CN109252246A - A kind of water soluble algae silicate antibiosis fiber and preparation method thereof - Google Patents
A kind of water soluble algae silicate antibiosis fiber and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of water soluble algae silicate antibiosis fiber and preparation method thereof, which includes: to weigh water soluble polymer to be dissolved in distilled water, and nano silver-carrying basic zirconium phosphate then is added and/or nano zine oxide, ultrasonic disperse are uniform；It weighs sodium alginate to be dissolved in mixed liquor, agitating and heating obtains spinning solution；Spinning solution is subjected to deaeration, is ejected in coagulating bath through metering pump-metered from spinneret；Prepare sodium ethylene diamine tetracetate solution；After fiber extrusion is removed water, it is placed in sodium ethylene diamine tetracetate aqueous solution and impregnates；It adds sodium carbonate, sodium bicarbonate and is sufficiently mixed, continue to impregnate；Prepare chitosan solution；After fiber extrusion is removed water, it is placed in chitosan solution and impregnates；Fiber extrusion is discharged, then through drying, rolling step to obtain the final product.The present invention has the advantages that meet that water is instant, effective component is easily absorbed, good anti-bacterial effect, and overcomes that classic water-soluble fibre strength is low, the shortcomings that being easily broken off, and is with a wide range of applications.
Description
Technical field
The invention belongs to fibre manufacturing technology fields, and in particular to a kind of water soluble algae silicate antibiosis fiber and its preparation
Method.
Background technique
Water-soluble fibre can dissolve in water or meet water and slowly hydrolyse to water soluble molecules (or compound), be it is a kind of very
Valuable functional differential fibers can be applied to papermaking, medical non-woven fabrics, feminine care cotton.However due to existing water
There is the problems such as intensity is low, is easily broken off in soluble fiber, limit the application range of water-soluble fibre when in use.
Alginate fibre is polysaccharide to extract in natural seaweed as raw material, and water-soluble metal salt solution is coagulating bath, is led to
Cross a kind of novel high-performance fiber that wet spinning production technology obtains.Due to having accumulated mineral abundant in ocean in seaweed
Matter, and containing ingredients such as snoozed compound, amino acid, fat and various vitamins, can have with the metabolism of active cell
Anti-inflammatory, antipruritic function, so alginate fibre has the effect of natural curing, moisturizing, beauty to human skin.
Alginate fibre is a kind of common water-soluble fibre, and the medical dressing being made into calcium alginate fibre can be seeped with wound
The sodium ion in liquid and blood carries out ion exchange out, releases calcium ion, calcium ion can accelerate clot in capillary end
Formation, haemostatic effect is especially good；With increasing for sodium ion amount is absorbed, calcium alginate is gradually converted into being dissolved in the alginic acid of water
Sodium forms gel thin-layer in wound surface, to prevent the dressing adhesion surface of a wound, mitigates patient pain, and the surface of a wound is made to keep one
Fixed humidity and temperature is that a good microcirculation environment is created in the healing of the surface of a wound, wound is promoted to heal early.Calcium alginate
10-20 times up to own wt of the liquid absorption amount of dressing.But calcium alginate dressing antibacterial ability is relatively weak, limits seaweed
Application of the fiber as medical dressing.
Therefore, develop a kind of chance water energy be slowly dissolved, the effective component in slow release alginate fibre and antimicrobial component and
Alginate fibre with higher-strength is with a wide range of applications and good market prospects.
Summary of the invention
The present invention solves the technical problem of in view of the deficiencies of the prior art, providing, a kind of water soluble algae hydrochlorate is anti-
Bacterium fiber and preparation method thereof, obtained water soluble algae silicate antibiosis fiber, which not only has, meets that water is instant, effective component is easy
Be absorbed, good anti-bacterial effect the advantages of, also overcome that classic water-soluble fibre strength is low, the shortcomings that being easily broken off, have extensive
Application prospect.
