CN109023573A - A kind of systemic activity antibacterial cellulose composite fibre and preparation method thereof - Google Patents
A kind of systemic activity antibacterial cellulose composite fibre and preparation method thereof Download PDFInfo
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- CN109023573A CN109023573A CN201810737890.2A CN201810737890A CN109023573A CN 109023573 A CN109023573 A CN 109023573A CN 201810737890 A CN201810737890 A CN 201810737890A CN 109023573 A CN109023573 A CN 109023573A
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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
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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
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/02—Chemical after-treatment of artificial filaments or the like during manufacture of cellulose, cellulose derivatives, or proteins
Abstract
The invention discloses a kind of systemic activity antibacterial cellulose composite fibres and preparation method thereof；Cellulose base silver/graphene oxide/zinc oxide composite fibre is using porous cellulose as bracket, and nano zine oxide and graphene oxide are distributed in cellulose matrix, and nano silver is coated on surface of nanometer zinc oxide.The present invention is ingenious to be dissolved into zinc oxide in cellulose using one step of biomineralization, add graphene oxide, utilize cellulose/zinc oxide reproducibility, cellulose base graphene oxide/burnett's solution is made, fiber is prepared by wet spinning technology, and fiber is made to immerse certain density silver nitrate solution, with daylight light irradiation, it is coated to nano silver on fiber, forms last cellulose silver/graphene oxide/zinc oxide composite fibre.This method is simple, environmentally protective, and obtained composite fibre has excellent anti-microbial property.
Description
Technical field
The present invention relates to a kind of systemic activity antibacterial cellulose composite fibres and preparation method thereof, belong to composite material neck
Domain.
Background technique
Cellulose is the most abundant renewable resource of nature, environmentally friendly, the development of bio-compatible and functional material
It plays an important role, since its unique response function and molecular characterization are expected to become the following main industrial chemicals.However function
Property difference become the bottleneck problem of cellulosic material development, be proved to be a kind of important for cellulose and function nano particle are compound
Cellulose modified means.It is limited however, being insoluble in common solvent by cellulose, prepares cellulose based nano composite wood at present
The method of material includes: 1) mechanical blending method, such as Alejandro using mixing-pressure rolling equipment under high pressure (750MPa)
Cellulose pulp and Zinc oxide powder are simply mixed, cellulose/zinc oxide thin slice is prepared.However, prepared by direct blending
Cellulose/zinc oxide composite is unfavorable for expanded production to the more demanding of equipment；2) chemical method, this method are mainly led to
It crosses for cellulose matrix to be dipped in the precursor solution of inorganic nano-particle and impregnate, then obtained through sol-gel, mainly include
Hydro-thermal method and two kinds of solvent heat, both need higher reaction temperature (90~150 DEG C) and longer reaction time (3~20h)；
3) Electrospinning Method, by performing the derivatization the modified cellulose derivative that solubility property is prepared and significantly improves to cellulose, so
It is dissolved in organic solvent together with inorganic nano-particle presoma afterwards and carries out electrospinning, the nano material after electrospinning by washing,
High-temperature process is finally prepared cellulose base inorganic nanometer particle compesite, however the composite material that Electrospinning Method is prepared
Mechanical property is to be improved.In addition, inorganic nano in the cellulose base inorganic nano-particle composite membrane that the above method is prepared
Particle is mainly distributed on the outside of cellulose matrix, and when being used as anti-biotic material, there are the short disadvantages of antibacterial time.
The problem to be solved in the present invention: although cellulose rich reserves and cheap, having a single function, and introduces inorganic receives
Rice corpuscles can solve this problem.Then, the cellulose base inorganic nanometer particle compesite preparation method reported is excessively
It is complicated, cumbersome, and nanoparticle is both dispersed in greatly the surface of fiber matrix material, and is easy to draw its reunion.
Summary of the invention
In view of the deficiencies of the prior art, the present invention proposes a kind of systemic activity antibacterial cellulose composite fibre and its preparations
Method: it is ingenious to utilize biomineralization, oxygen is prepared in situ from cellulose solution using the biomineralization of cellulose
Change zinc；In turn, it is by silver nitrate reduction under graphene oxide and illumination subsidiary conditions using the reducing end under neutral of cellulose
Silver is simultaneously introduced into composite fibre.
