CN107419519A - A kind of preparation method of the affine uvioresistant anti bacteria natural silk fiber of zinc oxide - Google Patents
A kind of preparation method of the affine uvioresistant anti bacteria natural silk fiber of zinc oxide Download PDFInfo
- Publication number
- CN107419519A CN107419519A CN201710578368.XA CN201710578368A CN107419519A CN 107419519 A CN107419519 A CN 107419519A CN 201710578368 A CN201710578368 A CN 201710578368A CN 107419519 A CN107419519 A CN 107419519A
- Authority
- CN
- China
- Prior art keywords
- silk fiber
- zinc oxide
- affine
- silk
- preparation
- 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.)
- Pending
Links
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 239000000835 fiber Substances 0.000 title claims abstract description 69
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 37
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 32
- PXFBZOLANLWPMH-UHFFFAOYSA-N 16-Epiaffinine Natural products C1C(C2=CC=CC=C2N2)=C2C(=O)CC2C(=CC)CN(C)C1C2CO PXFBZOLANLWPMH-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000005406 washing Methods 0.000 claims abstract description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 16
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims abstract description 13
- JJTUDXZGHPGLLC-UHFFFAOYSA-N lactide Chemical compound CC1OC(=O)C(C)OC1=O JJTUDXZGHPGLLC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000010695 polyglycol Substances 0.000 claims abstract description 11
- 229920000151 polyglycol Polymers 0.000 claims abstract description 11
- WWZKQHOCKIZLMA-UHFFFAOYSA-M octanoate Chemical compound CCCCCCCC([O-])=O WWZKQHOCKIZLMA-UHFFFAOYSA-M 0.000 claims abstract description 10
- 238000010792 warming Methods 0.000 claims abstract description 10
- 238000001994 activation Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 8
- 239000012535 impurity Substances 0.000 claims abstract description 8
- 238000009413 insulation Methods 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 8
- 239000007800 oxidant agent Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 8
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 7
- 229960001763 zinc sulfate Drugs 0.000 claims description 7
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 7
- 230000003115 biocidal effect Effects 0.000 abstract description 5
- 238000002791 soaking Methods 0.000 abstract description 5
- 238000004332 deodorization Methods 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract 1
- 229960001296 zinc oxide Drugs 0.000 description 27
- 230000000052 comparative effect Effects 0.000 description 19
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical class [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000004744 fabric Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 108010022355 Fibroins Proteins 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 241000255789 Bombyx mori Species 0.000 description 2
- 241000222122 Candida albicans Species 0.000 description 2
- 241000588724 Escherichia coli Species 0.000 description 2
- 241000191967 Staphylococcus aureus Species 0.000 description 2
- 230000000845 anti-microbial effect Effects 0.000 description 2
- 229940095731 candida albicans Drugs 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 1
- 102000008186 Collagen Human genes 0.000 description 1
- 108010035532 Collagen Proteins 0.000 description 1
- 229920000832 Cutin Polymers 0.000 description 1
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical class COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 125000003716 cholic acid group Chemical group 0.000 description 1
- 229920001436 collagen Polymers 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 210000000245 forearm Anatomy 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- -1 iso caprylates Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000005445 natural material Substances 0.000 description 1
- 238000012946 outsourcing Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 description 1
- 229940007718 zinc hydroxide Drugs 0.000 description 1
- 229910021511 zinc hydroxide Inorganic materials 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
- 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
- D06M11/44—Oxides or hydroxides of elements of Groups 2 or 12 of the Periodic Table; Zincates; Cadmates
-
- 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
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/003—Treatment with radio-waves or microwaves
-
- 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
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
- D06M10/08—Organic compounds
- D06M10/10—Macromolecular compounds
-
- 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
- D06M15/507—Polyesters
-
- 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
- D06M15/53—Polyethers
-
- 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
-
- 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
-
- 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
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/25—Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments
-
- 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
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/50—Modified hand or grip properties; Softening compositions
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention provides a kind of preparation method of the affine uvioresistant anti bacteria natural silk fiber of zinc oxide, comprise the following steps：After silk is gone into the removal of impurity, degumming, it is washed with deionized, is dried to obtain boiled silk；Boiled silk is used into strong oxidizer activation process, is then impregnated in zinc nitrate aqueous solution, is filtered, washing, then be soaked in ammoniacal liquor, temperature is adjusted, insulation obtains pre cap silk fiber；Dichloromethane is added into pre cap silk fiber to be well mixed; add poly glycol monomethyl ether, lactide, stannous iso caprylate mixing; under nitrogen protection; microwave treatment; filtering, washing, is placed in the steam of warming and humidifying and stands; washing, drying obtain the affine uvioresistant anti bacteria natural silk fiber of zinc oxide.Gained silk fiber of the invention not only has excellent uvioresistant performance, and bacteriostasis antibiosis deodorization, resistance to washing by soaking, good hygroscopicity are comfortable and easy to wear.