To achieve the above object, the invention adopts the following technical scheme:
A kind of preparation method of water soluble algae silicate antibiosis fiber, comprising the following steps:
(1) it weighs water soluble polymer to be dissolved in distilled water, then weighs nano silver-carrying basic zirconium phosphate and/or nano zine oxide
It is added in the water-soluble polymer solution, ultrasonic disperse is uniform, spare；
(2) sodium alginate is weighed to be dissolved in mixed liquor made from step (1), preparation obtains sodium alginate mixed aqueous solution,
Then 60 DEG C are heated with stirring to, microwave oscillation or high-speed stirred 2h obtain uniform spinning solution；
(3) spinning solution that step (2) is prepared carries out deaeration, is ejected to solidification from spinneret through metering pump-metered
In bath；
(4) sodium ethylene diamine tetracetate is prepared to the ethylenediamine tetraacetic that mass fraction is soluble in water, and preparation mass fraction is 5-8%
Sodium acetate solution；
(5) step (3) is placed in sodium ethylene diamine tetracetate aqueous solution and is impregnated after the fiber extrusion of coagulating bath removes water
40-60min；
(6) sodium carbonate and sodium bicarbonate are then added into the sodium ethylene diamine tetracetate aqueous solution of step (5), makes carbonic acid
Sodium, sodium bicarbonate and sodium ethylene diamine tetracetate aqueous solution are sufficiently mixed, and fiber continues to impregnate 20-30min；
(7) chitosan is dissolved in the aqueous acetic acid that mass fraction is 1%, it is molten that the chitosan that mass fraction is 2% is made
Liquid；
(8) after the fiber extrusion of immersion removes water, it will be placed in the chitosan solution of step (7) and impregnate in step (6)
Impregnate 10-20min；
(9) step (8) are discharged by the fiber extrusion impregnated, then through drying, rolling step up to the water-soluble sea
Alginates anti-bacterial fibre.
The present invention enables obtained water soluble algae silicate antibiosis fiber to meet water instant fastly by improving preparation process
Solution, and the antibacterial effect of fiber is improved, obtained water soluble algae silicate antibiosis fiber not only has chance water instant, effective
The advantages of ingredient is easily absorbed, good anti-bacterial effect, also overcomes that classic water-soluble fibre strength is low, the shortcomings that being easily broken off.This
Invention by the fiber after coagulating bath again successively via sodium ethylene diamine tetracetate aqueous solution, sodium ethylene diamine tetracetate sodium carbonate,
Sodium bicarbonate mixed aqueous solution, can be improved the dissolution rate and solution rate of obtained fiber, and make in sodium ion and fiber
Calcium ion, aluminium ion exchange, so that the sodium ion in fiber, calcium ion, aluminium composition is maintained at suitable range, into
And guarantee the intensity of fiber, while being conducive to improve the solubility property of fiber, so that fiber obtained by the present invention is met water instant fastly
Solution is at sticky liquid state.It again passes by after chitosan aqueous solution impregnates modification, can further improve obtained water-soluble
The pliability of property alginate anti-bacterial fibre.
Further, in the step (1), the water soluble polymer is pectin, carboxymethyl chitosan, polyoxyethylene
One of alkene, gelatin, polyvinyl alcohol, sodium carboxymethylcellulose are a variety of, nano silver-carrying in the water-soluble polymer solution
The mass fraction of basic zirconium phosphate is 0.05-0.2%, and the mass fraction of water soluble polymer is 5-10%.
Further, the specific steps of step (1) are as follows: weigh water soluble polymer and be dissolved in distilled water, then weigh and receive
Rice silver-loaded zirconium phosphate, zinc oxide are added in the water-soluble polymer solution, and ultrasonic disperse is uniform, spare, the high water solubility
In molecular solution, nano silver-carrying basic zirconium phosphate, zinc oxide total mass fraction be 0.05-0.2%, nano silver-carrying basic zirconium phosphate, oxidation
The mass ratio of zinc is 5:1, and the mass fraction of the water soluble polymer is 5-10%.
Further, in step (2), sodium alginate mass fraction is 4-6% in spinning solution.
Further, the specific steps of step (3) are as follows: the spinning solution that step (2) is prepared carries out deaeration, through counting
Amount pump-metered is ejected in the first coagulating bath from spinneret, and the first coagulating bath is calcium chloride aqueous citric acid solution, the first coagulating bath
Temperature be 50 DEG C, setting time 2-3min；Then it is washed with distilled water, is re-introduced into the second gelation, the second solidification
Bath is the aluminum sulfate solution that 40 DEG C of mass fraction is 5%, and the coagulating bath time is 10min.
Further, the specific steps of step (3) are as follows: the spinning solution that step (2) is prepared carries out deaeration, through counting
Amount pump-metered is ejected in the first coagulating bath from spinneret, and the first coagulating bath is calcium chloride aqueous citric acid solution, the first coagulating bath
Temperature be 50 DEG C, setting time 2-3min；Then it is washed with distilled water, is re-introduced into the second gelation, the second solidification
Bath is the aluminum sulfate solution that 40 DEG C of mass fraction is 5%, and the coagulating bath time is 10min；It is re-introduced into third coagulating bath, the
Three coagulating baths are chitosan-acetic acid solution, and the temperature of third coagulating bath is 30 DEG C, setting time 10min.Fiber passes through second
Road coagulating bath improves water soluble algae silicate antibiosis fibre strength obtained after the processing of aluminum sulfate solution, but meeting
The hygroscopicity of caused water soluble algae silicate antibiosis fiber declines, so addition third road coagulating bath, passes through third coagulating bath
After the processing of middle chitosan acetic acid solution, not only nano silver-carrying basic zirconium phosphate and/or nano zine oxide can be made to be not easy from alginate fibre
Surface falls off, moreover it is possible to avoid the moisture absorption because of the caused water soluble algae silicate antibiosis fiber after the processing of aluminum sulfate solution
Property decline the problem of, while keeping the flexibility of water soluble algae silicate antibiosis fiber.