A kind of systemic activity antibacterial cellulose composite fibre, using porous cellulose as bracket, nano zine oxide and oxidation
Graphene is distributed in cellulose matrix, and nano silver is coated on surface of nanometer zinc oxide.
A kind of systemic activity antibacterial cellulose composite fibre and preparation method thereof, preparation method includes the following steps:
Step 1: zinc oxide, sodium hydroxide, urea, which are sequentially added, dissolves them in water, be subsequently placed in cold in low temperature environment
Freeze to -11~-15 DEG C；Wherein oxidation zinc concentration is 0.5-2.0wt%；The concentration of sodium hydroxide is 6.5-7.5wt%；Urea
Concentration be 11-13wt%；
Step 2: in the aqueous systems for the pre-cooling that comminuted fibres element raw material is dipped in step 1, using metal stirring rod 8000 ~
10000 revs/min of high-speed stirreds make cellulose dissolution, obtain cellulose solution；
Step 3: being added graphene oxide in cellulose solution obtained in step 2, ultrasound keeps graphene oxide evenly dispersed
Into cellulose solution；
Step 4: the cellulose solution vacuum defoamation that step 3 is obtained is suppressed through compressed air, is measured for use as spinning solution
Pump, which is squeezed into coagulating bath, to be solidified；Oil bath in silver nitrate/glycerol/silicone oil mixed solution is entered back into after coagulating bath, wherein
Glycerol concentration is 1 ~ 5wt%, and silicone oil concentration is 2 ~ 4wt%, and with daylight light irradiation, is finally dried to obtain cellulose base silver/oxidation
Graphene/zinc oxide composite fibre；Wherein coagulating bath includes the first coagulating bath, the second gelation and third coagulating bath, ethylene glycol
For the first coagulating bath, ethyl alcohol is the second gelation, and water is third coagulating bath.
Pulverized fiber raw material used is sheet, and molecular weight cellulose concentration in 80000 or so, solution is 5wt%,
It needs to be cooled to -11~-15 DEG C before immersing the aqueous systems of pre-cooling.
Graphene oxide is made with reduction method in step 3, and mass fraction is 0.5 ~ 1.0wt%, 5 ~ 10min of ultrasound；
The temperature of the first coagulating bath ethylene glycol is 40 ~ 45 DEG C in step 4, and setting time is 5 ~ 10 seconds, the second gelation ethyl alcohol
Temperature is 30 ~ 35 DEG C, and setting time is 5 ~ 7 seconds, and it is 40 ~ 45 DEG C that third, which solidifies bath water temperature, and setting time is 5 ~ 10 seconds.Nitric acid
Silver concentration is 1 × 10-5~5×10-5Mol/L, fluorescent lamp 200w irradiate 2h.
The diameter of fiber is 15~30 μm, and Particle Size of Nanometer ZnO is 50 ~ 80nm, and nano silver partial size is 10 ~ 30nm, with fibre
Dimension element is used as bracket, and nano zine oxide and graphene oxide are distributed in cellulose matrix, and nano silver is coated on nano zine oxide
Surface.
Compare with the existing technology has marked improvement using technical solution of the present invention, and can obtain the utility model has the advantages that 1) this hair
The bright molecular characterization for making full use of natural fiber includes biomineralization activity and reproducibility, and the interface between bond material is mutual
Effect, and these techniques are mixed in conventional wet lay spinning technique, whole process does not use high temperature, high pressure and toxic reducing agent,
Green, environmental protection and be convenient for industrialized production；
2) nanofiller in cellulose base composite material is prepared and uniformly divides the surface and inside for being sprinkling upon cellulose matrix.Together
When, there are interfacial interactions abundant again between each nanofiller.The two common guarantee material composite fibre has efficient anti-
Bacterium activity and excellent antibacterial stability.
Specific embodiment
Technical solution of the present invention is further explained below in conjunction with specific embodiment.
