CN102454105B - Preparation method for superabsorbent antibacterial fiber - Google Patents
Preparation method for superabsorbent antibacterial fiber Download PDFInfo
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- CN102454105B CN102454105B CN201010517955.6A CN201010517955A CN102454105B CN 102454105 B CN102454105 B CN 102454105B CN 201010517955 A CN201010517955 A CN 201010517955A CN 102454105 B CN102454105 B CN 102454105B
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- polyglutamic acid
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Abstract
The invention discloses a preparation method for an antibacterial and absorbent polyglutamic acid fiber. The preparation method comprises the following step of: soaking a polyglutamic acid fiber into an aqueous solution of sodium hypochlorite, wherein a relational expression I between the soaking time T of the polyglutamic acid fiber and the concentration X of the aqueous solution of the sodium hypochlorite is that: (T-64.55X<2>+50X) is more than or equal to 10.2 and is less than or equal to 15.2 (I), wherein X=0.006-0.4 percent by weight.
Description
Technical field
The invention relates to a kind of preparation method of anti-bacterial fibre, particularly relevant for a kind of preparation method who possesses the high-hydroscopicity polyglutamic acid fiber of antibiotic property.
Background technology
High absorbency material because having the ability that can absorb moisture, and can retain the water with respect to the tens of quality to hundreds of times of sole mass, therefore its range of application is quite extensive after water suction.The conventional high absorbency material in this area mainly can be divided into two large classes, wherein a class be take carbohydrate as main, starch, chitosan, sodium alginate and carboxy methyl cellulose (Carboxymethyl cellulose for example, the polysaccharide such as CMC), this type of material is natural material, there is good Biodegradable, but because being limited to its water absorbent rate not high (being conventionally no more than 10 times), cause its application to be limited to.Another kind of is the macromolecule of chemical synthesis, polyester materials such as acrylates or vinyl alcohol.These materials have better water imbibition compared to aforesaid natural material, but it has preparation method more complicated, and may residual poisonous monomer and the problem such as alkali lye.In addition, this type of polyester material is not had a Biodegradable, after throwing aside, will work the mischief to environment.Therefore,, under environmental protection demand, generally still can select the poor natural polysaecharides material of water absorbing capacity as water-absorbing material.
Well known high absorbency material is often made into the kenel of glue or film.For example, in No. 6-322358th, Japanese patent laid-open, disclosed a kind of by gamma-radiation crosslinking technological, the crosslinked polyglutamic acid aqueous solution and make the method for high-hydroscopicity glue.The Ling U.S. the 4th, 572, No. 906 patent is also mentioned, utilizes the mixture of chitosan and gelatin can make a water imbibition film dressing.But the film disclosing in these technology and the surface of glue cannot provide the function of water conservancy diversion when contact liq, add and only depend on even curface to contact with liquid, thereby have too small problem with the contact area of liquid, and cause its whole rate of water absorption slower, it is restricted in the use.
If but by water-absorbing material fibration in addition, can effectively improve contact area, use the absorption rate increasing water.In addition, fibre structure also can provide diversion function, and rate of water absorption is got a promotion.In No. 200910137040.Xth, Chinese invention patent application, disclose and a kind ofly utilize natural polyglutamic acid to reel off raw silk from cocoons under partial cross-linked state, use the polyglutamic acid fiber that makes tool high-hydroscopicity.This technology fully solves the slower problem of natural water-absorbing material absorption speed well known in the art.
Only this kind of fiber, because having good Biodegradable, if while in use having part material to be decomposed, can cause integrally-built destruction and disintegration, causes its water imbibition to reduce.On the other hand, when its part material breakdown, just may form oligopeptides or amino acid monomer.Yet the nutrient source that these materials are microorganism, easily causes growing of microorganism.If this kind of fiber, for contacting with human body, even made to deposited material and is applied on medical care, cause most probably human body to be subject to the infection of microorganism.For avoiding the generation of this kind of harm, still need giving this kind of antibacterial ability that fiber is enough.