Description
Technical field
The present invention relates to textile technology field, especially, is related to a kind of affine uvioresistant anti bacteria natural silk fiber of zinc oxide
Preparation method.
Background technology
With the improvement of living standards, people increasingly pursue natural material product, such as silk, when silk is that matured silkworm cocoons
The concretionary continuous fiber of silk liquid is secreted, also referred to as " natural silk ".It is the animal that the mankind utilize earliest as wool
One of fiber, silk fiber are made up of two triangular in shape or half elliptic fibroin outsourcing silk gum, and cross section is oval.
Silk fiber is protein fibre, and silk gum and fibroin are its chief components, and wherein fibroin accounts for 3/4, and silk gum accounts for 1/4,
The cutin and collagen of silk and human body are all protein, and structure is very close, therefore, have fabulous human-body biological compatibility.
Silk fiber material turns into the first choice of people due to outstanding bioaffinity.But the antibiotic ultraviolet-resistant of silk fiber
It is poor；A kind of uvioresistant silkworm of modified zinc oxide is disclosed in Chinese patent CN104594025B (publication date 2015.05.06)
Silk preparation method, by silk go clean degumming after surface activation process, be impregnated in the precursor solution of zinc, then be soaked in
Reacted in reaction dissolvent, obtain the silk of zinc hydroxide covering, be placed in the steam of warming and humidifying and stand, take out washing drying,
The silk of modified zinc oxide is obtained, but affinity is poor, is easy to run off after washing by soaking, it would be highly desirable to solve.
The content of the invention
Based on technical problem existing for background technology, the present invention proposes a kind of affine uvioresistant anti bacteria natural silk of zinc oxide
The preparation method of fiber, gained silk fiber not only have excellent uvioresistant performance, and bacteriostasis antibiosis deodorization, resistance to immersion
Washing, good hygroscopicity are comfortable and easy to wear.
A kind of preparation method of the affine uvioresistant anti bacteria natural silk fiber of zinc oxide proposed by the present invention, including following step
Suddenly：
S1, after silk is gone into the removal of impurity, degumming, it is washed with deionized, is dried to obtain boiled silk；
S2, boiled silk used into strong oxidizer activation process, be then impregnated in zinc nitrate aqueous solution, filtered, washing,
It is soaked in again in ammoniacal liquor, adjusts temperature, insulation obtains pre cap silk fiber；
S3, into pre cap silk fiber add dichloromethane be well mixed, add poly glycol monomethyl ether, lactide,
Stannous iso caprylate mixes, and under nitrogen protection, microwave treatment, filters, washing, is placed in the steam of warming and humidifying and stands, water
Wash, drying obtains the affine uvioresistant anti bacteria natural silk fiber of zinc oxide.
The present invention, in one layer of zinc-oxide film of Surface Creation of silk, surface is covered after the activated processing of boiled silk
The silk of lid zinc-oxide film is immersed in dichloromethane, poly glycol monomethyl ether and lactide is added, in urging for stannous iso caprylate
Under change, forming copolymer has hydrophobic block end cholic acid group, can improve affinity of the zinc oxide on silk surface, surely
It is qualitative good, not easily runed off after washing by soaking, the hydrophilic block of copolymer surrounds outer formation protectiveness shell in addition, no
Only silk surface nondestructive is hindered, hygroscopicity is fabulous, comfortable and easy to wear, and preparation method is easy, and cost is cheap, suitable for big rule
Mould produces.