Further, lanolin, end of the lanolin in chitosan solution are also added in the chitosan solution of step (7)
Concentration is that mass fraction is 0.2%, to be further modified to fiber.
Further, the concrete operations of step (8) are as follows: after the fiber extrusion of immersion removes water, will be placed in step (6)
10-20min is impregnated in the chitosan solution of step (7), is then placed into the ethanol solution that mass fraction is 10-15%
It impregnates 3-5 minutes.Since ethyl alcohol can dissolve gas chromatography and inorganic matter, can improve obtained fiber chance water dissolution rate and
Rate of dissolution.
Further, in step (6), the mass ratio of sodium carbonate and sodium ethylene diamine tetracetate aqueous solution is 1:50-100, carbon
The mass ratio of sour hydrogen sodium and sodium ethylene diamine tetracetate aqueous solution is 1:100-150.In order to keep sodium carbonate, sodium bicarbonate faster more equal
Even the ethylenediamine tetra-acetic acid that is dissolved in is received in aqueous solution, can in advance dissolve sodium carbonate, a small amount of water of sodium bicarbonate, then again plus
Enter sodium ethylene diamine tetracetate aqueous solution.
The invention also discloses pass through water soluble algae silicate antibiosis fiber obtained by above-mentioned preparation method.
The invention also discloses a kind of above-mentioned water soluble algae silicate antibiosis fibers in medical treatment, the application of beauty treatment fields.By
Meeting water in water soluble algae silicate antibiosis fiber of the invention can quickly dissolve, and form sticky solution state, be conducive to fast instant
In solution and release alginate fiber to human skin have natural curing, moisturizing, beauty functions ingredient, therefore can generate
Better skin effect, therefore facial mask cloth can be fabricated to and be widely used in beauty treatment fields.In addition, the present invention is by improving preparation work
Nano silver-carrying basic zirconium phosphate and/or nano zine oxide are first dissolved in water soluble polymer by skill, improve nano silver-carrying basic zirconium phosphate and
Or distributing homogeneity of the nano zine oxide on alginate fibre, be conducive in use process the dissolution of antimicrobial component such as silver ion and
Release has better antibacterial effect.Water energy is met due to water soluble algae silicate antibiosis fiber of the invention again to be quickly dissolved into
Solution, therefore may also be fabricated which by spraying, when in sprinkling or coating to wound, it can be formed on its surface film, be conducive to the fast of wound
Speed healing, therefore can be widely applied to medical field.
To sum up, water soluble algae silicate antibiosis fiber market of the invention has a wide range of application, and using effect is good, has good
Market prospects.
Compared with prior art, the invention has the benefit that
(1) since alginate anti-bacterial fibre is prepared using silver to be applied on fabric in the prior art, there are silver
It with the adhesion property problem of fabric surface, such as should not clean, have obscission when cutting out, be also easy to produce surface covering and knitted with substrate
Phenomena such as object falls off, layering.Simultaneously in order to reach good anti-microbial property, so that the silver content of this dressing is very high, virtually
Improve the manufacturing cost of dressing.Reunite and be distributed in addition, prior art direct spraying nano silver powder is easy to produce nano silver
The problems such as uneven and easy to fall off, has seriously affected the antibacterial effect of dressing.And if inorganic antiseptic and alginate are total to
Wet spinning is carried out again with being prepared into spinning solution, will lead to that fibre strength is not high, and spinnability is poor.The present invention is by nano silver-carrying phosphorus
Sour zirconium and/or nano zine oxide are first dissolved in water soluble polymer, add sodium alginate be configured to uniform spinning solution into
Row wet spinning, alginate fibre surface and inside are distributed with nano silver-carrying basic zirconium phosphate and/or nano zine oxide after spinning, are not easy
It falls off from alginate fibre surface, improves antibiotic property.
(2) spinning solution is carried out twice or three coagulating baths by the present invention, and first of coagulating bath forms alginate antibacterial
Fiber after the processing of aluminum sulfate solution, makes water soluble algae silicate antibiosis fiber obtained subsequently into the second gelation
Intensity improves, but the hygroscopicity for the water soluble algae silicate antibiosis fiber that will lead to declines, so addition third road coagulating bath,
After processing by chitosan acetic acid solution in third coagulating bath, it can not only make nano silver-carrying basic zirconium phosphate and/or nano zine oxide
It is not easy to fall off from alginate fibre surface, moreover it is possible to avoid because of the caused water soluble algae hydrochlorate after the processing of aluminum sulfate solution
The problem of hygroscopicity decline of anti-bacterial fibre, while keeping the flexibility of water soluble algae silicate antibiosis fiber.