The antibacterial processing method of fiber, well known is generally in conjunction with the anti-biotic material of organic or inorganic on fiber.Wherein, inorganic antibacterial material is generally and contains metal ion (for example, Ag
+, Zn
2+) carrier, or nano metal particles (for example, nano silver particles).These inorganic antibacterial materials, by discharging these particles or ion, make it be combined with the cell protein of microorganism, cause bacterium to lose activity and reach antibacterial effect, and its antibacterial effect is conventionally comparatively long-acting.But inorganic antibacterial material, it processes preparation process complicated and expensive (the Ke You U.S. the 6th, 333, No. 093, the 6th on fiber, 451, No. 003 and the 6th, 267, No. 782 patent is known), also there are the problems such as cytotoxicity and rate of release are low, cause its whole antibacterial effect to be limited to.In addition, organic anti-bacterial material aspect, well known conventional quarternary ammonium salt is as disinfectant and the antiseptic of fiber, and it also has advantages of that antibacterial effect is lasting, but it has poor heat stability and can not use in the processing of plastics or fibre spinning, therefore in application, still have its restriction.
Therefore, develop the preparation method that a kind of preparation process is simple and easy and cost of manufacture is lower, to obtain the fiber of tool antibiotic property and tool high-hydroscopicity, have its necessity.
Summary of the invention
Main purpose of the present invention, is to provide the preparation method of a kind of tool high-hydroscopicity and tool antibiotic fiber.
Another object of the present invention, is to provide a kind of fiber by the prepared tool high-hydroscopicity of preparation method of the present invention and tool antibiotic property.
Another object of the present invention, is to provide a kind of by the prepared antimicrobial form water absorbing fabric of aforementioned fibers.
For reaching above-mentioned purpose of the present invention, pointed a kind of tool antibiotic property and the preparation method of tool high-hydroscopicity polyglutamic acid fiber according to the present invention, its step comprises provides a polyglutamic acid fiber to be soaked in aqueous sodium hypochlorite solution.Wherein, between the concentration X of this polyglutamic acid fiber soak time T and this aqueous sodium hypochlorite solution, there is the relational expression I being shown below:
10.2≤(T-64.55X
2+50X)≤15.2
(I)
Wherein, X=0.006-0.4wt%.
By the pointed preparation method of the present invention, can make easily the fiber of tool high-hydroscopicity and tool antibiotic property.In addition the prepared polyglutamic acid fiber of method produced according to the present invention, except still possessing good water suction, still has good antibiotic property, makes it be able to need not worry the problem of microbial contamination when application.
The specific embodiment
Pointed a kind of tool antibiotic property and the preparation method of tool high-hydroscopicity polyglutamic acid fiber according to the present invention, it is to be X (percentage by weight by a polyglutamic acid fiber being soaked in to concentration, wt%) in aqueous sodium hypochlorite solution, maintain a preset time T (minute).Wherein, between the concentration X of this polyglutamic acid fiber soak time T and this aqueous sodium hypochlorite solution, there is the relational expression I being shown below:
10.2≤(T-64.55X
2+50X)≤15.2
(I)
Wherein, X=0.006-0.4wt%.
According to the preparation method of disclosed tool antibiotic property and tool high-hydroscopicity polyglutamic acid fiber, when the operating condition numerical value of preparation, with above-mentioned relational expression T-64.55X
2+ 50X calculated the value of gained lower than 10.2 o'clock, easily had the problem of antibiotic property deficiency with the prepared fiber of preparation method of the present invention; Otherwise, if with above-mentioned relational expression T-64.55X
2+ 50X calculated the value of gained higher than 15.2 o'clock, though can make to there is enough antibiotic properties with the prepared fiber of preparation method of the present invention, easily too harsh because for the treatment of conditions under this situation, cause fibre structure to be damaged, and lose its due mechanical strength.
In addition,, when the clorox concentration X for the treatment of polyglutamic acid fiber is during lower than 0.006wt%, with the prepared fiber of preparation method of the present invention, easily have the problem of antibiotic property deficiency; Anti-, when the clorox concentration X for the treatment of polyglutamic acid fiber is during higher than 0.4wt%, though can make to there is enough antibiotic properties with the prepared fiber of preparation method of the present invention, but under this situation easily because treatment conditions are too harsh, cause fibre structure to be damaged, and lose its due mechanical strength.
Can be applicable to the polyglutamic acid fiber in the present invention, its preparation method is not particularly limited in the present invention.For example, the polyglutamic acid fiber method for making disclosing in No. 200910137040.Xth, Chinese invention patent application, it is to utilize natural polyglutamic acid to reel off raw silk from cocoons under partial cross-linked state, uses the polyglutamic acid fiber that makes tool high-hydroscopicity, but is not limited in this.The content disclosing in No. 200910137040.Xth, Chinese invention patent application, is all incorporated in the present invention.