Preferably, in S3, pre cap silk fiber, dichloromethane, poly glycol monomethyl ether, lactide, stannous iso caprylate
Mass ratio be 4-10：60-80：4-10：0.5-2：0.01-0.06.
Preferably, in S3, the time of microwave treatment is 15-25min, and the power of microwave treatment is 150-240W.
By limiting raw material proportioning and technological parameter in above-mentioned S3, make affinity in silk fiber obtained by the present invention higher,
Not easily runed off after soaking washing, and make gained silk fiber comfortable and easy to wear.
Preferably, in S2, the mass fraction of zinc sulfate solution is 30-40%.
Preferably, in S2, dip time 10-20min.
Preferably, in S2,50-60 DEG C is adjusted the temperature to, is incubated 10-20min.
The present invention makes the zinc-oxide film of silk Surface Creation more uniform by being adjusted to related process in S2,
And injury will not be produced to silk.
The gained affine uvioresistant anti bacteria natural silk fiber of zinc oxide of the invention not only has excellent uvioresistant performance, and
Bacteriostasis antibiosis deodorization, resistance to washing by soaking, good hygroscopicity are comfortable and easy to wear.
In addition to objects, features and advantages described above, the present invention also has other objects, features and advantages.
Below, the present invention is further detailed explanation.
Embodiment
Embodiments of the invention are described in detail below, but the present invention can be limited and covered according to claim
Multitude of different ways implement.
Embodiment 1
A kind of preparation method of the affine uvioresistant anti bacteria natural silk fiber of zinc oxide, comprises the following steps：
S1, after silk is gone into the removal of impurity, degumming, it is washed with deionized, is dried to obtain boiled silk；
S2, boiled silk used into strong oxidizer activation process, be then impregnated in the zinc sulfate water that mass fraction is 30%
20min in solution, filter, washing, then be soaked in the ammoniacal liquor that mass fraction is 40%, adjust the temperature to 60 DEG C, insulation
10min, obtain pre cap silk fiber；
S3, into 10 parts of pre cap silk fibers, 60 parts of dichloromethane of addition are well mixed by weight, are added 10 parts and are gathered
Glycol monoethyl ether, 0.5 part of lactide, the mixing of 0.06 part of stannous iso caprylate, under nitrogen protection, microwave treatment 15min are micro-
The power of ripple processing is 240W, is filtered, and washing, is placed in the steam of warming and humidifying and stands, and is washed, and drying obtains zinc oxide parent
With uvioresistant anti bacteria natural silk fiber.
Embodiment 2
A kind of preparation method of the affine uvioresistant anti bacteria natural silk fiber of zinc oxide, comprises the following steps：
S1, after silk is gone into the removal of impurity, degumming, it is washed with deionized, is dried to obtain boiled silk；
S2, boiled silk used into strong oxidizer activation process, be then impregnated in the zinc sulfate water that mass fraction is 40%
10min in solution, filter, washing, then be soaked in the ammoniacal liquor that mass fraction is 50%, adjust the temperature to 50 DEG C, insulation
20min, obtain pre cap silk fiber；
S3, into 4 parts of pre cap silk fibers, 80 parts of dichloromethane of addition are well mixed by weight, add 4 parts of poly- second
Glycol monomethyl ether, 2 parts of lactides, the mixing of 0.01 part of stannous iso caprylate, under nitrogen protection, microwave treatment 25min, at microwave
The power of reason is 150W, is filtered, and washing, is placed in the steam of warming and humidifying and stands, and is washed, and it is affine anti-that drying obtains zinc oxide
Ultraviolet anti bacteria natural silk fiber.
Embodiment 3
A kind of preparation method of the affine uvioresistant anti bacteria natural silk fiber of zinc oxide, comprises the following steps：
S1, after silk is gone into the removal of impurity, degumming, it is washed with deionized, is dried to obtain boiled silk；
S2, boiled silk used into strong oxidizer activation process, be then impregnated in the zinc sulfate water that mass fraction is 32%
18min in solution, filter, washing, then be soaked in the ammoniacal liquor that mass fraction is 40%, adjust the temperature to 58 DEG C, insulation
12min, obtain pre cap silk fiber；
S3, into 8 parts of pre cap silk fibers, 65 parts of dichloromethane of addition are well mixed by weight, add 8 parts of poly- second
Glycol monomethyl ether, 1 part of lactide, the mixing of 0.04 part of stannous iso caprylate, under nitrogen protection, microwave treatment 18min, at microwave
The power of reason is 220W, is filtered, and washing, is placed in the steam of warming and humidifying and stands, and is washed, and it is affine anti-that drying obtains zinc oxide
Ultraviolet anti bacteria natural silk fiber.