Embodiment 1
First step configuration NaOH/ urea/Zinc oxide water solvent is simultaneously refrigerated to -11 DEG C in cold well, combines aqueous systems by 7wt%
NaOH, 12wt% urea, 1wt% zinc oxide and water composition；Comminuted fibres element raw material is added to NaOH/ urea/oxygen by second step
Change in zinc aqueous systems, quickly stirred to dissolve with metallic rod, obtains cellulose solution, mixing speed is 8000 revs/min, fine
Tieing up plain concentration is 5wt%；0.5wt% graphene oxide is added in third step in obtained cellulose solution, and ultrasonic 5min makes to aoxidize
Graphene uniform is distributed in cellulose solution；4th step by cellulose solution vacuum defoamation for use as spinning solution, through compressing
Air is suppressed, metering pump is squeezed into coagulating bath and solidifies, and wherein ethylene glycol is the first coagulating bath, and temperature is 45 DEG C, solidification 5
Second, ethyl alcohol is the second gelation, and temperature is 30 DEG C, is solidified 5 seconds, and water is third coagulating bath, 40 DEG C of temperature, is solidified 5 seconds；By solidifying
Gu entering back into oil bath in silver nitrate/glycerol/silicone oil mixed solution after bath, wherein silver nitrate concentration is 3 × 10-5Mol/L, glycerol are dense
Degree is 1wt%, and silicone oil concentration is 2wt%, and with 200w daylight light irradiation 2h, is finally dried to obtain cellulose base silver/graphite oxide
Alkene/zinc oxide composite fibre.
The diameter of composite fibre obtained, fiber is 25 μm, Particle Size of Nanometer ZnO 60nm, and nano silver partial size is
20nm.Gained composite fibre has excellent anti-microbial property, and composite fibre is to Escherichia coli, staphylococcus aureus in 3 hours
And the killing rate of Pseudomonas be after 100%, 30 days its 88%, 87% is still reached to the killing rate of above-mentioned three kinds of bacteriums
With 89%；85%, 81% and 82% is still reached to the killing rate of above-mentioned three kinds of bacteriums in 3 hours after living through 10 washings.
Embodiment 2
First step configuration NaOH/ urea/Zinc oxide water solvent is simultaneously refrigerated to -11 DEG C in cold well, combines aqueous systems by 7wt%
NaOH, 12wt% urea, 2wt% zinc oxide and water composition；Comminuted fibres element raw material is added to NaOH/ urea/oxygen by second step
Change in zinc aqueous systems, quickly stirred to dissolve with metallic rod, obtains cellulose solution, mixing speed is 8000 revs/min, fine
Tieing up plain concentration is 5wt%；1.0wt% graphene oxide is added in third step in obtained cellulose solution, and ultrasonic 5min makes to aoxidize
Graphene uniform is distributed in cellulose solution；4th step by cellulose solution vacuum defoamation for use as spinning solution, through compressing
Air is suppressed, metering pump is squeezed into coagulating bath and solidifies, and wherein ethylene glycol is the first coagulating bath, and temperature is 45 DEG C, solidification 5
Second, ethyl alcohol is the second gelation, and temperature is 30 DEG C, is solidified 5 seconds, and water is third coagulating bath, 40 DEG C of temperature, is solidified 5 seconds；By solidifying
Gu entering back into oil bath in silver nitrate/glycerol/silicone oil mixed solution after bath, wherein silver nitrate concentration is 5 × 10-5Mol/L, glycerol are dense
Degree is 5wt%, and silicone oil concentration is 4wt%, and with 200w daylight light irradiation 2h, is finally dried to obtain cellulose base silver/graphite oxide
Alkene/zinc oxide composite fibre.
The diameter of composite fibre obtained, fiber is 30 μm, Particle Size of Nanometer ZnO 50nm, and nano silver partial size is
18nm.Gained composite fibre has excellent anti-microbial property, and composite fibre is to Escherichia coli, staphylococcus aureus in 3 hours
And the killing rate of Pseudomonas be after 100%, 30 days its 97%, 94% is still reached to the killing rate of above-mentioned three kinds of bacteriums
With 95%；92%, 88% and 90% is still reached to the killing rate of above-mentioned three kinds of bacteriums in 3 hours after living through 10 washings.