Can be applicable to polyglutamic acid of the present invention, its molecular weight is not particularly limited, and considers operational convenience, and preferably is between 500-2, and between 000,000, better person is between 1,000-2 again, between 000,000.
In addition, in preparation method of the present invention, because aqueous sodium hypochlorite solution is strong oxidizer, for avoiding high temperature to cause the possibility of vigorous reaction release chlorine, temperature when therefore the aforementioned hypochlorous sodium aqueous solution carries out chlorination processing is preferably and remains on below ambient temperature.
The aforementioned hypochlorous sodium aqueous solution carries out in the step of chlorination processing, for making the sodium hypochlorite reaction in polyglutamic acid fiber and aqueous sodium hypochlorite solution comparatively quick, can further to aqueous sodium hypochlorite solution, bestow with external force and make its disturbance.For example, can stir by magnetite, shake up, blade stirring etc., any mode that other can apply well-known to those skilled in the art, range of application of the present invention is not limited to this measure.
For preparation method of the present invention is had, preferably prepare effect, the better system of pH value of aforementioned aqueous sodium hypochlorite solution is in the scope of 6-8; When under the too high alkaline environment of pH value, easily cause the sodium hypochlorite reaction speed in polyglutamic acid fiber and aqueous sodium hypochlorite solution slow, degree of oxidation is poor and effect is clear; And when pH is lower than 6 time, reaction speed can promote, but can cause the fracture of peptide bond (amide bond) and the decline of molecular weight simultaneously, and has destroyed the structure of polyglutamic acid fiber.
For controlling the pH value of aforementioned aqueous sodium hypochlorite solution, can remain in required scope in course of reaction, the better pH value buffer that can further add in aqueous sodium hypochlorite solution is used the pH value that regulates aqueous sodium hypochlorite solution.
The pH value buffer can be applicable in the present invention is not particularly limited, comprise but be not limited only to, phosphate aqueous solution, aqueous ammonium chloride solution, aqueous acetic acid, the dibastic sodium phosphate aqueous solution, the sodium hydrogen phosphate aqueous solution or the benzoic acid aqueous solution, or the mixed liquor of above-mentioned solution.
Disclosed tool antibiotic property and tool water imbibition polyglutamic acid fiber are to reach antibacterial effect by halogen amine functional group.The halogen amine functional group of N-X (X can be Cl, Br or I), under microorganism exists, in water, be subject to can slowly dissociate under the effect of hydrone, and the free halide ion with oxidation that discharges, the microorganisms such as this halide ion can killing bacteria, mould, therefore can obtain antibacterial effect.
Have the knack of person skilled in the art of the present invention, by explanation of the present invention, when recognizing, tool antibiotic property of the present invention and absorptive polyglutamic acid fiber can further be made fabric by textile technology well known in the art, Nonwovens (non-woven) for example, but be not limited in this.
Below enumerate several embodiment with elaboration method of the present invention more, right its use for illustrating only, not in order to limit the present invention, protection scope of the present invention when with claim the person of being defined be as the criterion.
Embodiment
The preparation of polyglutamic acid fiber
Get polyglutamic acid sodium salt (taste is red, Taiwan) and add the concentration that water is mixed with 6wt%.Afterwards, in the polyglutamic acid aqueous solution preparing, add the DGEEG (Ethylene glycoldiglycidyl ether, TOKYO YASEI, Japan) of using as crosslinking agent.With respect to the polyglutamic acid aqueous solution of every 100g, the addition of crosslinking agent is 7 μ L crosslinking agent/g polyglutamic acid aqueous solution, and in the polyglutamic acid aqueous solution, adding the initial viscosity that does not carry out cross-linking reaction after crosslinking agent is 56.4cp.
