CN106012070A - Novel slow-release antibacterial cellulose fibers and preparation method thereof - Google Patents
Novel slow-release antibacterial cellulose fibers and preparation method thereof Download PDFInfo
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- CN106012070A CN106012070A CN201610531060.5A CN201610531060A CN106012070A CN 106012070 A CN106012070 A CN 106012070A CN 201610531060 A CN201610531060 A CN 201610531060A CN 106012070 A CN106012070 A CN 106012070A
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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
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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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- Artificial Filaments (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention discloses novel slow-release antibacterial cellulose fibers and a preparation method thereof. At present, high reaction temperature, long reaction time and cumbersome operation steps are needed for the preparation process of a cellulose and nano ZnO antibacterial composite material; in addition, for the cellulose and nano ZnO composite material prepared through a traditional method, nano ZnO is mainly distributed outside a cellulose substrate, so that the composite material is not durable in washing and short in duration time of the antibacterial effect. According to the novel slow-release antibacterial cellulose fibers and the preparation method thereof, the cellulose and ZnO composite fibers are prepared in one step through wet spinning by means of interaction of hydrogen-bond interfaces in the solution and condensed state conversion process, wherein ZnO nanoparticles are distributed on the surface and interior of the cellulose substrate, the slow-release effect is achieved, and a lasting antibacterial effect can be achieved.
Description
Invention field
The present invention relates to a kind of new sustained release anti-bacterial fibre cellulose fiber and preparation method thereof, belong to biological material
Field.
Technical background
ZnO is a kind of important multifunctional semiconductor material, and energy gap is 3.37eV, exciton bundle under room temperature
Tie up and can be up to 60meV.Wherein nano-ZnO possesses its skin effect not available for body lump material, little
Dimensional effect and macro quanta tunnel effect etc..Such as: buergerite ZnO nanocrystal has dissymmetrical structure,
Pressurized can occur dipole to separate, and shows piezoelectric property;Meanwhile, crystal grain defect the band structure caused
Change makes it to C2H2、CO、CH3The gases such as OH all show the gas-sensitive property of excellence;Particularly, nanometer
Metal ion and living radical that ZnO discharges can efficiently be killed and bacteria removal, have and significantly press down
Bacterium effect.In recent years, nano ZnO particles is carried on suitable high-molecular matrix material and becomes complex function material
The study hotspot in material field, its three dimensional structure that can give inorganic nano-particle macroscopic view and pliability, to enter
One step widens its range of application.
Cellulose is the renewable plant resources that nature is the abundantest, due to response function and the molecule of its uniqueness
Characteristic is expected to become following main industrial chemicals.But, cellulose has the strongest hydrogen bond and closely piles up
Crystal structure, it is difficult to melted and dissolve processing.At present, tModified Cellulose Fibers element film, fiber and nothing
Spin the products such as cloth mainly to be prepared by viscose process, there is stable chemical nature, bio-compatible, intensity height
Etc. characteristic, they packing, separate, the industrial circle such as weaving is all widely used.But, functional difference
Become the bottleneck problem of cellulosic material development.Cellulose and function nano particle composite quilt are proved a kind of
Important cellulose modified means.Recently, preparation and the performance study of cellulose/ZnO composite causes people
Extensive concern, but limited by cellulose dissolution difficulty, current its preparation method includes: 1) machinery is altogether
Mixed method, as Alejandro etc. uses mixing-pressure rolling equipment (750MPa) under elevated pressure conditions by cellulose
Pulp and ZnO powder are simply mixed and prepare cellulose/ZnO thin slice, and wherein the content of ZnO is
1.21~2.28wt%, and there is certain anti-microbial property.But, direct blending prepares cellulose/ZnO
Composite is higher to the requirement of equipment, is unfavorable for that extension produces.2) chemical method, the method is mainly passed through
Cellulose matrix is dipped in zinc salt precursor solution immersion, then obtains through sol-gel, mainly include water
Full-boiled process and solvent thermal two kinds, both need higher reaction temperature (90~150 DEG C) and longer response time
(3~20h);Meanwhile, cellulose matrix need to repeatedly immerse precursor solution and carries out depositing to improve composite wood
The content of nano-ZnO in material.3) Electrospinning Method, prepares acetic acid by cellulose is performed the derivatization modification
Cellulose, is then together dissolved in organic solvent by itself and presoma zinc salt and carries out electrospinning, the nanometer material after electrospinning
Material finally prepares cellulose/ZnO nano hybridized film through washing, high-temperature process, but prepared by Electrospinning Method
The composite materials property obtained has much room for improvement.Additionally, cellulose/ZnO that said method prepares is multiple
Condensation material, nano-ZnO is mainly distributed on the outside of cellulose matrix, during as anti-biotic material, exists and is weak to
Washing and the short disadvantage of antibacterial time.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, it is proposed that a kind of new sustained release anti-bacterial fibre cellulose fiber and system thereof
Preparation Method.