(3) present invention is by the fiber after coagulating bath again successively via sodium ethylene diamine tetracetate aqueous solution, ethylenediamine tetraacetic
Sodium acetate sodium carbonate, sodium bicarbonate mixed aqueous solution, can be improved the dissolution rate and solution rate of obtained fiber, and make sodium
Ion is exchanged with calcium ion, the aluminium ion in fiber, is maintained at the sodium ion in fiber, calcium ion, aluminium composition
Suitable range, and then guarantee the intensity of fiber, while being conducive to improve the solubility of fiber, make fiber obtained by the present invention
It meets water and is quickly dissolved into sticky liquid state.After again passing by chitosan aqueous solution immersion modification, it can further improve institute
The pliability of water soluble algae silicate antibiosis fiber obtained.
(4) during the preparation process, undope water soluble algae silicate antibiosis fiber of the invention other toxic or irritations
Solvent so that water soluble algae silicate antibiosis fiber made from this method have more higher safety, better biofacies
Capacitive, while there is good hygroscopicity, breaking strength and elongation at break.
(5) water soluble algae silicate antibiosis fiber market of the invention has a wide range of application, and can be used as facial mask cloth, Medical coating
Material, eye mask non-woven fabrics etc. are applied to medical treatment, beauty treatment fields, and using effect is good, have good market prospects: due to the present invention
Water soluble algae silicate antibiosis fiber meet water can quickly dissolve, form sticky solution state, be conducive to quickly dissolve and release
In alginate fiber to human skin have natural curing, moisturizing, beauty functions ingredient, therefore can generate better protect
Skin effect, therefore facial mask cloth can be fabricated to and be widely used in beauty treatment fields.In addition, the present invention will be received by improving preparation process
Rice silver-loaded zirconium phosphate and/or nano zine oxide are first dissolved in water soluble polymer, improve nano silver-carrying basic zirconium phosphate and/or nano oxygen
Change distributing homogeneity of the zinc on alginate fibre, be conducive to the dissolution and release of antimicrobial component such as silver ion in use process, has
There is better antibacterial effect.Water energy is met due to water soluble algae silicate antibiosis fiber of the invention again and is quickly dissolved into solution, because
This may also be fabricated which by spraying, when in sprinkling or coating to wound, can be formed on its surface film, be conducive to the quick healing of wound,
Therefore it can be widely applied to medical field.
Specific embodiment
The following specific embodiments are described below, is described in further details to technical solution of the present invention and effect.
Following the description is used to explain the present invention, rather than limitation of the present invention.
Embodiment 1
A kind of preparation method of water soluble algae silicate antibiosis fiber the following steps are included:
(1) it weighs gelatin to be dissolved in distilled water, then weighs nano silver-carrying basic zirconium phosphate and be added in the gelatin solution, ultrasound
It is uniformly dispersed, the mass fraction that nano silver-carrying basic zirconium phosphate is prepared is 0.05%, and the mixing that the mass fraction of gelatin is 5% is molten
Liquid；
(2) it weighs sodium alginate to be dissolved in mixed liquor made from step (1), preparation obtains sodium alginate mass fraction and is
4% sodium alginate aqueous solution, is then heated with stirring to 60 DEG C, and it is molten to obtain uniform spinning by microwave oscillation or high-speed stirred 2h
Liquid；
(3) spinning solution that step (2) is prepared carries out deaeration, is ejected to first from spinneret through metering pump-metered
In coagulating bath, first coagulating bath be the mass fraction of calcium chloride be 2%, the calcium chloride that the mass fraction of citric acid is 1%
Aqueous citric acid solution, the temperature of the first coagulating bath are 50 DEG C, setting time 2-3min；Then it is washed with distilled water, is re-introduced into
Into the second gelation, the second gelation is the aluminum sulfate solution that 40 DEG C of mass fraction is 5%, and setting time is
10min；
(4) sodium ethylene diamine tetracetate is prepared to the ethylenediamine tetrem that mass fraction is soluble in water, and preparation mass fraction is 5%
Acid sodium solution；
(5) step (3) is placed in sodium ethylene diamine tetracetate aqueous solution and is impregnated after the fiber extrusion of coagulating bath removes water
40min；
(6) then sodium carbonate and sodium bicarbonate will be added in the sodium ethylene diamine tetracetate aqueous solution of step (5), makes sodium carbonate
It is sufficiently mixed with sodium ethylene diamine tetracetate aqueous solution, fiber continues to impregnate 20min, wherein sodium carbonate and sodium ethylene diamine tetracetate
The mass ratio of aqueous solution is 1:50, and the mass ratio of sodium bicarbonate and sodium ethylene diamine tetracetate aqueous solution is 1:150；
(7) chitosan is dissolved in the aqueous acetic acid that mass fraction is 1%, it is molten that the chitosan that mass fraction is 2% is made
Liquid；
(8) after the fiber extrusion of immersion removes water, it will be placed in the chitosan solution of step (7) and impregnate in step (6)
10min is impregnated, then places into the ethanol solution that mass fraction is 10-15% and impregnates 3-5 minutes；
(9) step (8) are discharged by the fiber extrusion impregnated, then through drying, rolling step up to the water-soluble sea
Alginates anti-bacterial fibre.