In the aforementioned polyglutamic acid aqueous solution, add after crosslinking agent, with the stir speed (S.S.) of 50rpm, at 60 ℃, carry out cross-linking reaction, when viscosity rises to 82cp (approximately 240 minutes), it is reeled off raw silk from cocoons by spinning mouth.For avoiding not yet continuing to be cross-linked by spinning the polyglutamic acid aqueous solution of mouth, the polyglutamic acid aqueous solution can be cooled to 6 ℃ to slow down cross-linking reaction.By aforementioned, by spinning the reel off raw silk from cocoons fiber of gained of mouth, pass in the isopropyl alcohol (model TG-078-000000-75NL, the bright chemical industry of scape, Taiwan) as solidification liquid, make its sizing.Afterwards, after prepared polyglutamic acid fiber is collected, move to oven dry (approximately 20 hours) in 60 ℃ of baking ovens.By this, can successfully make polyglutamic acid fiber.
The preparation of upgrading polyglutamic acid fiber
Embodiment 1:
Polyglutamic acid fiber is immersed in the aqueous sodium hypochlorite solution that concentration is 0.4wt%, and with the phosphate aqueous solution of 0.5N, pH value is adjusted between 6-8, soak and take out afterwards for 40 seconds.With this fiber of intermediate water rinse, standingly treat that it is dry.
Embodiment 2:
Polyglutamic acid fiber is immersed in the aqueous sodium hypochlorite solution that concentration is 0.3wt%, and with the phosphate aqueous solution of 0.5N, pH value is adjusted between 6-8, soak after 1 minute and take out.With this fiber of intermediate water rinse, standingly treat that it is dry.
Embodiment 3:
Polyglutamic acid fiber is immersed in the aqueous sodium hypochlorite solution that concentration is 0.16wt%, and with the phosphate aqueous solution of 0.5N, pH value is adjusted between 6-8, soak after 4 minutes and take out.With this fiber of intermediate water rinse, standingly treat that it is dry.
Embodiment 4:
Polyglutamic acid fiber is immersed in the aqueous sodium hypochlorite solution that concentration is 0.078wt%, and with the phosphate aqueous solution of 0.5N, pH value is adjusted between 6-8, soak after 7 minutes and take out.With this fiber of intermediate water rinse, standingly treat that it is dry.
Embodiment 5:
Polyglutamic acid fiber is immersed in the aqueous sodium hypochlorite solution that concentration is 0.006wt%, and with the phosphate aqueous solution of 0.5N, pH value is adjusted between 6-8, soak after 10 minutes and take out.With this fiber of intermediate water rinse, standingly treat that it is dry.
Comparative example 1:
Polyglutamic acid fiber is immersed in the aqueous sodium hypochlorite solution that concentration is 0.005wt%, and with the phosphate aqueous solution of 0.5N, pH value is adjusted between 6-8, soak after 10 minutes and take out.With this fiber of intermediate water rinse, standingly treat that it is dry.
Comparative example 2:
Polyglutamic acid fiber is immersed in the aqueous sodium hypochlorite solution that concentration is 0.4wt%, and with the phosphate aqueous solution of 0.5N, pH value is adjusted between 6-8, soak and take out afterwards for 20 seconds.With this fiber of intermediate water rinse, standingly treat that it is dry.
Comparative example 3:
Polyglutamic acid fiber is immersed in the aqueous sodium hypochlorite solution that concentration is 0.16wt%, and with the phosphate aqueous solution of 0.5N, pH value is adjusted between 6-8, although soak after 20 minutes, find that fibre structure also exists, lost intensity and easily loose.
Comparative example 4:
Polyglutamic acid fiber is immersed in the aqueous sodium hypochlorite solution that concentration is 0.3wt%, and with the phosphate aqueous solution of 0.5N, pH value is adjusted between 6-8, soak after 10 minutes and find that polyglutamic acid fiber has lost configuration and become glue and easily loose.
Comparative example 5:
Polyglutamic acid fiber is immersed in the aqueous sodium hypochlorite solution that concentration is 0.6wt%, and with the phosphate aqueous solution of 0.5N, pH value is adjusted between 6-8, but polyglutamic acid fiber at contact aqueous sodium hypochlorite solution simultaneously, produces the phenomenon that obvious structure crumbles, and decomposes completely in 30 minutes.
Comparative example 6:
Polyglutamic acid fiber is immersed in the aqueous sodium hypochlorite solution that concentration is 0.4wt%, and with the phosphate aqueous solution of 0.5N, pH value is adjusted into 5.5, soak and take out afterwards for 40 seconds.With this fiber of intermediate water rinse, standingly treat that it is dry.Though find that polyglutamic acid fiber structure also exists, lost intensity and easily loose.