The present invention provides a kind of new sustained release anti-bacterial fibre cellulose fiber and preparation method thereof.Utilize solution-condensed state
Hydrogen bond interfacial interaction wet spinning one-step method in transition process prepares cellulose/ZnO composite fibre, its
Middle ZnO nanoparticle is distributed in surface and the inside of cellulose matrix, has slow release effect, and it is permanent to play
Antibacterial action.
The preparation method of a kind of new sustained release anti-bacterial fibre cellulose fiber, wherein ZnO nanoparticle is distributed in fiber
The surface of cellulose fiber substrate and inside, its preparation method comprises the following steps:
Step one: zinc oxide, sodium hydroxide, carbamide are sequentially added in water and make them dissolve, is subsequently placed in
Low temperature environment is refrigerated to-13~-15 DEG C;Wherein oxidation zinc concentration is 0.4-2.0wt%;Sodium hydroxide
Concentration is 6-7.5wt%;The concentration of carbamide is 10-13wt%
Step 2: in the aqueous systems of the pre-cooling that comminuted fibres element raw material is dipped in step one, 9000~12000
Rev/min high-speed stirred makes cellulosic material dispersed wherein, obtains cellulose dispersion liquid;
Step 3: cellulose dispersion liquid vacuum defoamation step 2 obtained is for use as spinning solution, compressed
Air is suppressed, dosing pump is squeezed in coagulating bath solidification;Finally it is dried to obtain novel cellulose/nano-ZnO
Composite fibre;Wherein coagulating bath includes the first coagulating bath and the second gelation, and ethylene glycol is the first coagulating bath,
Water is the second gelation.
In step 2, pulverized fiber raw material used is lamellar, and its length or a diameter of 0.5~5mm, thickness is
0.5~2mm, cellulosic material needed to be cooled to-7~15 DEG C before immersing the aqueous systems of pre-cooling.
The temperature of the first described coagulating bath ethylene glycol is 15~25 DEG C, and setting time is 2~5 seconds;Second coagulates
Gu the temperature of bath water is 30~70 DEG C, setting time is 3~10 seconds.
A kind of new sustained release anti-bacterial fibre cellulose fiber, a diameter of 15~30 μm of fiber, the content of ZnO is 5~20
Wt%;Wherein 50~70% nano-ZnO be distributed in the surface of fiber, spreading depth is 0.5~5 μm, averagely
Particle diameter is 100~220 nanometers;30~50% nano-ZnO be distributed in the inside of cellulose fiber substrate, its
Mean diameter is 30~120 nanometers.
The most relatively, use technical solution of the present invention to have marked improvement, and beneficial effect can be obtained:
The present invention is with cellulose-NaOH/ carbamide/zinc oxide aqueous solution as spinning solution, by solution-condensed state
Hydrogen bond interfacial interaction one-step method in transition process builds and obtains cellulose/ZnO composite fibre;With public
The research work opening report is compared, and this method mild condition, preparation process are simple, it is simple to industrializing implementation.
In the cellulose that the present invention prepares/ZnO composite fibre, ZnO is distributed in inside and the surface of fiber, has
Sustained-release antibacterial and wash resistant characteristic.
Accompanying drawing explanation
Fig. 1 is the surface picture of a kind of new sustained release anti-bacterial fibre cellulose fiber;
Fig. 2 is the cross-section photograph of a kind of new sustained release anti-bacterial fibre cellulose fiber.
