CN106087092B - A kind of preparation method of antibacterial, ventilating functional fibre - Google Patents
A kind of preparation method of antibacterial, ventilating functional fibre Download PDFInfo
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- CN106087092B CN106087092B CN201610682052.0A CN201610682052A CN106087092B CN 106087092 B CN106087092 B CN 106087092B CN 201610682052 A CN201610682052 A CN 201610682052A CN 106087092 B CN106087092 B CN 106087092B
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- antibacterial
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
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- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Artificial Filaments (AREA)
Abstract
The present invention relates to textile material field, discloses a kind of preparation method of antibacterial, ventilating functional fibre, carries out according to the following steps:Step 1:Carry the preparation of silver-colored γ cyclodextrin;Step 2:The preparation of cellulose fibroin titanium dioxide xerogel particles;Step 3:The preparation of antibacterial, ventilating master batch;Step 4:Spinning.Antibacterial, ventilating functional fibre produced by the present invention has sustained-release antibacterial effect, timeliness length;And the compliance and comfortableness of fiber are not interfered with, fibre strength is also strengthened in addition.
Description
Technical field
The present invention relates to textile material field, more particularly to a kind of preparation method of antibacterial, ventilating functional fibre.
Background technology
With the increasingly raising of people's living standard, requirement of the people for dress also improves constantly.Nowadays people for
Dress ornament is not only particular about style, and the functional requirements also more and more higher of the fabric for dress ornament.
Especially in terms of health, in life, people inevitably touch various bacteriums, fungi etc.
Microorganism, these microorganisms are spread disease, so as to influence the body of people under suitable external condition by modes such as contacts
Health and normal work, studying and living.In addition, the gas permeability of textile material is also critically important for health, if spun
The poor air permeability of material is knitted, the moisture of skin surface can be caused can not exclude in time, so as to trigger various diseases.
Reach antibacterial functions, current common practice is the practical dressing liquid with antibacterial functions to entering to textile material
Row dipping, makes antimicrobial component be attached to textile material surface, so that textile material has antibiotic property.But way so
The comfortableness of textile material can be had a strong impact on, textile material feel can be partially hard, and gas permeability degradation.In addition, antimicrobial component
Textile material surface is attached to, its fastness is relatively low, not water-fastness, is easily lost in, poor in timeliness.
The content of the invention
In order to solve the above-mentioned technical problem, the invention provides a kind of preparation method of antibacterial, ventilating functional fibre.This hair
Bright obtained antibacterial, ventilating functional fibre has sustained-release antibacterial effect, timeliness length;And the compliance of fiber and comfortable is not interfered with
Property, fibre strength is also strengthened in addition.
The present invention concrete technical scheme be:A kind of preparation method of antibacterial, ventilating functional fibre, is carried out according to the following steps:
Step 1:Gamma-cyclodextrin is formulated as the gamma-cyclodextrin solution that mass concentration is 4-6%, to gamma-cyclodextrin solution
Middle addition quality is the silver nitrate of 0.3-0.5 times of gamma-cyclodextrin, after stirring, solution ph is controlled in 4-6, in lucifuge
Under the conditions of, it is heated to 50-60 DEG C and is incubated 2-3h, be then centrifuged for isolated solid, solid is cleaned, after drying, be dissolved in hydrogen
In sodium hydroxide solution, the sodium borohydride that quality is solid 0.5-1.5% is added into sodium hydroxide solution, adjusts pH to 7-8, so
After be stirred, be made after centrifuging and drying again and carry silver-colored gamma-cyclodextrin.
Step 2:By cellulose, fibroin albumen be formulated as cellulose mass concentration be 2-4%, fibroin albumen quality concentration be
1-3% mixed solution, mixed solution quality 0.5-1.5% load silver gamma-cyclodextrin is successively added into mixed solution and is mixed
Solution quality 0.1-0.3% ethylene glycol diglycidylether is closed, mixed sols is made after being uniformly dispersed, by mixed sols and two
Titanium oxide hydrosol 4-6 in mass ratio:1 mixing, is transferred in -10 DEG C to -6 DEG C of environment after stirring and freezes 2-3 days, ice
Thawed after jelly, cellulose-fibroin-titanium dioxide hydrogel is made;With ethanol to cellulose-fibroin-titanium dioxide water-setting
After glue carries out solvent displacement for several times, cellulose-fibroin-titanium dioxide alcogel is made;To cellulose-fibroin-titanium dioxide alcohol
Gel carries out supercritical fluid drying, eventually passes through grinding and cellulose-fibroin-titanium dioxide xerogel particles are made.