Embodiment 2
A kind of preparation method of water soluble algae silicate antibiosis fiber the following steps are included:
(1) it weighs polyvinyl alcohol to be dissolved in distilled water, then weighing nano silver-carrying basic zirconium phosphate, to be added to the polyvinyl alcohol molten
In liquid, ultrasonic disperse is uniform, and the mass fraction that nano silver-carrying basic zirconium phosphate is prepared is 0.2%, the mass fraction of polyvinyl alcohol
For 10% mixed solution；
(2) it weighs sodium alginate to be dissolved in mixed liquor made from step (1), preparation obtains sodium alginate mass fraction and is
6% sodium alginate aqueous solution, is then heated with stirring to 60 DEG C, and it is molten to obtain uniform spinning by microwave oscillation or high-speed stirred 2h
Liquid；
(3) spinning solution that step (2) is prepared carries out deaeration, is ejected to first from spinneret through metering pump-metered
In coagulating bath, first coagulating bath be the mass fraction of calcium chloride be 3%, the calcium chloride that the mass fraction of citric acid is 1%
Aqueous citric acid solution, the temperature of the first coagulating bath are 50 DEG C, setting time 2-3min；Then it is washed with distilled water, is re-introduced into
Into the second gelation, the second gelation is the aluminum sulfate solution that 40 DEG C of mass fraction is 5%, and setting time is
10min；
(4) sodium ethylene diamine tetracetate is prepared to the ethylenediamine tetrem that mass fraction is soluble in water, and preparation mass fraction is 8%
Acid sodium solution；
(5) step (3) is placed in sodium ethylene diamine tetracetate aqueous solution and is impregnated after the fiber extrusion of coagulating bath removes water
60min；
(6) then sodium carbonate and sodium bicarbonate will be added in the sodium ethylene diamine tetracetate aqueous solution of step (5), makes sodium carbonate
It is sufficiently mixed with sodium ethylene diamine tetracetate aqueous solution, fiber continues to impregnate 30min, sodium carbonate and sodium ethylene diamine tetracetate aqueous solution
Mass ratio be 1:100, the mass ratio of sodium bicarbonate and sodium ethylene diamine tetracetate aqueous solution is 1:100；
(7) chitosan is dissolved in the aqueous acetic acid that mass fraction is 1%, it is molten that the chitosan that mass fraction is 2% is made
Liquid；
(8) after the fiber extrusion of immersion removes water, it will be placed in the chitosan solution of step (7) and impregnate in step (6)
Impregnate 20min；
(9) step (8) are discharged by the fiber extrusion impregnated, then through drying, rolling step up to the water-soluble sea
Alginates anti-bacterial fibre.
Embodiment 3
A kind of preparation method of water soluble algae silicate antibiosis fiber the following steps are included:
(1) it weighs polyvinyl alcohol and sodium carboxymethylcellulose is dissolved in distilled water, then weigh nano silver-carrying basic zirconium phosphate and add
Enter into the Polymer Solution, ultrasonic disperse is uniform, and the mass fraction that nano silver-carrying basic zirconium phosphate is prepared is 0.1%, poly- second
The mixed solution that the mass fraction of enol is 5%, the mass fraction of sodium carboxymethylcellulose is 2%；
(2) it weighs sodium alginate to be dissolved in mixed liquor made from step (1), preparation obtains sodium alginate mass fraction and is
5% sodium alginate aqueous solution, is then heated with stirring to 60 DEG C, and it is molten to obtain uniform spinning by microwave oscillation or high-speed stirred 2h
Liquid；
(3) spinning solution that step (2) is prepared carries out deaeration, is ejected to first from spinneret through metering pump-metered
In coagulating bath, first coagulating bath be the mass fraction of calcium chloride be 3%, the calcium chloride that the mass fraction of citric acid is 1%
Aqueous citric acid solution, the temperature of the first coagulating bath are 50 DEG C, setting time 2-3min；Then it is washed with distilled water, is re-introduced into
Into the second gelation, the second gelation is the aluminum sulfate solution that 40 DEG C of mass fraction is 5%, and setting time is
10min is re-introduced into third coagulating bath, and the third coagulating bath is chitosan acetic acid solution, and the temperature of third coagulating bath is
30 DEG C, setting time 10min；
(4) sodium ethylene diamine tetracetate is prepared to the ethylenediamine tetrem that mass fraction is soluble in water, and preparation mass fraction is 6%
