiber and dressing liquid is 1:
200；Dressing liquid temperature is 55 DEG C；Dip time is 8h.
Ageing-resistant test is carried out with type silk fiber to ageing-resistant silk fiber made from the embodiment of the present invention 1, is surveyed
Strip part is：Ageing-resistant silk fiber is placed into 200h with type silk fiber in the case where illumination is the halogen lamp of l250lx, away from
From for 30cm, temperature is controlled at 30 DEG C.It carries out fracture strength and elongation at break is tested, ageing-resistant silk fiber is compared
With type silk fiber, the high 30-40% of fracture strength, the high 20-30% of elongation at break.
Mothproof effect is carried out by ageing-resistant silk fiber made from the embodiment of the present invention 1 to be tested, mothproof effect can
Up to 1-2, and after repeatedly washing, better effects can be still kept.In addition to ageing-resistant silk fiber fabric and same type
Silk fiber fabric carries out stiffness test, ageing-resistant silk fiber boardness to decline 3-5% or so, therefore to silk
The pliability of fiber influences little.
Raw materials used in the present invention, equipment is unless otherwise noted the common raw material, equipment of this field；In the present invention
Method therefor is unless otherwise noted the conventional method of this field.
The above is only presently preferred embodiments of the present invention, is not imposed any restrictions to the present invention, every according to the present invention
Technical spirit still falls within the technology of the present invention side to any simple modification, change and equivalent transformation made by above example
The protection domain of case.
Claims (5)
1. a kind of preparation method of ageing-resistant silk fiber, it is characterised in that carry out according to the following steps：
Step 1：By gamma-cyclodextrin, adjacent iodosobenzoic acid, dimethyl sulfoxide (DMSO) 5-10 in mass ratio:3-5:100 mixing, completely
Solution is reacted into 8-16h in 40-50 DEG C of ultrasound bath after dissolving；It is filtered after reaction, takes filtrate, stirred filtrate with acetone
40-50 times of dilution is mixed, filters again, takes solid, the water of 30-35 times of solid masses is used in combination to be dissolved, then carries out third time
Filtering takes filtrate, and gamma-cyclodextrin list aldehyde is made after dry, spare；
Step 2：It is molten that gamma-cyclodextrin list aldehyde in part obtained above is formulated as the gamma-cyclodextrin list aldehyde that mass concentration is 4-6%
Liquid adds the silver nitrate that quality is 0.3-0.5 times of gamma-cyclodextrin list aldehyde into gamma-cyclodextrin list aldehyde solution, after stirring evenly,
Solution ph is controlled in 4-6, under the conditions of being protected from light, 50-60 DEG C is heated to and keeps the temperature 2-3h, be then centrifuged for isolated solid
Body, solid is cleaned, after drying, is dissolved in sodium hydroxide solution, and it is solid 0.5- that quality is added into sodium hydroxide solution
1.5% sodium borohydride adjusts pH to 7-8, is then stirred, and is made after centrifuging and drying again and carries silver γ-ring paste
Smart list aldehyde；
Step 3：Cellulose, fibroin albumen are formulated as a concentration of 2-4% of cellulose quality, a concentration of 1- of fibroin albumen quality
3% mixed solution, successively added into mixed solution mixed solution quality 0.5-1.5% load silver gamma-cyclodextrin list aldehyde and
The ethylene glycol diglycidylether of mixed solution quality 0.1-0.3%, after being uniformly dispersed be made mixed sols, by mixed sols with
Titania hydrosol 4-6 in mass ratio:1 mixing, is transferred in -10 DEG C to -6 DEG C of environment after stirring evenly and freezes 2-3 days,
It thaws after frost, cellulose-fibroin-titanium dioxide hydrogel is made；With ethyl alcohol to cellulose-fibroin-titanium dioxide water
After gel carries out solvent displacement for several times, cellulose-fibroin-titanium dioxide alcogel is made；To cellulose-fibroin-titanium dioxide
Alcogel carries out supercritical fluid drying, eventually passes through grinding and cellulose-fibroin-titanium dioxide xerogel particles are made；
Step 4：Silk fiber, gamma-cyclodextrin list aldehyde and cellulose-silk are successively added into the aqueous hydrochloric acid solution that pH value is 5-6
Element-titanium dioxide xerogel particles is heated to 38-42 DEG C of reaction 2-3h, wherein silk fiber, gamma-cyclodextrin after stirring evenly
The mass ratio of single aldehyde, cellulose-fibroin-titanium dioxide xerogel particles and aqueous hydrochloric acid solution is 2-3:3-5:1-3:100；Then
Enough sodium cyanoborohydrides are added, reacts 3-5 days, reaction solution is finally adjusted to neutrality, silk fiber is taken out and cleaned；
Step 5：By step 4 treated silk fiber impregnation in dressing liquid, takes out and be dried after dipping, be made
Ageing-resistant silk fiber；The dressing liquid includes the mothproof essential oil of 5-15wt%, the hydrophilic amino silicone oil of 1-3wt%, 10-
The ethyl alcohol of 30wt% and the water of surplus.