Step 3:Cellulose-fibroin-titanium dioxide xerogel particles are prepared in the dispersion liquid that mass concentration is 3-5%,
Add acrylic acid, polyethylene glycol and ammonium persulfate respectively into dispersion liquid, react 2-4h under 55-65 DEG C of stirring condition;Its
Middle cellulose-fibroin-titanium dioxide xerogel particles, acrylic acid, polyethylene glycol and ammonium persulfate mass ratio are 1:0.3-0.4:
0.3-0.4:0.02-0.03;Natural cooling after reaction, when reactant is in mucus shape, mucus is dried in vacuo, and carry out powder
It is broken, antibacterial, ventilating master batch is made.
Step 4:Antibacterial, ventilating master batch is mixed with viscose rayon spinning solution, melt spinning is carried out by spinning-drawing machine, is made
Antibacterial, ventilating functional fibre.
Step 1 of the present invention carries out carrying silver using the complexing power of cyclodextrin, is made and carries silver-colored gamma-cyclodextrin, so as to anti-
Bacterium function;Step 2 cellulose, fibroin albumen, the obtained cellulose-fibroin-titanium dioxide xerogel particles of silver-colored gamma-cyclodextrin are carried,
With extra specific surface area and three-dimensional open-framework, there is good gas permeability, and from cellulose, fibroin albumen as main
Material, can lift the tensile strength of fiber, and titanium dioxide also has outstanding antibiotic property and anti-light 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 3 is by cellulose-fibroin-titanium dioxide
Titanium xerogel particles and acrylic acid, the compound obtained antibacterial, ventilating master batch of polyethylene glycol, the antibacterial, ventilating master batch is in spinning solution
Good dispersion.Step 4 is by antibacterial, ventilating master batch and the common spinning of rayon spinning liquid.Because viscose rayon main component is alpha fibre
Element, and also contain cellulose in cellulose-fibroin-titanium dioxide xerogel particles, therefore compatibility, good dispersion, with reference to jail
Degree is high.
Further, the particle diameter of the cellulose-fibroin-titanium dioxide xerogel particles is less than or equal to 1 micron.
Further, the particle diameter of the antibacterial, ventilating master batch is 2-3 microns.
Further, the antibacterial, ventilating master batch and viscose rayon spinning solution 4-8 in mass ratio:92-96 is mixed.
It is compared with the prior art, the beneficial effects of the invention are as follows:Antibacterial, ventilating functional fibre produced by the present invention has slow
Release antibacterial effect, timeliness length;And the compliance and comfortableness of fiber are not interfered with, fibre strength is also strengthened in addition.
Embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
A kind of preparation method of antibacterial, ventilating functional fibre, is carried out according to the following steps:
Step 1:Gamma-cyclodextrin is formulated as the gamma-cyclodextrin solution that mass concentration is 5%, into gamma-cyclodextrin solution
The silver nitrate that quality is 0.4 times of gamma-cyclodextrin is added, after stirring, solution ph is controlled 5, under the conditions of lucifuge, added
Heat is to 55 DEG C and is incubated 2.5h, is then centrifuged for isolated solid, solid is cleaned, after drying, is dissolved in sodium hydroxide solution,
The sodium borohydride that quality is solid 1% is added into sodium hydroxide solution, pH to 7.5 is adjusted, is then stirred, centrifuges again
It is made after separating and drying and carries silver-colored gamma-cyclodextrin.