Acid sodium solution；
(5) step (3) is placed in sodium ethylene diamine tetracetate aqueous solution and is impregnated after the fiber extrusion of coagulating bath removes water
50min；
(6) then sodium carbonate and sodium bicarbonate will be added in the sodium ethylene diamine tetracetate aqueous solution of step (5), makes sodium carbonate
It is sufficiently mixed with sodium ethylene diamine tetracetate aqueous solution, fiber continues to impregnate 25min, wherein sodium carbonate and sodium ethylene diamine tetracetate
The mass ratio of aqueous solution is 1:80, and the mass ratio of sodium bicarbonate and sodium ethylene diamine tetracetate aqueous solution is 1:120；
(7) chitosan is dissolved in the aqueous acetic acid that mass fraction is 1%, it is molten that the chitosan that mass fraction is 2% is made
Liquid；
(8) after the fiber extrusion of immersion removes water, it will be placed in the chitosan solution of step (7) and impregnate in step (6)
Impregnate 15min；
(9) step (8) are discharged by the fiber extrusion impregnated, then through drying, rolling step up to the water-soluble sea
Alginates anti-bacterial fibre.
Wherein, lanolin, final concentration of the lanolin in chitosan solution are also added in the chitosan solution of step (7)
It is 0.2% for mass fraction.
Embodiment 4
A kind of preparation method of water soluble algae silicate antibiosis fiber the following steps are included:
(1) it weighs polyvinyl alcohol and sodium carboxymethylcellulose is dissolved in distilled water, then weigh nano silver-carrying basic zirconium phosphate and add
Enter into the Polymer Solution, ultrasonic disperse is uniform, and the mass fraction that nano silver-carrying basic zirconium phosphate is prepared is 0.14%, poly- second
The mass fraction of enol is 5%, the mixed solution that the mass fraction of sodium carboxymethylcellulose is 3%；
(2) it weighs sodium alginate to be dissolved in mixed liquor made from step (1), preparation obtains sodium alginate mass fraction and is
5% sodium alginate aqueous solution, is then heated with stirring to 60 DEG C, and it is molten to obtain uniform spinning by microwave oscillation or high-speed stirred 2h
Liquid；
(3) spinning solution that step (2) is prepared carries out deaeration, is ejected to first from spinneret through metering pump-metered
In coagulating bath, first coagulating bath be the mass fraction of calcium chloride be 3%, the calcium chloride that the mass fraction of citric acid is 1%
Aqueous citric acid solution, the temperature of the first coagulating bath are 50 DEG C, setting time 2-3min；Then it is washed with distilled water, is re-introduced into
Into the second gelation, the second gelation is the aluminum sulfate solution that 40 DEG C of mass fraction is 5%, and setting time is
10min is re-introduced into third coagulating bath, and the third coagulating bath is chitosan acetic acid solution, and the temperature of third coagulating bath is
30 DEG C, setting time 10min；
(4) sodium ethylene diamine tetracetate is prepared to the ethylenediamine tetrem that mass fraction is soluble in water, and preparation mass fraction is 8%
Acid sodium solution；
(5) step (3) is placed in sodium ethylene diamine tetracetate aqueous solution and is impregnated after the fiber extrusion of coagulating bath removes water
60min；
(6) then sodium carbonate and sodium bicarbonate will be added in the sodium ethylene diamine tetracetate aqueous solution of step (5), makes sodium carbonate
It is sufficiently mixed with sodium ethylene diamine tetracetate aqueous solution, fiber continues to impregnate 25min, wherein sodium carbonate and sodium ethylene diamine tetracetate
The mass ratio of aqueous solution is 1:90, and the mass ratio of sodium bicarbonate and sodium ethylene diamine tetracetate aqueous solution is 1:100；
(7) chitosan is dissolved in the aqueous acetic acid that mass fraction is 1%, it is molten that the chitosan that mass fraction is 2% is made
Liquid；
(8) after the fiber extrusion of immersion removes water, it will be placed in the chitosan solution of step (7) and impregnate in step (6)
Impregnate 20min；
(9) step (8) are discharged by the fiber extrusion impregnated, then through drying, rolling step up to the water-soluble sea
Alginates anti-bacterial fibre.
Wherein, lanolin, final concentration of the lanolin in chitosan solution are also added in the chitosan solution of step (7)
It is 0.2% for mass fraction.