Embodiment 4
A kind of preparation method of the affine uvioresistant anti bacteria natural silk fiber of zinc oxide, comprises the following steps：
S1, after silk is gone into the removal of impurity, degumming, it is washed with deionized, is dried to obtain boiled silk；
S2, boiled silk used into strong oxidizer activation process, be then impregnated in the zinc sulfate water that mass fraction is 38%
12min in solution, filter, washing, then be soaked in the ammoniacal liquor that mass fraction is 50%, adjust the temperature to 52 DEG C, insulation
18min, obtain pre cap silk fiber；
S3, into 6 parts of pre cap silk fibers, 75 parts of dichloromethane of addition are well mixed by weight, add 6 parts of poly- second
Glycol monomethyl ether, 1.5 parts of lactides, 0.02 part of stannous iso caprylate mixing, under nitrogen protection, microwave treatment 22min, microwave
The power of processing is 180W, is filtered, and washing, is placed in the steam of warming and humidifying and stands, and is washed, and it is affine that drying obtains zinc oxide
Uvioresistant anti bacteria natural silk fiber.
Embodiment 5
A kind of preparation method of the affine uvioresistant anti bacteria natural silk fiber of zinc oxide, comprises the following steps：
S1, after silk is gone into the removal of impurity, degumming, it is washed with deionized, is dried to obtain boiled silk；
S2, boiled silk used into strong oxidizer activation process, be then impregnated in the zinc sulfate water that mass fraction is 35%
15min in solution, filter, washing, then be soaked in the ammoniacal liquor that mass fraction is 45%, adjust the temperature to 55 DEG C, insulation
15min, obtain pre cap silk fiber；
S3, into 7g pre cap silk fibers, addition 70g dichloromethane is well mixed, addition 7g poly glycol monomethyl ethers,
1.2g lactides, the mixing of 0.03g stannous iso caprylates, under nitrogen protection, microwave treatment 20min, the power of microwave treatment is
200W, filter, washing, be placed in the steam of warming and humidifying and stand, wash, drying obtains the affine uvioresistant antibacterial of zinc oxide
Silk fiber.
Comparative example 1
Compared with Example 5, its difference is：It is same as Example 5 without poly glycol monomethyl ether, remaining step in S3.
Comparative example 2
Compared with Example 5, its difference is：Poly glycol monomethyl ether is 2g, remaining step and the phase of embodiment 5 in S3
Together.
Comparative example 3
Compared with Example 5, its difference is：Poly glycol monomethyl ether is 12g, remaining step and the phase of embodiment 5 in S3
Together.
Comparative example 4
Compared with Example 5, its difference is：It is same as Example 5 without lactide, remaining step in S3.
Comparative example 5
Compared with Example 5, its difference is：Lactide is 0.2g in S3, and remaining step is same as Example 5.
Comparative example 6
Compared with Example 5, its difference is：Lactide is 2.5g in S3, and remaining step is same as Example 5.
Comparative example 7
Compared with Example 5, its difference is：It is same as Example 5 without stannous iso caprylate, remaining step in S3.
Comparative example 8
Compared with Example 5, its difference is：It is same as Example 5 without microwave treatment, remaining step in S3.
Comparative example 9
Compared with Example 5, its difference is：" microwave treatment 20min, the power of microwave treatment change for 200W " in S3
" to be warming up to 70 DEG C, being incubated 30min ", remaining step is same as Example 5.