Specific implementation method
Below in conjunction with specific embodiment, technical scheme is illustrated further.
Embodiment 1
First zinc oxide, sodium hydroxide, carbamide are sequentially added in water and make them dissolve, wherein zinc oxide,
Sodium hydroxide, urea concentration are respectively 0.4wt%, 7wt%, 11wt%, are subsequently placed in low temperature environment cold
Freeze to-13 DEG C;Simultaneously by cellulosic material powder slabbing, its a diameter of 0.5mm, thickness is 0.5mm,
And it is cooled to-7 DEG C in advance;Then the comminuted fibres element raw material of pre-cooling is immersed in the aqueous systems of pre-cooling, 9000 turns
/ point high-speed stirred makes cellulose dispersed wherein;Finally by cellulose dispersion liquid vacuum defoamation for use as spinning
Stock solution, compressed air is suppressed, dosing pump is squeezed in coagulating bath solidification;Wherein ethylene glycol be first coagulate
Gu bath, temperature is 15 DEG C, and setting time is 2 seconds;Water is the second gelation, and temperature is 30 DEG C, solidification
Time is 3 seconds;Finally it is dried to obtain novel cellulose/nano-ZnO composite fibre, as shown in Figure 1 and Figure 2;
A diameter of 15 μm of composite fibre, the content of ZnO is 5wt%;Wherein the nano-ZnO of 50% is distributed in
The surface of composite fibre, spreading depth is 0.5 μm, and mean diameter is 100 nanometers;The nano-ZnO of 50%
Being distributed in the inside of cellulose fiber substrate, its mean diameter is 30 nanometers;In 3 hours, composite fibre is to greatly
The killing rate of enterobacteria and staphylococcus aureus is 100%, and after 30 days, above two antibacterial is killed by it
Rate still reaches 90% and 92%;Live through in latter 3 hours of 10 washings to the killing rate of above two antibacterial still
Reach 88% and 90%.
Embodiment 2
First 2.0wt% zinc oxide, 7.5wt% sodium hydroxide, 10wt% carbamide are sequentially added in water and make it
Dissolve, be subsequently placed in low temperature environment and be refrigerated to-15 DEG C;Simultaneously by cellulosic material powder slabbing, its
A diameter of 5mm, thickness is 2mm, and is cooled to 15 DEG C in advance;Then by the comminuted fibres element raw material of pre-cooling
Immersing in the aqueous systems of pre-cooling, 10000 revs/min of high-speed stirred make cellulose dispersed wherein;Finally by fibre
Dimension element dispersion liquid vacuum defoamation is for use as spinning solution, and compressed air is suppressed, dosing pump is squeezed into solidification
Bath solidifies;Wherein ethylene glycol is the first coagulating bath, and temperature is 25 DEG C, and setting time is 5 seconds;Water is
The second gelation, temperature is 70 DEG C, and setting time is 10 seconds;Finally it is dried to obtain novel cellulose/receive
Rice ZnO composite fibre;A diameter of 30 μm of composite fibre, the content of ZnO is 20wt%;Wherein 70%
Nano-ZnO be distributed in the surface of composite fibre, spreading depth is 5 μm, and mean diameter is 220 nanometers;
The nano-ZnO of 30% is distributed in the inside of cellulose fiber substrate, and its mean diameter is 120 nanometers;3 is little
Time interior composite fibre the killing rate of escherichia coli and staphylococcus aureus is 98%, after 30 days, it is to upper
The killing rate stating two kinds of antibacterials still reaches 89% and 90%;Live through 10 times in washing latter 3 hours above-mentioned two
The killing rate planting antibacterial still reaches 82% and 87%.
