CN103483468A - Method for preparing antibacterial agent for fiber fabric - Google Patents
Method for preparing antibacterial agent for fiber fabric Download PDFInfo
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- CN103483468A CN103483468A CN201310410449.0A CN201310410449A CN103483468A CN 103483468 A CN103483468 A CN 103483468A CN 201310410449 A CN201310410449 A CN 201310410449A CN 103483468 A CN103483468 A CN 103483468A
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Abstract
The invention relates to a method for preparing an antibacterial agent for a fiber fabric. The method comprises the following steps of dissolving a raw material chitosan into a 2 percent solution of acetic acid, stirring the solution until the chitosan is completely dissolved, performing precipitation by using a 30 percent solution of NaOH, washing precipitates until the precipitates are neutral, and performing suction filtration; placing the precipitates into a three-opening flask, adding water, stirring the mixture, raising temperature to 60 to 80 DEG C, adding glycidol trimethyl ammonium chloride, and performing reaction for 12 to 24 hours to obtain a clear and transparent light yellow liquid; precipitating the liquid by using mixed liquor of ethanol and acetone, performing suction filtration, and performing vacuum drying for 48 hours to obtain a crude product; dissolving the crude product in water, pouring the solution into a mixed solution of ethanol and acetone, performing reprecipitation and suction filtration, performing vacuum drying for 24 hours at 50 DEG C, performing soxhlet extraction for 24 hours at 80 DEG C by using ethanol, and performing suction filtration and vacuum drying to obtain a refined product. The method has the beneficial effects that a cotton fabric can be endowed with an antibacterial property within the whole pH value range after the obtained product is used for finishing the cotton fabric, and the problems of the conventional antibacterial agent are effectively solved.
Description
Technical field
The invention belongs to antibacterial fabric agent technical field, be specifically related to a kind of preparation method of the antiseptic-germicide for fabric.
Background technology
Enhancing along with people's self health consciousness, germ resistance to durable consumer goods such as sanitary product, daily necessities, water treatment device, food product pack, clothes has had higher requirement, adds antiseptic-germicide and prevents that the commodity of microbial reproduction from starting to be subject to human consumer's favor.
At present, antiseptic-germicide employed both at home and abroad is divided into inorganic antiseptic and the large class of organic antibacterial agent two by structure.Though the inorganic antiseptic antibacterial effect is lasting, acid and alkali-resistance, wash resistant, fast light good heat resistance, look easily occurs and become, and must make ultrafine powder and be evenly distributed on product surface, selective to carrier; Though organic antibacterial agent is dispersing and mixing, not easy to change, thermo-labile easily, bacterium may develop immunity to drugs to it, and the degradation production of some organic antibacterial agent also has certain toxic side effect.
Chitosan has certain advantage as natural antibacterial agent, and due to its aboundresources, nontoxic, pollution-free and have good biocompatibility and biodegradability, thereby the Application and Development progress is very fast.Its amino has very strong reactivity, and the amino acid and protein that forms human body is had to high affinity, by amino ion, angles the mechanism of interaction, restricting bacterial degree of freedom to have germ resistance.For chitosan molecule amount, deacetylation difference, also different to inhibition, the lethality of bacterium, and it is water insoluble, must dissolve with acid before arranging, then mix with a large amount of linking agents, fabric is processed comparatively loaded down with trivial details.And chitosan o'clock can lose cationic in pH >=6.5 to be caused poorly water-soluble and can only be confined to use under acidic conditions.Therefore, how the anti-microbial effect of chitosan can be applied in whole pH value scope, become the center of gravity of present researchist's research.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of preparation method of the antiseptic-germicide for fabric is provided, to chitosan, carry out quaternised modified, obtain chitosan quaternary ammonium salt derivatives, and cotton fabric is arranged, give its germ resistance in whole pH value scope, effectively solved the detrimentally affect to human body, textiles self performance and the poor problem of antibacterial effect that existing antiseptic-germicide exists.
A kind of preparation method of the antiseptic-germicide for fabric, comprise the steps:
Step 1: accurately take a certain amount of chitosan raw material with analytical balance, it is dissolved in 2% acetum, stir, after dissolving fully to chitosan, the NaOH solution precipitation with 30%, be washed to neutrality, suction filtration;
Step 2: the pretreated chitosan of above-mentioned process is put into to there-necked flask, add a certain amount of water, stir and be warming up to 60～80 ℃, then add the glycidyl trimethylammonium chloride with the chitosan certain mol proportion, react 12～24 hours, obtain the weak yellow liquid of clear;
Step 3: the 1:1 mixed solution precipitation of ethanol and acetone for the weak yellow liquid of the clear that step 2 is obtained, suction filtration, vacuum-drying 48 hours, obtain the raw product of chitosan quaternary ammonium salt derivatives;
Step 4: the raw product of the product that step 3 the is obtained dissolving of blunging, pour into while stirring in ethanol and the acetone mixing solutions with the 1:4 mixing, reprecipitation, suction filtration, 50 ℃ of lower vacuum-drying 24 hours, then use ethanol 80 ℃ of lower soxhlet extractions 24 hours, suction filtration, vacuum-drying, obtain the highly finished product of chitosan quaternary ammonium salt derivatives.