Comparative example 7:
Polyglutamic acid fiber is immersed in the aqueous sodium hypochlorite solution that concentration is 0.4wt%, and with the phosphate aqueous solution of 0.5N, pH value is adjusted into 8.5, soak and take out afterwards for 40 seconds.With this fiber of intermediate water rinse, standingly treat that it is dry.Though find that polyglutamic acid fiber structure also exists, lost intensity and easily loose.
Antibacterial test
The antibacterial activity test of most of antiseptics is that the microorganism via the wide scope of antagonism comprises that Gram-positive and gram-negative micro-organism assess.Test organisms liquid of the present invention is staphylococcus aureus (Staphylococcus aureus, BCRC Number 15211) and Escherichia coli (Escherichia coli, BCRC Number 11446).Wherein, this staphylococcus aureus is a gram-positive bacteria, and Escherichia coli are Gram-negative bacterias.
A. the cultivation of bacterial strain
On agar medium by a preservation, pick out staphylococcus aureus and the Escherichia coli of a single bacterium colony (single colony), be seeded to respectively in the 15mL centrifuge tube of a LB cultured solution of broth that contains 2000 μ L (LB broth), then this centrifuge tube concussion is lasted to 10 minutes, after fully loose floating thalline, then formed stock (stock) bacterium liquid is carried out to 10 times of serial dilutions (10-fold serial dilution) with LB cultured solution of broth, to obtain thering are different extension rates (10
-1, 10
-2, 10
-3, 10
-4and 10
-5diluted bacterium liquid doubly).Afterwards, 100 μ L being had to the staphylococcus aureus of different extension rates and colibacillary bacterium liquid is seeded to respectively on different agar mediums and with triangular glass rod and is coated with equably.Then, the incubator that the agar medium that is coated with bacterium liquid is placed in to 37 ℃ is cultivated, last after 14-24 hour, it is the bacterium liquid of the different extension rates of the observable growth situation after painting dish, and the denumerable colony-forming units that goes out agar scope (20-300CFU), this step can determine that bacterium can normal growth under this environment.The colony-forming units of basis agar medium as calculated, gets appropriate stock bacterium liquid and adjusts bacterial concentration with aqua sterilisa again, take and obtains a concentration as 10
6-10
7the test organisms liquid of CFU/mL.
B. antibacterial qualitative test
Getting 100 μ L concentration is 10
6-10
7cFU/mL test organisms liquid (staphylococcus aureus and Escherichia coli) is seeded to respectively on different agar mediums, and is coated with equably with triangular glass rod.Then, embodiment 1-5 and the prepared sample of comparative example 1-2 be cut into respectively to a tablet and cover on the above-mentioned agar medium that contains test organisms liquid, then these agar mediums being placed in to the incubator of 37 ℃ and cultivating and last 14-24 hour.Afterwards, observe these sample surfaces and around.
With perusal, find example 1-5 sample surfaces and around without bacterium colony, produce, but inhibition zone not obvious infers that it is that contact is antibacterial, therefore can not discharge antipathogenic composition, but its sample itself and sample below there is no bacterium colony, produce.And comparative example 1-2 sample surfaces and all have bacterium colony to produce around can to see sample surfaces and be covered with bacterium colony around.
Treated fiber in comparative example 3-7, because its fibre structure undercapacity is easily loose, or disintegration and cannot be shaped to fiber, therefore cannot further carry out antibacterial tests test.
C. antibacterial quantitative test
This test is to assess according to the antibacterial benchmark of Static Contact AATCC 100.The sample of example 1-5 and comparative example 1-2 is cut into 2 * 2cm
2the bottle end of the smooth serum bottle of putting into 50mL respectively after size, getting 20 μ L staphylococcus aureus original bacteria liquids is inoculated on each sample, make bacterium liquid on sample, contact respectively 0 with 24 hours (contacting 0hr washes away immediately) and cultivate, just with the Tween80 solution of 20mL, bacterium liquid is swept away afterwards, then do respectively 10
-1, 10
-2, 10
-3, 10
-4with 10
-5dilution, respectively takes out 100 μ L from the solution of above-mentioned five kinds of dilution ratios and is placed in different solid mediums and is coated on agar equably.The agar of painting dish is put in the incubator of 37 ℃.After cultivating 14-24 hour, i.e. the bacterium liquid of observable under rinsing in test piece, with different dilution ratios, the growth situation after painting dish step, and by the denumerable agar counting that goes out the bacterium colony of scope (20-300CFU), and record it.