Step 2:By cellulose, fibroin albumen be formulated as cellulose mass concentration be 3%, fibroin albumen quality concentration be
2% mixed solution, the load silver gamma-cyclodextrin and mixed solution matter of mixed solution quality 1% are successively added into mixed solution
The ethylene glycol diglycidylether of amount 0.2%, mixed sols is made after being uniformly dispersed, by mixed sols and titania hydrosol
In mass ratio 5:1 mixing, is transferred in -8 DEG C of environment after stirring and freezes 2.5 days, thawed after frost, and fiber is made
Element-fibroin-titanium dioxide hydrogel;After solvent displacement for several times is carried out to cellulose-fibroin-titanium dioxide hydrogel with ethanol,
Cellulose-fibroin-titanium dioxide alcogel is made;Supercritical fluid is carried out to cellulose-fibroin-titanium dioxide alcogel
It is dry, eventually pass through grinding and cellulose-fibroin-titanium dioxide xerogel particles that particle diameter is less than or equal to 1 micron are made.
Step 3:Cellulose-fibroin-titanium dioxide xerogel particles are prepared in the dispersion liquid that mass concentration is 4%, to
Acrylic acid, polyethylene glycol and ammonium persulfate are added in dispersion liquid respectively, reacts 3h under 60 DEG C of stirring condition;Wherein fiber
Element-fibroin-titanium dioxide xerogel particles, acrylic acid, polyethylene glycol and ammonium persulfate mass ratio are 1:0.35:0.35:
0.025;Natural cooling after reaction, when reactant is in mucus shape, mucus is dried in vacuo, and crushed, obtained particle diameter is
The antibacterial, ventilating master batch of 2-3 microns.
Step 4:By antibacterial, ventilating master batch and viscose rayon spinning solution in mass ratio 6:94 mixing, are melted by spinning-drawing machine
Melt spinning, antibacterial, ventilating functional fibre is made.
Embodiment 2
A kind of preparation method of antibacterial, ventilating functional fibre, is carried out according to the following steps:
Step 1:Gamma-cyclodextrin is formulated as the gamma-cyclodextrin solution that mass concentration is 4%, into gamma-cyclodextrin solution
The silver nitrate that quality is 0.3 times of gamma-cyclodextrin is added, after stirring, solution ph is controlled 4, under the conditions of lucifuge, added
Heat is to 50 DEG C and is incubated 3h, is then centrifuged for isolated solid, solid is cleaned, after drying, is dissolved in sodium hydroxide solution, to
The sodium borohydride that quality is solid 0.5% is added in sodium hydroxide solution, pH to 7 is adjusted, is then stirred, again centrifugation point
From and be made after drying and carry silver-colored gamma-cyclodextrin.
Step 2:By cellulose, fibroin albumen be formulated as cellulose mass concentration be 2%, fibroin albumen quality concentration be
1% mixed solution, the load silver gamma-cyclodextrin and mixed solution of mixed solution quality 0.5% are successively added into mixed solution
The ethylene glycol diglycidylether of quality 0.1%, mixed sols is made after being uniformly dispersed, mixed sols is water-soluble with titanium dioxide
Glue in mass ratio 4:1 mixing, is transferred in -10 DEG C of environment after stirring and freezes 2 days, thawed after frost, and fibre is made
Tie up element-fibroin-titanium dioxide hydrogel;Solvent displacement for several times is carried out to cellulose-fibroin-titanium dioxide hydrogel with ethanol
Afterwards, cellulose-fibroin-titanium dioxide alcogel is made;Supercritical fluid is carried out to cellulose-fibroin-titanium dioxide alcogel
Dry, eventually pass through grinding and cellulose-fibroin-titanium dioxide xerogel particles that particle diameter is less than or equal to 1 micron are made.
Step 3:Cellulose-fibroin-titanium dioxide xerogel particles are prepared in the dispersion liquid that mass concentration is 3%, to
Acrylic acid, polyethylene glycol and ammonium persulfate are added in dispersion liquid respectively, reacts 4h under 55 DEG C of stirring condition;Wherein fiber
Element-fibroin-titanium dioxide xerogel particles, acrylic acid, polyethylene glycol and ammonium persulfate mass ratio are 1:0.3:0.3:0.02;Instead
Natural cooling after answering, when reactant is in mucus shape, mucus is dried in vacuo, and crushed, particle diameter is made as 2-3 microns
Antibacterial, ventilating master batch.