Reaction formula is
The beneficial effect that the present invention has is: chitosan aboundresources, nontoxic, pollution-free and have good biocompatibility and a biodegradability.Chitosan quaternary ammonium salt derivatives prepared as raw material by the chitosan of take, and cotton fabric is arranged, give its germ resistance in whole pH value scope, effectively solved the detrimentally affect to human body, textiles self performance and the poor problem of antibacterial effect that existing antiseptic-germicide exists.
Embodiment
In order further to understand advantage of the present invention, below enumerate several specific embodiments, so that effect of the present invention is done to further understanding.
Embodiment mono-:
A kind of preparation method of the antiseptic-germicide for fabric, comprise the steps:
Step 1: accurately take a certain amount of chitosan raw material with analytical balance, it is dissolved in 2% acetum, stir, after dissolving fully to chitosan, the NaOH solution precipitation with 30%, be washed to neutrality, suction filtration;
Step 2: the pretreated chitosan of above-mentioned process is put into to there-necked flask, add a certain amount of water, stir and to be warming up to 70 ℃, then add the glycidyl trimethylammonium chloride that the mol ratio with chitosan is 1:8, react 24 hours, obtain the weak yellow liquid of clear;
Step 3: the 1:1 mixed solution precipitation of ethanol and acetone for the weak yellow liquid of the clear that step 2 is obtained, suction filtration, vacuum-drying 48 hours, obtain the raw product of chitosan quaternary ammonium salt derivatives;
Step 4: the raw product of the product that step 3 the is obtained dissolving of blunging, pour into while stirring in ethanol and the acetone mixing solutions with the 1:4 mixing, reprecipitation, suction filtration, 50 ℃ of lower vacuum-drying 24 hours, then use ethanol 80 ℃ of lower soxhlet extractions 24 hours, suction filtration, vacuum-drying, obtain the highly finished product of chitosan quaternary ammonium salt derivatives.
Embodiment bis-:
A kind of preparation method of the antiseptic-germicide for fabric, comprise the steps:
Step 1: accurately take a certain amount of chitosan raw material with analytical balance, it is dissolved in 2% acetum, stir, after dissolving fully to chitosan, the NaOH solution precipitation with 30%, be washed to neutrality, suction filtration;
Step 2: the pretreated chitosan of above-mentioned process is put into to there-necked flask, add a certain amount of water, stir and to be warming up to 60 ℃, the glycidyl trimethylammonium chloride that then to add with the chitosan mol ratio be 1:10, react 24 hours, obtain the weak yellow liquid of clear;
Step 3: the 1:1 mixed solution precipitation of ethanol and acetone for the weak yellow liquid of the clear that step 2 is obtained, suction filtration, vacuum-drying 48 hours, obtain the raw product of chitosan quaternary ammonium salt derivatives;
Step 4: the raw product of the product that step 3 the is obtained dissolving of blunging, pour into while stirring in ethanol and the acetone mixing solutions with the 1:4 mixing, reprecipitation, suction filtration, 50 ℃ of lower vacuum-drying 24 hours, then use ethanol 80 ℃ of lower soxhlet extractions 24 hours, suction filtration, vacuum-drying, obtain the highly finished product of chitosan quaternary ammonium salt derivatives.
Embodiment tri-:
A kind of preparation method of the antiseptic-germicide for fabric, comprise the steps:
Step 1: accurately take a certain amount of chitosan raw material with analytical balance, it is dissolved in 2% acetum, stir, after dissolving fully to chitosan, the NaOH solution precipitation with 30%, be washed to neutrality, suction filtration;
Step 2: the pretreated chitosan of above-mentioned process is put into to there-necked flask, add a certain amount of water, stir and to be warming up to 80 ℃, the glycidyl trimethylammonium chloride that then to add with the chitosan mol ratio be 1:6, react 12 hours, obtain the weak yellow liquid of clear;
Step 3: the 1:1 mixed solution precipitation of ethanol and acetone for the weak yellow liquid of the clear that step 2 is obtained, suction filtration, vacuum-drying 48 hours, obtain the raw product of chitosan quaternary ammonium salt derivatives;
Step 4: the raw product of the product that step 3 the is obtained dissolving of blunging, pour into while stirring in ethanol and the acetone mixing solutions with the 1:4 mixing, reprecipitation, suction filtration, 50 ℃ of lower vacuum-drying 24 hours, then use ethanol 80 ℃ of lower soxhlet extractions 24 hours, suction filtration, vacuum-drying, obtain the highly finished product of chitosan quaternary ammonium salt derivatives.