Embodiment 3
First 1.0wt% zinc oxide, 7wt% sodium hydroxide, 13wt% carbamide are sequentially added in water and make them
Dissolve, be subsequently placed in low temperature environment and be refrigerated to-14 DEG C;Simultaneously by cellulosic material powder slabbing, it is straight
Footpath is 3mm, and thickness is 1mm, and is cooled to 10 DEG C in advance;Then the comminuted fibres element raw material of pre-cooling is soaked
Entering in the aqueous systems of pre-cooling, 12000 revs/min of high-speed stirred make cellulose dispersed wherein;Finally by fiber
Element dispersion liquid vacuum defoamation is for use as spinning solution, and compressed air is suppressed, dosing pump is squeezed into coagulating bath
Middle solidification;Wherein ethylene glycol is the first coagulating bath, and temperature is 20 DEG C, and setting time is 3 seconds;Water is
Two coagulating baths, temperature is 50 DEG C, and setting time is 7 seconds;Finally it is dried to obtain novel cellulose/nano-ZnO
Composite fibre;A diameter of 20 μm of composite fibre, the content of ZnO is 10wt%;The wherein nanometer of 60%
ZnO is distributed in the surface of composite fibre, and spreading depth is 2.5 μm, and mean diameter is 150 nanometers;40%
Nano-ZnO be distributed in the inside of cellulose fiber substrate, its mean diameter is 80 nanometers;In 3 hours again
Condensating fiber is 100% to the killing rate of escherichia coli and staphylococcus aureus, and after 30 days, it is to above two
The killing rate of antibacterial still reaches 93% and 95%;Live through 10 times in washing latter 3 hours above two antibacterial
Killing rate still reach 88% and 90%
Embodiment 4
First 0.8wt% zinc oxide, 6wt% sodium hydroxide, 12wt% carbamide are sequentially added in water and make them
Dissolve, be subsequently placed in low temperature environment and be refrigerated to-14 DEG C;Simultaneously by cellulosic material powder slabbing, it is straight
Footpath is 2.0mm, and thickness is 0.8mm, and is cooled to 0 DEG C in advance;Then by former for the comminuted fibres element of pre-cooling
Material immerses in the aqueous systems of pre-cooling, and 11000 revs/min of high-speed stirred make cellulose dispersed wherein;Finally will
Cellulose dispersion liquid vacuum defoamation is for use as spinning solution, and compressed air is suppressed, dosing pump is squeezed into coagulating
Gu solidify in Yu;Wherein ethylene glycol is the first coagulating bath, and temperature is 18 DEG C, and setting time is 3 seconds;Water
For the second gelation, temperature is 40 DEG C, and setting time is 5 seconds;Finally it is dried to obtain novel cellulose/receive
Rice ZnO composite fibre;A diameter of 20 μm of composite fibre, the content of ZnO is 10wt%;Wherein 55%
Nano-ZnO be distributed in the surface of composite fibre, spreading depth is 1.5 μm, and mean diameter is 130 to receive
Rice;The nano-ZnO of 45% is distributed in the inside of cellulose fiber substrate, and its mean diameter is 35 nanometers;3
In hour, composite fibre is 100% to the killing rate of escherichia coli and staphylococcus aureus, and after 30 days, it is right
The killing rate of above two antibacterial still reaches 87% and 89%;Live through 10 times in washing latter 3 hours above-mentioned
The killing rate of two kinds of antibacterials still reaches 82% and 85%.
Embodiment 5
First 1.8wt% zinc oxide, 6wt% sodium hydroxide, 10wt% carbamide are sequentially added in water and make them
Dissolve, be subsequently placed in low temperature environment and be refrigerated to-14 DEG C;Simultaneously by cellulosic material powder slabbing, it is straight
Footpath is 3.5mm, and thickness is 1.5mm, and is cooled to 13 DEG C in advance;Then by former for the comminuted fibres element of pre-cooling
Material immerses in the aqueous systems of pre-cooling, and 9000 revs/min of high-speed stirred make cellulose dispersed wherein;Finally will
Cellulose dispersion liquid vacuum defoamation is for use as spinning solution, and compressed air is suppressed, dosing pump is squeezed into coagulating
Gu solidify in Yu;Wherein ethylene glycol is the first coagulating bath, and temperature is 23 DEG C, and setting time is 4.5 seconds;
Water is the second gelation, and temperature is 55 DEG C, and setting time is 8 seconds;Finally be dried to obtain novel cellulose/
Nano-ZnO composite fibre;A diameter of 25 μm of composite fibre, the content of ZnO is 17wt%;Wherein 60%
Nano-ZnO be distributed in the surface of composite fibre, spreading depth is 4.5 μm, and mean diameter is 100 to receive
Rice;The nano-ZnO of 50% is distributed in the inside of cellulose fiber substrate, and its mean diameter is 180 nanometers;
In 3 hours, composite fibre is 100% to the killing rate of escherichia coli and staphylococcus aureus, after 30 days its
The killing rate of above two antibacterial is still reached 94% and 96%;Live through 10 times in washing latter 3 hours upper
The killing rate stating two kinds of antibacterials still reaches 90% and 88%.