2. a kind of preparation method of ageing-resistant silk fiber as described in claim 1, which is characterized in that the cellulose-silk
The grain size of element-titanium dioxide xerogel particles is less than or equal to 1 micron.
3. a kind of preparation method of ageing-resistant silk fiber as described in claim 1, which is characterized in that the silk fiber exists
By pretreatment before step 4：Silk fiber is swollen 1-3h in the water that temperature is 35-45 DEG C, is then taken out, in mass ratio
1:Silk fiber is impregnated in the solution of potassium carbonate that mass concentration is 0.2-0.4% by 60-80, boils 0.5-1h；Finally by silkworm
Silk fiber taking-up is dried spare.
4. a kind of preparation method of ageing-resistant silk fiber as described in claim 1, which is characterized in that silk fibroin in step 5
The impregnation technology of dimension is：The mass ratio of silk fiber and dressing liquid is 1:100-200；Dressing liquid temperature is 45-55 DEG C；When dipping
Between be 8-10h.
5. a kind of preparation method of ageing-resistant silk fiber as described in claim 1 or 4, which is characterized in that described in step 5
Mothproof essential oil is one or more mixtures in cedarwood essential oil, Lavender, Peppermint essential oil, cinnamomum camphora essential oil.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610686157.3A CN106319929B (en) | 2016-08-17 | 2016-08-17 | A kind of preparation method of ageing-resistant silk fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610686157.3A CN106319929B (en) | 2016-08-17 | 2016-08-17 | A kind of preparation method of ageing-resistant silk fiber |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106319929A CN106319929A (en) | 2017-01-11 |
| CN106319929B true CN106319929B (en) | 2018-07-31 |
Family
ID=57744270
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610686157.3A Active CN106319929B (en) | 2016-08-17 | 2016-08-17 | A kind of preparation method of ageing-resistant silk fiber |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106319929B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107142717A (en) * | 2017-06-28 | 2017-09-08 | 南通大学 | A kind of production method of the anti-aging geotextiles of the hydrosol |
| CN108309168A (en) * | 2017-12-31 | 2018-07-24 | 广州海鑫无纺布实业有限公司 | A kind of preparation method of high-durability frosted cleaning cloth |
| CN114904388B (en) * | 2022-04-18 | 2023-08-22 | 广西科技大学 | Ag@ essential oil @ cyclodextrin/bamboo charcoal @ TiO 2 Nanomaterial and application thereof |
| CN115748255B (en) * | 2022-11-28 | 2024-06-25 | 浙江理工大学 | High-conductivity scrubbing-resistant intelligent sensing silk fiber and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102373618A (en) * | 2011-11-18 | 2012-03-14 | 张家港耐尔纳米科技有限公司 | Silver-carried alginic acid fiber and preparation method thereof |
| CN104530437A (en) * | 2014-12-02 | 2015-04-22 | 天津工业大学 | Preparation method of cyclodextrin grafted chitosan polymer with water pollutant separating property |
| 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 |
| CN105837861A (en) * | 2016-04-03 | 2016-08-10 | 苏鑫 | Composite natural polymer gel material |
-
2016
- 2016-08-17 CN CN201610686157.3A patent/CN106319929B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102373618A (en) * | 2011-11-18 | 2012-03-14 | 张家港耐尔纳米科技有限公司 | Silver-carried alginic acid fiber and preparation method thereof |
| CN104530437A (en) * | 2014-12-02 | 2015-04-22 | 天津工业大学 | Preparation method of cyclodextrin grafted chitosan polymer with water pollutant separating property |
| 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 |