Embodiment 3
First step configuration NaOH/ urea/Zinc oxide water solvent is simultaneously refrigerated to -12 DEG C in cold well, combines aqueous systems by 6.5wt%
NaOH, 11wt% urea, 2wt% zinc oxide and water composition；Comminuted fibres element raw material is added to NaOH/ urea/oxygen by second step
Change in zinc aqueous systems, quickly stirred to dissolve with metallic rod, obtains cellulose solution, mixing speed is 8000 revs/min, fine
Tieing up plain concentration is 5wt%；1.0wt% graphene oxide is added in third step in obtained cellulose solution, and ultrasonic 5min makes to aoxidize
Graphene uniform is distributed in cellulose solution；4th step by cellulose solution vacuum defoamation for use as spinning solution, through compressing
Air is suppressed, metering pump is squeezed into coagulating bath and solidifies, and wherein ethylene glycol is the first coagulating bath, and temperature is 45 DEG C, solidification 5
Second, ethyl alcohol is the second gelation, and temperature is 30 DEG C, is solidified 5 seconds, and water is third coagulating bath, 40 DEG C of temperature, is solidified 5 seconds；By solidifying
Gu entering back into oil bath in silver nitrate/glycerol/silicone oil mixed solution after bath, wherein silver nitrate concentration is 5 × 10-5Mol/L, glycerol are dense
Degree is 5wt%, and silicone oil concentration is 4wt%, and with 200w daylight light irradiation 2h, is finally dried to obtain cellulose base silver/graphite oxide
Alkene/zinc oxide composite fibre.
The diameter of composite fibre obtained, fiber is 40 μm, Particle Size of Nanometer ZnO 60nm, and nano silver partial size is
25nm.Gained composite fibre has excellent anti-microbial property, and composite fibre is to Escherichia coli, staphylococcus aureus in 3 hours
And the killing rate of Pseudomonas be after 100%, 30 days its 93%, 91% is still reached to the killing rate of above-mentioned three kinds of bacteriums
With 92%；90%, 88% and 89% is still reached to the killing rate of above-mentioned three kinds of bacteriums in 3 hours after living through 10 washings.
Embodiment 4
First step configuration NaOH/ urea/Zinc oxide water solvent is simultaneously refrigerated to -12 DEG C in cold well, combines aqueous systems by 6.5wt%
NaOH, 11wt% urea, 2wt% zinc oxide and water composition；Comminuted fibres element raw material is added to NaOH/ urea/oxygen by second step
Change in zinc aqueous systems, quickly stirred to dissolve with metallic rod, obtains cellulose solution, mixing speed is 8000 revs/min, fine
Tieing up plain concentration is 5wt%；1.0wt% graphene oxide is added in third step in obtained cellulose solution, and ultrasonic 5min makes to aoxidize
Graphene uniform is distributed in cellulose solution；4th step by cellulose solution vacuum defoamation for use as spinning solution, through compressing
Air is suppressed, metering pump is squeezed into coagulating bath and solidifies, and wherein ethylene glycol is the first coagulating bath, and temperature is 40 DEG C, solidification 10
Second, ethyl alcohol is the second gelation, and temperature is 35 DEG C, is solidified 7 seconds, and water is third coagulating bath, and temperature 45 C solidifies 10 seconds；By
Oil bath in silver nitrate/glycerol/silicone oil mixed solution is entered back into after coagulating bath, wherein silver nitrate concentration is 5 × 10-5Mol/L, glycerol
Concentration is 5wt%, and silicone oil concentration is 4wt%, and with 200w daylight light irradiation 2h, is finally dried to obtain cellulose base silver/oxidation stone
Black alkene/zinc oxide composite fibre.
The diameter of composite fibre obtained, fiber is 35 μm, Particle Size of Nanometer ZnO 45nm, and nano silver partial size is
22nm.Gained composite fibre has excellent anti-microbial property, and composite fibre is to Escherichia coli, staphylococcus aureus in 3 hours
And the killing rate of Pseudomonas be after 100%, 30 days its 95%, 92% is still reached to the killing rate of above-mentioned three kinds of bacteriums
With 93%；89%, 86% and 88% is still reached to the killing rate of above-mentioned three kinds of bacteriums in 3 hours after living through 10 washings.