At this, we define the sterilizing ability of sample by bacterium colony residual volume, and formula is as follows:
After A:20 μ L original bacteria liquid contacts with sample, via 20mL Tween 80, wash away (washing away immediately), the bacterium liquid of collecting under washing away carries out painting dish, cultivates the clump count after 14-24h.
After B:20 μ L original bacteria liquid contacts 24h with sample, via 20mL Tween 80, wash away, the bacterium liquid of collecting under washing away carries out painting dish, cultivates the clump count after 14-24h.
When B is during much larger than A, representative sample there is no antibacterial ability.Its antibacterial result is as shown in Table 1:
Table one, quantitative antibacterial experiment experimental result
From antibacterial quantitative experiment result, in the sample of example 1-5, all can see its antibacterial effect, but comparative example 1-2 is without antibacterial ability.From the result of comparative example 1-7, soak time is too short or clorox concentration is too low again, and upgrading rate is not high, and does not have enough antibiotic effects; If soak time is oversize or clorox concentration is too high, make fiber in immersion process, lose gradually its mechanical strength, cause structural collapse and cannot further apply.Therefore must be with in disclosed preparation process parameter area, there are enough antibiotic effects prepared upgraded fiber side, and can maintain the configuration of polyglutamic acid fiber.
But as described above, be only preferred embodiment of the present invention, not in order to limit scope of the invention process, any those skilled in the art, within without departing from the spirit or scope of the invention, the simple equivalence of doing changes or modifies, and all still remains within the scope of the patent.
Claims (6)
1. a method of preparing tool antibiotic property and absorptive polyglutamic acid fiber, its step comprises: provide a polyglutamic acid fiber to be soaked in the aqueous sodium hypochlorite solution that pH value is 6-8, allow polyglutamic acid fiber there is the halogen amine functional group of antibacterial N-X, wherein X is Cl, Br or I, and wherein unit for minute this polyglutamic acid fiber soak time T and the concentration X of this aqueous sodium hypochlorite solution between, there is the relational expression I being shown below:
10.2≤(T-64.55X
2+50X)≤15.2 (Ⅰ)
Wherein, X=0.006-0.4wt%.
2. the method for claim 1, wherein this polyglutamic acid fiber is obtained by polyglutamic acid spinning after crosslinked.
3. the method for claim 1, wherein this aqueous sodium hypochlorite solution also comprises a pH value buffer.
4. method as claimed in claim 3, wherein this pH value buffer is phosphate aqueous solution, aqueous ammonium chloride solution, aqueous acetic acid, the dibastic sodium phosphate aqueous solution, the sodium hydrogen phosphate aqueous solution, the benzoic acid aqueous solution, or the mixed liquor of above-mentioned solution.
5. tool antibiotic property and an absorptive polyglutamic acid fiber, it is obtained by the method for claim 1.
6. tool antibiotic property and an absorptive polyglutamic acid fabric, it is obtained by fiber as claimed in claim 5.
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| CN102995460A (en) * | 2012-12-11 | 2013-03-27 | 海安县恒源丝织品有限公司 | Pure flax fabric |
| CN103572405A (en) * | 2013-11-07 | 2014-02-12 | 安徽工贸职业技术学院 | Polyglutamic acid antibacterial fiber |
| CN105289339B (en) * | 2015-11-16 | 2017-11-14 | 中国科学院长春应用化学研究所 | A kind of antibacterial ultrafiltration membrane and preparation method thereof and film renovation process |
| CN105795986A (en) * | 2016-04-29 | 2016-07-27 | 华南再生棉纱（梧州）有限公司 | Method for preparing high water-absorption bath towel with recycled cotton yarns |
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| US7858539B2 (en) * | 2007-04-09 | 2010-12-28 | Milliken & Company | Processes for generating halamine compounds on textile substrates to produce antimicrobial finish |
| TWI353397B (en) * | 2009-04-07 | 2011-12-01 | Far Eastern New Century Corp | Water-insoluble polyglutamic acid fiber and produc |
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