Embodiment 5
A kind of preparation method of water soluble algae silicate antibiosis fiber the following steps are included:
(1) it weighs polyvinyl alcohol and sodium carboxymethylcellulose is dissolved in distilled water, then weigh nano silver-carrying basic zirconium phosphate, oxygen
Change zinc to be added in the Polymer Solution, ultrasonic disperse is uniform, and the mass fraction that nano silver-carrying basic zirconium phosphate is prepared is
0.1%, the mass fraction of zinc oxide is 0.02%, and the mass fraction of polyvinyl alcohol is 5%, the quality point of sodium carboxymethylcellulose
The mixed solution that number is 3%；
(2) it weighs sodium alginate to be dissolved in mixed liquor made from step (1), preparation obtains sodium alginate mass fraction and is
5% sodium alginate aqueous solution, is then heated with stirring to 60 DEG C, and it is molten to obtain uniform spinning by microwave oscillation or high-speed stirred 2h
Liquid；
(3) spinning solution that step (2) is prepared carries out deaeration, is ejected to first from spinneret through metering pump-metered
In coagulating bath, first coagulating bath be the mass fraction of calcium chloride be 3%, the calcium chloride that the mass fraction of citric acid is 1%
Aqueous citric acid solution, the temperature of the first coagulating bath are 50 DEG C, setting time 2-3min；Then it is washed with distilled water, is re-introduced into
Into the second gelation, the second gelation is the aluminum sulfate solution that 40 DEG C of mass fraction is 5%, and setting time is
10min；It is re-introduced into third coagulating bath, the third coagulating bath is chitosan acetic acid solution, and the temperature of third coagulating bath is
30 DEG C, setting time 10min；
(4) sodium ethylene diamine tetracetate is prepared to the ethylenediamine tetrem that mass fraction is soluble in water, and preparation mass fraction is 6%
Acid sodium solution；
(5) step (3) is placed in sodium ethylene diamine tetracetate aqueous solution and is impregnated after the fiber extrusion of coagulating bath removes water
60min；
(6) then sodium carbonate and sodium bicarbonate will be added in the sodium ethylene diamine tetracetate aqueous solution of step (5), makes sodium carbonate
It is sufficiently mixed with sodium ethylene diamine tetracetate aqueous solution, fiber continues to impregnate 30min, wherein sodium carbonate and sodium ethylene diamine tetracetate
The mass ratio of aqueous solution is 1:100, and the mass ratio of sodium bicarbonate and sodium ethylene diamine tetracetate aqueous solution is 1:120；
(7) chitosan is dissolved in the aqueous acetic acid that mass fraction is 1%, it is molten that the chitosan that mass fraction is 2% is made
Liquid；
(8) after the fiber extrusion of immersion removes water, it will be placed in the chitosan solution of step (7) and impregnate in step (6)
Impregnate 15min；
(9) step (8) are discharged by the fiber extrusion impregnated, then through drying, rolling step up to the water-soluble sea
Alginates anti-bacterial fibre.
Wherein, lanolin, final concentration of the lanolin in chitosan solution are also added in the chitosan solution of step (7)
It is 0.2% for mass fraction.
Performance measurement is carried out to fiber obtained by embodiment 1-5.
Mechanics Performance Testing: testing according to GB/T 14337-2008 " chemical fibre Erichsen test method ", test 50
It is secondary, gauge 20mm, pre-tension 0.1cN, tensile speed 20mm/min.The result shows that water soluble algae obtained by the present invention
Silicate antibiosis fiber intensity with higher and elongation at break, breaking strength 2.1-2.6cN/dtex, elongation at break are
21.4-24.8%.
Fiber is met water-soluble and can be tested: fiber obtained by clip embodiment of the present invention 1-5 is put into proper amount of clear water,
Stirring at normal temperature makes it dissolve, the results showed that, water soluble algae silicate antibiosis fiber obtained by the present invention has good water-soluble
Property, it can be completely dissolved after meeting water 15-28 seconds.
For those of ordinary skill in the art, introduction according to the present invention is not departing from the principle of the present invention and essence
In the case where mind, modification, change, replacement and the deformation that specific embodiment is carried out still fall within protection scope of the present invention it
It is interior.