Embodiment 5
First step configuration NaOH/ urea/Zinc oxide water solvent is simultaneously refrigerated to -13 DEG C in cold well, combines aqueous systems by 7.5wt%
NaOH, 13wt% urea, 0.5wt% zinc oxide and water composition；Second step by comminuted fibres element raw material be added to NaOH/ urea/
It in Zinc oxide water system, is quickly stirred to dissolve with metallic rod, obtains cellulose solution, mixing speed is 10000 revs/min
Clock, cellulose concentration 5wt%；Third step is added 0.5wt% graphene oxide in obtained cellulose solution, ultrasonic 10min,
Evenly spread to graphene oxide in cellulose solution；4th step by cellulose solution vacuum defoamation for use as spinning solution,
Suppressed through compressed air, metering pump is squeezed into coagulating bath and solidifies, wherein ethylene glycol be the first coagulating bath, temperature be 40 DEG C,
Solidification 10 seconds, ethyl alcohol are the second gelation, and temperature is 35 DEG C, are solidified 7 seconds, and water is third coagulating bath, temperature 45 C, solidification 10
Second；Oil bath in silver nitrate/glycerol/silicone oil mixed solution is entered back into after coagulating bath, wherein silver nitrate concentration is 1 × 10- 5Mol/L, glycerol concentration 1wt%, silicone oil concentration are 2wt%, and with 200w daylight light irradiation 2h, are finally dried to obtain cellulose
Ji Yin/graphene oxide/zinc oxide composite fibre.
The diameter of composite fibre obtained, fiber is 50 μm, Particle Size of Nanometer ZnO 50nm, and nano silver partial size is
26nm.Gained composite fibre has excellent anti-microbial property, and composite fibre is to Escherichia coli, staphylococcus aureus in 3 hours
And the killing rate of Pseudomonas be after 100%, 30 days its 88%, 84% is still reached to the killing rate of above-mentioned three kinds of bacteriums
With 89%；84%, 81% and 83% is still reached to the killing rate of above-mentioned three kinds of bacteriums in 3 hours after living through 10 washings.
Embodiment 6
First step configuration NaOH/ urea/Zinc oxide water solvent is simultaneously refrigerated to -15 DEG C in cold well, combines aqueous systems by 7.5wt%
NaOH, 13wt% urea, 2.0wt% zinc oxide and water composition；Second step by comminuted fibres element raw material be added to NaOH/ urea/
It in Zinc oxide water system, is quickly stirred to dissolve with metallic rod, obtains cellulose solution, mixing speed is 10000 revs/min
Clock, cellulose concentration 5wt%；Third step is added 1.0wt% graphene oxide in obtained cellulose solution, ultrasonic 10min,
Evenly spread to graphene oxide in cellulose solution；4th step by cellulose solution vacuum defoamation for use as spinning solution,
Suppressed through compressed air, metering pump is squeezed into coagulating bath and solidifies, wherein ethylene glycol be the first coagulating bath, temperature be 40 DEG C,
Solidification 10 seconds, ethyl alcohol are the second gelation, and temperature is 35 DEG C, are solidified 7 seconds, and water is third coagulating bath, temperature 45 C, solidification 10
Second；Oil bath in silver nitrate/glycerol/silicone oil mixed solution is entered back into after coagulating bath, wherein silver nitrate concentration is 5 × 10- 5Mol/L, glycerol concentration 5wt%, silicone oil concentration are 4wt%, and with 200w daylight light irradiation 2h, are finally dried to obtain cellulose
Ji Yin/graphene oxide/zinc oxide composite fibre.
The diameter of composite fibre obtained, fiber is 46 μm, Particle Size of Nanometer ZnO 38nm, and nano silver partial size is
22nm.Gained composite fibre has excellent anti-microbial property, and composite fibre is to Escherichia coli, staphylococcus aureus in 3 hours
And the killing rate of Pseudomonas be after 100%, 30 days its 99%, 95% is still reached to the killing rate of above-mentioned three kinds of bacteriums
With 96%；95%, 91% and 92% is still reached to the killing rate of above-mentioned three kinds of bacteriums in 3 hours after living through 10 washings.
Claims (7)
1. a kind of systemic activity antibacterial cellulose composite fibre, is made of cellulose, nano silver, zinc oxide and graphene oxide,
It is characterized by: the diameter of the composite fibre is 15~30 μm, Particle Size of Nanometer ZnO is 50 ~ 80nm, and nano silver partial size is
10 ~ 30nm, nano silver, zinc oxide and graphene oxide are distributed in the surface and inside of cellulose matrix.
2. a kind of systemic activity antibacterial cellulose composite fibre according to claim 1, it is characterised in that: the composite fibre
Excellent bactericidal effect, sterilizing rate 100% are all had to Escherichia coli, staphylococcus aureus and Pseudomonas.