3-5 of the embodiment of the present invention and comparative example 1-15 is subjected to performance test, its result is as follows：
| Elongation at break, % | Hydroscopicity, % | |
| Embodiment 3 | 99 | 30 |
| Embodiment 4 | 96 | 32 |
| Embodiment 5 | 101 | 34 |
| Comparative example 1 | 63 | 19 |
| Comparative example 2 | 76 | 23 |
| Comparative example 3 | 82 | 25 |
| Comparative example 4 | 66 | 22 |
| Comparative example 5 | 77 | 23 |
| Comparative example 6 | 86 | 26 |
| Comparative example 7 | 64 | 21 |
| Comparative example 8 | 69 | 24 |
| Comparative example 9 | 84 | 28 |
After 200 washings, performance test is carried out again, its result is as follows：
As seen from the above table,；The silk of surface of the present invention covering zinc-oxide film is through poly glycol monomethyl ether, lactide, different
Stannous octoate cooperation handle, make gained silk fiber hydrophily it is fabulous, moisture pick-up properties is excellent, and mechanical property is fabulous.
By the affine uvioresistant anti bacteria natural silk fiber of zinc oxide obtained by embodiment 3-5 with untreated silk fiber, openly
Day carries out performance survey for the uvioresistant silk of modified zinc oxide obtained by the Chinese patent CN104594025B on May 6th, 2015
Examination, it is as shown in the table to its ultraviolet-resistent property, mechanical property, moisture pick-up properties result：
By the affine uvioresistant anti bacteria natural silk fiber of the gained zinc oxide of embodiment 5 and untreated silk fiber, publication date
Uvioresistant silk for modified zinc oxide obtained by the Chinese patent CN104594025B on May 6th, 2015 is made into fabric, then
Influence of the above-mentioned fabric to human body is tested, test condition is：Temperature is 19-21 DEG C, and humidity is 48-52%R.H. indoor bar
Under part, the man and Ms that randomly select 20-40 year are tested, and are first adapted to environment 10min, are then put on test fabric
30min, to being tested before wearing the clothes and after wearing the clothes in the middle part of the forearm of human body, its result is as shown in the table：
By the affine uvioresistant anti bacteria natural silk fiber of the gained zinc oxide of embodiment 5 and untreated silk fiber, publication date
Anti-microbial property survey is carried out for the uvioresistant silk of modified zinc oxide obtained by the Chinese patent CN104594025B on May 6th, 2015
Examination, its result are as shown in the table：
| Bacteriostasis rate | Embodiment 5 | Untreated silk fiber | The uvioresistant silk of modified zinc oxide |
| Candida albicans, % | 96 | 23 | 90 |
| Staphylococcus aureus, % | 97 | 18 | 90 |
| Escherichia coli, % | 98 | 25 | 92 |
By the affine uvioresistant anti bacteria natural silk fiber of the gained zinc oxide of embodiment 5 and untreated silk fiber, publication date
For on May 6th, 2015 Chinese patent CN104594025B obtained by modified zinc oxide uvioresistant silk wash 200 times it is laggard
Row anti-microbial property test, its result are as shown in the table：
| Embodiment 5 | Untreated silk fiber | The uvioresistant silk of modified zinc oxide | |
| Candida albicans, % | 88 | 20 | 50 |
| Staphylococcus aureus, % | 90 | 17 | 48 |
| Escherichia coli, % | 89 | 22 | 52 |
By the affine uvioresistant anti bacteria natural silk fiber of the gained zinc oxide of embodiment 5 and untreated silk fiber, publication date
For on May 6th, 2015 Chinese patent CN104594025B obtained by modified zinc oxide uvioresistant silk wash 200 times it is laggard
Row ultraviolet-resistent property, Mechanics Performance Testing, its result are as shown in the table：
| Embodiment 5 | Untreated silk fiber | The uvioresistant silk of modified zinc oxide | |
| Uvioresistant coefficient, UPF | 95 | 5 | 52 |
| Ultimate strength, N | 261 | 175 | 203 |
| Elongation at break, % | 94 | 43 | 46 |
| Hydroscopicity, % | 30 | 15 | 16 |
From above-mentioned data, the anti-ultraviolet property of the affine uvioresistant anti bacteria natural silk fiber of zinc oxide obtained by this method
Excellent, washing resistance performance is fabulous, and the antibiotic property of fabric and mechanical strength have a lifting, and good hygroscopicity is comfortable and easy to wear.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.Within the spirit and principles of the invention, that is made is any
Modification, equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (6)
1. a kind of preparation method of the affine uvioresistant anti bacteria natural silk fiber of zinc oxide, it is characterised in that comprise the following steps：
S1, after silk is gone into the removal of impurity, degumming, it is washed with deionized, is dried to obtain boiled silk；
S2, boiled silk used into strong oxidizer activation process, be then impregnated in zinc nitrate aqueous solution, filtered, washing, then soak
Steep in ammoniacal liquor, adjust temperature, insulation obtains pre cap silk fiber；
S3, add dichloromethane into pre cap silk fiber and be well mixed, add poly glycol monomethyl ether, lactide, different pungent
Sour stannous mixing, under nitrogen protection, microwave treatment, filters, washing, is placed in the steam of warming and humidifying and stands, wash, drying
Obtain the affine uvioresistant anti bacteria natural silk fiber of zinc oxide.