Claims (4)
1. the preparation method of a new sustained release anti-bacterial fibre cellulose fiber, it is characterised in that:
Step one: zinc oxide, sodium hydroxide, carbamide are sequentially added in water and make them dissolve, so
It is placed in low temperature environment and is refrigerated to-13~-15 DEG C;Wherein oxidation zinc concentration is 0.4-2.0wt%;
The concentration of sodium hydroxide is 6-7.5wt%;The concentration of carbamide is 10-13wt%;
Step 2: in the aqueous systems of the pre-cooling that comminuted fibres element raw material is dipped in step one,
9000~12000 revs/min of high-speed stirred make cellulosic material dispersed wherein, obtain cellulose and divide
Dissipate liquid;
Step 3: the cellulose dispersion liquid vacuum defoamation that step 2 is obtained for use as spinning solution,
Compressed air is suppressed, dosing pump is squeezed in coagulating bath solidification;Finally it is dried to obtain novel fibre
Dimension element/nano-ZnO composite fibre;Wherein coagulating bath includes the first coagulating bath and the second gelation,
Ethylene glycol is the first coagulating bath, and water is the second gelation.
The preparation side of a kind of new sustained release anti-bacterial fibre cellulose fiber the most according to claim 1
Method, it is characterised in that: in step 2, pulverized fiber raw material used is lamellar, its length or diameter
Being 0.5~5mm, thickness is 0.5~2mm, and cellulosic material needed before immersing the aqueous systems of pre-cooling
It is cooled to-7~15 DEG C.
The preparation side of a kind of new sustained release anti-bacterial fibre cellulose fiber the most according to claim 1
Method, it is characterised in that: the temperature of the first described coagulating bath ethylene glycol is 15~25 DEG C, during solidification
Between be 2~5 seconds;The temperature of the second gelation water is 30~70 DEG C, and setting time is 3~10 seconds.
4. a new sustained release anti-bacterial fibre cellulose fiber, it is characterised in that: fiber a diameter of
15~30 μm, the content of ZnO is 5~20wt%;Wherein 50~70% nano-ZnO be distributed in fibre
The surface of dimension, spreading depth is 0.5~5 μm, and mean diameter is 100~220 nanometers;30~50%
Nano-ZnO be distributed in the inside of cellulose fiber substrate, its mean diameter is 30~120 nanometers.
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Cited By (4)
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CN106894231A (en) * | 2017-02-27 | 2017-06-27 | 东华大学 | A kind of preparation method of the flax spinning material with air-cleaning function |
CN109023573A (en) * | 2018-07-06 | 2018-12-18 | 浙江理工大学 | A kind of systemic activity antibacterial cellulose composite fibre and preparation method thereof |
CN114574992A (en) * | 2022-04-01 | 2022-06-03 | 雅香丽化妆用品(深圳)有限公司 | Composite filament yarn containing bio-based material, preparation method thereof and toothbrush |
CN115161841A (en) * | 2022-08-15 | 2022-10-11 | 罗莱生活科技股份有限公司 | Zinc oxide modified fiber blended fabric and preparation method thereof |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106894231A (en) * | 2017-02-27 | 2017-06-27 | 东华大学 | A kind of preparation method of the flax spinning material with air-cleaning function |
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CN114574992A (en) * | 2022-04-01 | 2022-06-03 | 雅香丽化妆用品(深圳)有限公司 | Composite filament yarn containing bio-based material, preparation method thereof and toothbrush |
CN115161841A (en) * | 2022-08-15 | 2022-10-11 | 罗莱生活科技股份有限公司 | Zinc oxide modified fiber blended fabric and preparation method thereof |
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Application publication date: 20161012 |