| CN105837861A (en) * | 2016-04-03 | 2016-08-10 | 苏鑫 | Composite natural polymer gel material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106319929A (en) | 2017-01-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106319929B (en) | A kind of preparation method of ageing-resistant silk fiber | |
| CN105256544B (en) | A kind of high-performance natural silk fiber and preparation method thereof | |
| CN101724920B (en) | Method for preparing regenerated silk fiber by means of dry spinning | |
| US20030134120A1 (en) | Natural fiber coated with chitosan and a method for producing the same | |
| CN108998858B (en) | Hydrogel type alginate fiber membrane cloth and preparation method thereof | |
| CN110904522A (en) | Fullerene skin-friendly composite fiber and preparation method thereof | |
| CN110682626B (en) | Antibacterial graphene cloth and preparation method thereof | |
| CN108468206A (en) | A kind of preparation method of the silk fabric of functionalization | |
| CN105821518B (en) | A kind of preparation method of pupa albumen/lotus cellulose composite fiber | |
| CN106928729A (en) | A kind of nanometer silver antimicrobial regenerated silk fibroin material and preparation method thereof | |
| CN108660755A (en) | A kind of preparation method of the modified silk fiber of highly hygroscopic moisture retention | |
| CN106987944B (en) | Sun-proof anti-bacterial fibre mixed yarn | |
| WO2020224261A1 (en) | Boron-doped biologically active glass microspheres and preparation method therefor and use thereof | |
| CN104878467A (en) | Nano-aluminum oxide-feeding silkworm rearing method for preparing high-performance silk and product prepared by nano-aluminum oxide-feeding silkworm rearing method | |
| CN108277548B (en) | Graphene polyester flame-retardant fiber and preparation method thereof | |
| CN105951211A (en) | Antibacterial self-cleaned artificial wig fiber containing peacock feather | |
| CN106319954B (en) | A kind of preparation method of mothproof silk fiber | |
| CN101503834B (en) | Collagen - Na-MMT complex fiber, and spinning technological process thereof | |
| EP3369859B1 (en) | High performance natural silk fiber and preparation method thereof | |
| CN105316785A (en) | Preparation method of Chinese mugwort fibers | |
| CN110183860A (en) | A kind of fibroin/nylon composite materials and its application | |
| CN110453311A (en) | A kind of warming chitin fiber and preparation method thereof | |
| CN107338651A (en) | A kind of technique that highly hygroscopic moisturizing stretch-proof fabric is prepared using silk | |
| CN112323163A (en) | Lavender-containing viscose fiber and preparation method thereof | |
| CN113774659A (en) | Preparation method of centella asiatica fiber |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20180709 Address after: 515000 Si Huang industrial zone, Lu Gang Town, Chaonan District, Shantou, Guangdong Applicant after: Yongxin Shantou Weaving Co., Ltd. Address before: 322304 No. 147 village, Pan Feng Village, Panan County, Jinhua, Zhejiang Applicant before: Chen Kaitai |
|
| TA01 | Transfer of patent application right | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 515000 Si Huang industrial zone, Lu Gang Town, Chaonan District, Shantou, Guangdong Patentee after: Huamei Fashion Co.,Ltd. Address before: 515000 Si Huang industrial zone, Lu Gang Town, Chaonan District, Shantou, Guangdong Patentee before: SHANTOU YONGXIN WEAVING Co.,Ltd. |
|
| CP01 | Change in the name or title of a patent holder | ||
| CP03 | Change of name, title or address |
Address after: 515000 lianbei Industrial Zone, Heping Town, Chaoyang District, Shantou City, Guangdong Province Patentee after: Huamei Fashion Group Co.,Ltd. Address before: 515000 Si Huang industrial zone, Lu Gang Town, Chaonan District, Shantou, Guangdong Patentee before: Huamei Fashion Co.,Ltd. |
|
| CP03 | Change of name, title or address |