2. the preparation method of the affine uvioresistant anti bacteria natural silk fiber of zinc oxide according to claim 1, it is characterised in that S3
In, pre cap silk fiber, dichloromethane, poly glycol monomethyl ether, lactide, the mass ratio of stannous iso caprylate are 4-10：60-
80：4-10：0.5-2：0.01-0.06.
3. the preparation method of the affine uvioresistant anti bacteria natural silk fiber of zinc oxide according to claim 1, it is characterised in that S3
In, the time of microwave treatment is 15-25min, and the power of microwave treatment is 150-240W.
4. according to the preparation method of the affine uvioresistant anti bacteria natural silk fiber of any one of the claim 1-3 zinc oxide, it is special
Sign is, in S2, the mass fraction of zinc sulfate solution is 30-40%.
5. according to the preparation method of the affine uvioresistant anti bacteria natural silk fiber of any one of the claim 1-3 zinc oxide, it is special
Sign is, in S2, dip time 10-20min.
6. according to the preparation method of the affine uvioresistant anti bacteria natural silk fiber of any one of the claim 1-3 zinc oxide, it is special
Sign is, in S2, adjusts the temperature to 50-60 DEG C, is incubated 10-20min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710578368.XA CN107419519A (en) | 2017-07-16 | 2017-07-16 | A kind of preparation method of the affine uvioresistant anti bacteria natural silk fiber of zinc oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710578368.XA CN107419519A (en) | 2017-07-16 | 2017-07-16 | A kind of preparation method of the affine uvioresistant anti bacteria natural silk fiber of zinc oxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107419519A true CN107419519A (en) | 2017-12-01 |
Family
ID=60427198
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710578368.XA Pending CN107419519A (en) | 2017-07-16 | 2017-07-16 | A kind of preparation method of the affine uvioresistant anti bacteria natural silk fiber of zinc oxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107419519A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109680480A (en) * | 2018-11-28 | 2019-04-26 | 湖州品创孵化器有限公司 | A kind of preparation method of health uvioresistant silk fabric |
| CN109695150A (en) * | 2018-11-28 | 2019-04-30 | 湖州品创孵化器有限公司 | A kind of preparation method of pro-skin type uvioresistant silk fabric |
| CN113417092A (en) * | 2021-06-24 | 2021-09-21 | 苏州市德赫亚新纺织科技有限公司 | Preparation method of antibacterial, acarid-removing and ultraviolet-proof silk fabric |
| CN116694077A (en) * | 2023-05-06 | 2023-09-05 | 宁国市瑞普密封件有限公司 | High-strength polyphenylene sulfide-based plastic and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1900141A (en) * | 2006-07-12 | 2007-01-24 | 哈尔滨工业大学 | Process for in site preparing poly lactic acid/poly ethylene glycol copolymer by microwave radiation |
| CN104594025A (en) * | 2015-02-03 | 2015-05-06 | 湖州新创丝织品有限公司 | Method for preparing novel zinc-oxide-modified ultraviolet-resistant silk |
| CN106835673A (en) * | 2017-03-27 | 2017-06-13 | 广西科技大学 | A kind of UV resistance zinc oxide silk composite fiber and preparation method thereof |
-
2017
- 2017-07-16 CN CN201710578368.XA patent/CN107419519A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1900141A (en) * | 2006-07-12 | 2007-01-24 | 哈尔滨工业大学 | Process for in site preparing poly lactic acid/poly ethylene glycol copolymer by microwave radiation |
| CN104594025A (en) * | 2015-02-03 | 2015-05-06 | 湖州新创丝织品有限公司 | Method for preparing novel zinc-oxide-modified ultraviolet-resistant silk |