Step 4:By antibacterial, ventilating master batch and viscose rayon spinning solution in mass ratio 4:96 mixing, are melted by spinning-drawing machine
Melt spinning, antibacterial, ventilating functional fibre is made.
Embodiment 3
A kind of preparation method of antibacterial, ventilating functional fibre, is carried out according to the following steps:
Step 1:Gamma-cyclodextrin is formulated as the gamma-cyclodextrin solution that mass concentration is 6%, into gamma-cyclodextrin solution
The silver nitrate that quality is 0.5 times of gamma-cyclodextrin is added, after stirring, solution ph is controlled 6, under the conditions of lucifuge, added
Heat is to 60 DEG C and is incubated 2h, is then centrifuged for isolated solid, solid is cleaned, after drying, is dissolved in sodium hydroxide solution, to
The sodium borohydride that quality is solid 1.5% is added in sodium hydroxide solution, pH to 8 is adjusted, is then stirred, again centrifugation point
From and be made after drying and carry silver-colored gamma-cyclodextrin.
Step 2:By cellulose, fibroin albumen be formulated as cellulose mass concentration be 4%, fibroin albumen quality concentration be
3% mixed solution, the load silver gamma-cyclodextrin and mixed solution of mixed solution quality 1.5% are successively added into mixed solution
The ethylene glycol diglycidylether of quality 0.3%, mixed sols is made after being uniformly dispersed, mixed sols is water-soluble with titanium dioxide
Glue in mass ratio 6:1 mixing, is transferred in -6 DEG C of environment after stirring and freezes 3 days, thawed after frost, and fiber is made
Element-fibroin-titanium dioxide hydrogel;After solvent displacement for several times is carried out to cellulose-fibroin-titanium dioxide hydrogel with ethanol,
Cellulose-fibroin-titanium dioxide alcogel is made;Supercritical fluid is carried out to cellulose-fibroin-titanium dioxide alcogel
It is dry, eventually pass through grinding and cellulose-fibroin-titanium dioxide xerogel particles that particle diameter is less than or equal to 1 micron are made.
Step 3:Cellulose-fibroin-titanium dioxide xerogel particles are prepared in the dispersion liquid that mass concentration is 5%, to
Acrylic acid, polyethylene glycol and ammonium persulfate are added in dispersion liquid respectively, reacts 2h under 65 DEG C of stirring condition;Wherein fiber
Element-fibroin-titanium dioxide xerogel particles, acrylic acid, polyethylene glycol and ammonium persulfate mass ratio are 1:0.4:0.4:0.03;Instead
Natural cooling after answering, when reactant is in mucus shape, mucus is dried in vacuo, and crushed, particle diameter is made as 2-3 microns
Antibacterial, ventilating master batch.
Step 4:By antibacterial, ventilating master batch and viscose rayon spinning solution in mass ratio 8:92 mixing, are melted by spinning-drawing machine
Melt spinning, antibacterial, ventilating functional fibre is made.
Raw materials used in the present invention, equipment, it is the conventional raw material, equipment of this area unless otherwise noted;In the present invention
Method therefor, it is the conventional method of this area unless otherwise noted.
It is described above, only it is presently preferred embodiments of the present invention, not the present invention is imposed any restrictions, it is every according to the present invention
Any simple modification, change and the equivalent transformation that technical spirit is made to above example, still fall within the technology of the present invention side
The protection domain of case.