3. a kind of systemic activity antibacterial cellulose composite fibre according to claim 1, it is characterised in that: the composite fibre
With the excellent washable effect of antibacterial, after washing 50-500 times, sterilizing rate is still able to maintain 95-100%.
4. a kind of systemic activity antibacterial cellulose composite fibre preparation method as described in one of claim 1-3, including it is as follows
Step:
Step 1: zinc oxide, sodium hydroxide, urea, which are sequentially added, dissolves them in water, be subsequently placed in cold in low temperature environment
Freeze to -11~-15 DEG C, wherein oxidation zinc concentration is 0.5-2.0wt%；The concentration of sodium hydroxide is 6.5-7.5wt%；Urea
Concentration be 11-13wt%；
Step 2: in the aqueous systems for the pre-cooling that comminuted fibres element raw material is dipped in step 1, using metal stirring rod 8000 ~
10000 revs/min of high-speed stirreds make cellulose dissolution, obtain cellulose solution；
Step 3: being added graphene oxide in cellulose solution obtained in step 2, continues stirring 5 minutes ~ 2 hours, makes oxygen
Graphite alkene is evenly spread in cellulose solution, and wherein the content of graphene oxide is 0.5 ~ 1.0wt%；
Step 4: the cellulose solution that step 3 is obtained is put into NaOH solution tank NaOH mesolow deaeration, for use as spinning solution；
Step 5: step 4 spinning solution is solidified in coagulating bath through spinneret, and coagulating bath is coagulated including the first coagulating bath, second
Gu bath and third coagulating bath, ethylene glycol is the first coagulating bath, and ethyl alcohol is the second gelation, and water is third coagulating bath；
Step 6: the fiber after step 5 is solidified immerses oil bath, and oil bath group is divided into silver nitrate, glycerol, silicone oil and water, wherein sweet
Oil concentration is 1 ~ 5wt%, and silicone oil concentration is 2 ~ 4wt%, and silver nitrate concentration is 1 × 10-5~5×10-5mol/L；Fiber after oiling
The standing and drying under daylight, fluorescent lamp or high voltage mercury lamp radiation, stand 2h, finally obtain cellulose base silver/graphene oxide/
Zinc oxide composite fibre.
5. systemic activity antibacterial cellulose composite fibre preparation method according to claim 4, it is characterised in that: step 2
In pulverized fiber raw material used be sheet, molecular weight cellulose concentration in 80000 or so, solution is 5wt%, pre- immersing
It needs to be cooled to -11~-15 DEG C before cold aqueous systems.
6. systemic activity antibacterial cellulose composite fibre preparation method according to claim 4, it is characterised in that: step 3
Middle graphene oxide is made with reduction method, and mass fraction is 0.5 ~ 1.0wt%, 5 ~ 10min of ultrasound.
7. systemic activity antibacterial cellulose composite fibre preparation method according to claim 4, it is characterised in that: step 5
In the temperature of the first coagulating bath ethylene glycol be 40 ~ 45 DEG C, setting time is 5 ~ 10 seconds, the temperature of the second gelation ethyl alcohol is 30 ~
35 DEG C, setting time is 5 ~ 7 seconds, and it is 40 ~ 45 DEG C that third, which solidifies bath water temperature, and setting time is 5 ~ 10 seconds；Silver nitrate concentration is 1
×10-5~5×10-5Mol/L, fluorescent lamp 200w irradiate 2h.
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| CN110042488A (en) * | 2019-04-23 | 2019-07-23 | 武汉大学 | A kind of preparation method of inexpensive, green, efficient high strength fibre element silk |
| CN113802200A (en) * | 2021-08-30 | 2021-12-17 | 兰州大学 | Functionalized graphene oxide/bacterial cellulose composite fiber and preparation method and application thereof |
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| CN110042488A (en) * | 2019-04-23 | 2019-07-23 | 武汉大学 | A kind of preparation method of inexpensive, green, efficient high strength fibre element silk |
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| CN113802200A (en) * | 2021-08-30 | 2021-12-17 | 兰州大学 | Functionalized graphene oxide/bacterial cellulose composite fiber and preparation method and application thereof |
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Application publication date: 20181218 |