| CN106835673A (en) * | 2017-03-27 | 2017-06-13 | 广西科技大学 | A kind of UV resistance zinc oxide silk composite fiber and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109680480A (en) * | 2018-11-28 | 2019-04-26 | 湖州品创孵化器有限公司 | A kind of preparation method of health uvioresistant silk fabric |
| CN109695150A (en) * | 2018-11-28 | 2019-04-30 | 湖州品创孵化器有限公司 | A kind of preparation method of pro-skin type uvioresistant silk fabric |
| CN113417092A (en) * | 2021-06-24 | 2021-09-21 | 苏州市德赫亚新纺织科技有限公司 | Preparation method of antibacterial, acarid-removing and ultraviolet-proof silk fabric |
| CN116694077A (en) * | 2023-05-06 | 2023-09-05 | 宁国市瑞普密封件有限公司 | High-strength polyphenylene sulfide-based plastic and preparation method thereof |
| CN116694077B (en) * | 2023-05-06 | 2024-03-08 | 宁国市瑞普密封件有限公司 | High-strength polyphenylene sulfide-based plastic and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107419519A (en) | A kind of preparation method of the affine uvioresistant anti bacteria natural silk fiber of zinc oxide | |
| CN107313244A (en) | The technique that a kind of use silk prepares uvioresistant antibiotic fabric | |
| CN105821660B (en) | A kind of modified silk fiber of highly hygroscopic moisture retention and preparation method thereof | |
| CN104294595A (en) | Production process for anti-bacterial deodorant textile | |
| CN110592938A (en) | Antibacterial modified silk fiber and preparation method thereof | |
| CN106012551A (en) | Preparation method for blended yarns of hemp cotton and antibacterial fibers | |
| CN108004762B (en) | Antibacterial silk product with nano-copper and preparation method thereof | |
| CN103243557B (en) | Oxidized sodium alginate modified textile fiber as well as preparation method and application thereof | |
| CN110409192B (en) | Nano carboxyl chitosan in-situ coating fabric and preparation method thereof | |
| CN107869048A (en) | A kind of antibacterial modified natural fiber of functional polysaccharide and preparation method thereof | |
| CN109680480A (en) | A kind of preparation method of health uvioresistant silk fabric | |
| CN105239380A (en) | Antibacterial mildew-resistant textile and preparation method thereof | |
| CN113089151A (en) | Three-dimensional antibacterial yarn containing cotton fibers, preparation method of three-dimensional antibacterial yarn and towel product | |
| JP2004131647A (en) | Composite of silk protein with chitosan and method for producing the same | |
| CN113308893A (en) | Weather-resistant antibacterial fabric and preparation method thereof | |
| CN112458595A (en) | Antibacterial health-care and anti-ultraviolet environment-friendly composite fabric and production device thereof | |
| CN113152082A (en) | Antibacterial home textile fabric containing sesbania fibers and preparation method thereof | |
| CN113151925A (en) | Polyquaternary ammonium salt/aloe antibacterial fiber, preparation method thereof and application thereof in antibacterial towels | |
| KR101125253B1 (en) | Skin-core fiber comprising anionic polymer salt and cellulose, and method for manufacturing the same | |
| CN104562262A (en) | Antistatic textile fiber material and preparation method thereof | |
| JP2011017108A (en) | Treatment agent for textile, method for producing antibacterial/antifungal textile product, and the resultant antibacterial/antifungal textile product | |
| CN115613359A (en) | Antibacterial protein modified viscose fiber and manufacturing process thereof | |
| CN110761073A (en) | Antibacterial fabric | |
| CN107338651A (en) | A kind of technique that highly hygroscopic moisturizing stretch-proof fabric is prepared using silk | |
| CN112127153A (en) | Antibacterial and deodorant textile and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171201 |