Claims (4)
1. a kind of preparation method of antibacterial, ventilating functional fibre, it is characterised in that carry out according to the following steps:
Step 1:Gamma-cyclodextrin is formulated as the gamma-cyclodextrin solution that mass concentration is 4-6%, added into gamma-cyclodextrin solution
Add the silver nitrate that quality is 0.3-0.5 times of gamma-cyclodextrin, after stirring, solution ph is controlled in 4-6, in lucifuge condition
Under, it is heated to 50-60 DEG C and is incubated 2-3h, be then centrifuged for isolated solid, solid is cleaned, after drying, be dissolved in hydroxide
In sodium solution, the sodium borohydride that quality is solid 0.5-1.5% is added into sodium hydroxide solution, adjusts pH to 7-8, Ran Houjin
Row stirring, it is made after centrifuging and dry again and carries silver-colored gamma-cyclodextrin;
Step 2:By cellulose, fibroin albumen be formulated as cellulose mass concentration be 2-4%, fibroin albumen quality concentration be 1-
3% mixed solution, mixed solution quality 0.5-1.5% load silver gamma-cyclodextrin and mixing are successively added into mixed solution
Solution quality 0.1-0.3% ethylene glycol diglycidylether, mixed sols is made after being uniformly dispersed, by mixed sols and dioxy
Change titanium hydrosol 4-6 in mass ratio:1 mixing, is transferred in -10 DEG C to -6 DEG C of environment after stirring and freezes 2-3 days, freezes
After thawed, be made cellulose-fibroin-titanium dioxide hydrogel;With ethanol to cellulose-fibroin-titanium dioxide hydrogel
After carrying out solvent displacement for several times, cellulose-fibroin-titanium dioxide alcogel is made;Cellulose-fibroin-titanium dioxide alcohol is coagulated
Glue carries out supercritical fluid drying, eventually passes through grinding and cellulose-fibroin-titanium dioxide xerogel particles are made;
Step 3:Cellulose-fibroin-titanium dioxide xerogel particles is prepared in the dispersion liquid that mass concentration is 3-5%, to point
Acrylic acid, polyethylene glycol and ammonium persulfate are added in dispersion liquid respectively, reacts 2-4h under 55-65 DEG C of stirring condition;It is wherein fine
It is 1 to tie up element-fibroin-titanium dioxide xerogel particles, acrylic acid, polyethylene glycol and ammonium persulfate mass ratio:0.3-0.4:0.3-
0.4:0.02-0.03;Natural cooling after reaction, when reactant is in mucus shape, mucus is dried in vacuo, and crushed, made
Obtain antibacterial, ventilating master batch;
Step 4:Antibacterial, ventilating master batch is mixed with viscose rayon spinning solution, melt spinning is carried out by spinning-drawing machine, antibacterial is made
Airing function fiber.
A kind of 2. preparation method of antibacterial, ventilating functional fibre as claimed in claim 1, it is characterised in that the cellulose-
The particle diameter of fibroin-titanium dioxide xerogel particles is less than or equal to 1 micron.
A kind of 3. preparation method of antibacterial, ventilating functional fibre as claimed in claim 1 or 2, it is characterised in that the antibacterial
The particle diameter of air-permeable masterbatch is 2-3 microns.
A kind of 4. preparation method of antibacterial, ventilating functional fibre as claimed in claim 1 or 2, it is characterised in that the antibacterial
Air-permeable masterbatch and viscose rayon spinning solution 4-8 in mass ratio:92-96 is mixed.
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CN106948021A (en) * | 2017-05-04 | 2017-07-14 | 冯志容 | A kind of preparation method of Multifunctional silk fiber |
CN107501961A (en) * | 2017-09-17 | 2017-12-22 | 钱景 | Titanium dioxide/Nano Silver/silk magnetic porous composite material and preparation method thereof |
CN108149485A (en) * | 2017-12-13 | 2018-06-12 | 天津宝兴威科技股份有限公司 | A kind of preparation method of beta-cyclodextrin nano silver antibacterial fabric |
CN111286870A (en) * | 2020-02-28 | 2020-06-16 | 山东省农业科学院农产品研究所 | Preparation method of degradable nanofiber antibacterial preservative film |
CN112011282B (en) * | 2020-08-17 | 2021-06-29 | 深圳市方胜光学材料科技有限公司 | 3D protective film and preparation process thereof |
CN114849655A (en) * | 2022-03-17 | 2022-08-05 | 安徽农业大学 | Water-insoluble cyclodextrin polymer-based antibacterial microsphere material and preparation method thereof |
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