Claims (10)
1. a kind of preparation method of water soluble algae silicate antibiosis fiber, which comprises the following steps:
(1) it weighs water soluble polymer to be dissolved in distilled water, then weighs nano silver-carrying basic zirconium phosphate and/or nano zine oxide is added
Into the water-soluble polymer solution, ultrasonic disperse is uniform, spare；
(2) it weighs sodium alginate to be dissolved in mixed liquor made from step (1), preparation obtains sodium alginate mixed aqueous solution, then
It is heated with stirring to 60 DEG C, microwave oscillation or high-speed stirred 2h obtain uniform spinning solution；
(3) spinning solution that step (2) is prepared carries out deaeration, is ejected to coagulating bath from spinneret through metering pump-metered
In；
(4) sodium ethylene diamine tetracetate is prepared to the ethylenediamine tetra-acetic acid that mass fraction is soluble in water, and preparation mass fraction is 5-8%
Sodium solution；
(5) step (3) is placed in sodium ethylene diamine tetracetate aqueous solution after the fiber extrusion of coagulating bath removes water and impregnates 40-
60min；
(6) sodium carbonate and sodium bicarbonate are then added into the sodium ethylene diamine tetracetate aqueous solution of step (5), makes sodium carbonate, carbon
Sour hydrogen sodium is sufficiently mixed with sodium ethylene diamine tetracetate aqueous solution, and fiber continues to impregnate 20-30min；
(7) chitosan is dissolved in the aqueous acetic acid that mass fraction is 1%, the chitosan solution that mass fraction is 2% is made；
(8) it after the fiber extrusion of immersion removes water, will be placed in the chitosan solution of step (7) and impregnate in step (6)
10-20min；
(9) step (8) are discharged by the fiber extrusion impregnated, then through drying, rolling step up to the water soluble algae acid
Salt anti-bacterial fibre.
2. a kind of preparation method of water soluble algae silicate antibiosis fiber as described in claim 1, which is characterized in that step
(1) in, the water soluble polymer is pectin, carboxymethyl chitosan, polyethylene glycol oxide, gelatin, polyvinyl alcohol, carboxymethyl cellulose
One of plain sodium is a variety of, and in water-soluble polymer solution, the mass fraction of nano silver-carrying basic zirconium phosphate is 0.05-0.2%, water
The mass fraction of soluble macromolecular is 5-10%.
3. a kind of preparation method of water soluble algae silicate antibiosis fiber as described in claim 1, which is characterized in that step
(1) specific steps are as follows: weigh water soluble polymer and be dissolved in distilled water, then weigh nano silver-carrying basic zirconium phosphate, zinc oxide adds
Entering into the water-soluble polymer solution, ultrasonic disperse is uniform, and it is spare, in the water-soluble polymer solution, nano silver-carrying phosphorus
Sour zirconium, zinc oxide total mass fraction be 0.05-0.2%, nano silver-carrying basic zirconium phosphate, zinc oxide mass ratio be 5:1, the water
The mass fraction of soluble macromolecular is 5-10%.
4. a kind of preparation method of water soluble algae silicate antibiosis fiber as described in claim 1, which is characterized in that step
(2) in, sodium alginate mass fraction is 4-6% in the spinning solution.
5. a kind of preparation method of water soluble algae silicate antibiosis fiber as described in claim 1, which is characterized in that step
(3) specific steps are as follows: the spinning solution that step (2) is prepared carries out deaeration, sprays through metering pump-metered from spinneret
Into the first coagulating bath, the first coagulating bath is calcium chloride aqueous citric acid solution, and the temperature of the first coagulating bath is 50 DEG C, setting time
For 2-3min；Then it is washed with distilled water, is re-introduced into the second gelation, the second gelation is that 40 DEG C of mass fraction is
5% aluminum sulfate solution, coagulating bath time are 10min.
6. a kind of preparation method of water soluble algae silicate antibiosis fiber as described in claim 1, which is characterized in that step
(3) specific steps are as follows: the spinning solution that step (2) is prepared carries out deaeration, sprays through metering pump-metered from spinneret
Into the first coagulating bath, the first coagulating bath is calcium chloride aqueous citric acid solution, and the temperature of the first coagulating bath is 50 DEG C, setting time
For 2-3min；Then it is washed with distilled water, is re-introduced into the second gelation, the second gelation is that 40 DEG C of mass fraction is
5% aluminum sulfate solution, coagulating bath time are 10min；It is re-introduced into third coagulating bath, third coagulating bath is chitosan acetic acid
Solution, the temperature of third coagulating bath are 30 DEG C, setting time 10min.
7. a kind of preparation method of water soluble algae silicate antibiosis fiber as claimed in claim 6, which is characterized in that step
(7) lanolin is also added in chitosan solution, final concentration of mass fraction of the lanolin in chitosan solution is
0.2%.
8. a kind of preparation method of water soluble algae silicate antibiosis fiber as described in claim 1, which is characterized in that step
(6) in, the mass ratio of sodium carbonate and sodium ethylene diamine tetracetate aqueous solution is 1:50-100, sodium bicarbonate and sodium ethylene diamine tetracetate
The mass ratio of aqueous solution is 1:100-150.
9. water obtained by a kind of preparation method of water soluble algae silicate antibiosis fiber of any of claims 1-8
Solubility alga silicate antibiosis fiber.
10. a kind of water soluble algae silicate antibiosis fiber as claimed in claim 9 is in medical treatment, the application of beauty treatment fields.
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