Reaction formula of the present invention is:
In sum, above embodiment is only in order to illustrate the present invention and unrestricted technical scheme described in the invention; Therefore, although this specification sheets has been described in detail the present invention with reference to each above-mentioned embodiment,, those of ordinary skill in the art should be appreciated that still and can modify or be equal to replacement the present invention; And all do not break away from technical scheme and the improvement thereof of the spirit and scope of the present invention, it all should be encompassed in claim scope of the present invention.
Claims (2)
1. the preparation method for the antiseptic-germicide of fabric, is characterized in that, comprises the steps:
Step 1: take the chitosan raw material with analytical balance, it is dissolved in 2% acetum, stir, after dissolving fully to chitosan, the NaOH solution precipitation with 30%, be washed to neutrality, suction filtration;
Step 2: the pretreated chitosan of above-mentioned process is put into to there-necked flask, add water, stir and be warming up to 60～80 ℃, then add glycidyl trimethylammonium chloride, react 12～24 hours, obtain the weak yellow liquid of clear;
Step 3: the 1:1 mixed solution precipitation of ethanol and acetone for the weak yellow liquid of the clear that step 2 is obtained, suction filtration, vacuum-drying 48 hours, obtain the raw product of chitosan quaternary ammonium salt derivatives;
Step 4: the raw product of the product that step 3 the is obtained dissolving of blunging, pour into while stirring in ethanol and the acetone mixing solutions with the 1:4 mixing, reprecipitation, suction filtration, 50 ℃ of lower vacuum-drying 24 hours, then use ethanol 80 ℃ of lower soxhlet extractions 24 hours, suction filtration, vacuum-drying, obtain the highly finished product of chitosan quaternary ammonium salt derivatives.
2. the preparation method of the antiseptic-germicide for fabric according to claim 1, is characterized in that, comprises the steps:
Step 1: take the chitosan raw material with analytical balance, it is dissolved in 2% acetum, stir, after dissolving fully to chitosan, the NaOH solution precipitation with 30%, be washed to neutrality, suction filtration;
Step 2: the pretreated chitosan of above-mentioned process is put into to there-necked flask, add water, stir and to be warming up to 70 ℃, the glycidyl trimethylammonium chloride that then to add with the chitosan mol ratio be 1:8, react 24 hours, obtains the weak yellow liquid of clear;
Step 3: the 1:1 mixed solution precipitation of ethanol and acetone for the weak yellow liquid of the clear that step 2 is obtained, suction filtration, vacuum-drying 48 hours, obtain the raw product of chitosan quaternary ammonium salt derivatives; Step 4: the raw product of the product that step 3 the is obtained dissolving of blunging, pour into while stirring in ethanol and the acetone mixing solutions with the 1:4 mixing, reprecipitation, suction filtration, 50 ℃ of lower vacuum-drying 24 hours, then use ethanol 80 ℃ of lower soxhlet extractions 24 hours, suction filtration, vacuum-drying, obtain the highly finished product of chitosan quaternary ammonium salt derivatives.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310410449.0A CN103483468A (en) | 2013-09-11 | 2013-09-11 | Method for preparing antibacterial agent for fiber fabric |
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| CN201310410449.0A CN103483468A (en) | 2013-09-11 | 2013-09-11 | Method for preparing antibacterial agent for fiber fabric |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107338505A (en) * | 2016-12-13 | 2017-11-10 | 吴国宪 | A kind of anti-bacterial fibre for low frequency electromagnetic physiotherapy cushion and preparation method thereof |
| CN109316824A (en) * | 2018-09-26 | 2019-02-12 | 东华大学 | A kind of preparation method of Quaternary Ammonium Salt of Chitosan polyvinyl alcohol antimicrobial filtering composite material |
| CN113024687A (en) * | 2021-03-03 | 2021-06-25 | 晋大纳米科技（厦门）有限公司 | Preparation method of quaternary ammonium salinization modified soluble chitosan antibacterial agent, antibacterial agent and antibacterial fiber |
-
2013
- 2013-09-11 CN CN201310410449.0A patent/CN103483468A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 商成杰: "《纺织品抗菌及防螨整理》", 31 January 2009 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107338505A (en) * | 2016-12-13 | 2017-11-10 | 吴国宪 | A kind of anti-bacterial fibre for low frequency electromagnetic physiotherapy cushion and preparation method thereof |
| CN109316824A (en) * | 2018-09-26 | 2019-02-12 | 东华大学 | A kind of preparation method of Quaternary Ammonium Salt of Chitosan polyvinyl alcohol antimicrobial filtering composite material |
| CN113024687A (en) * | 2021-03-03 | 2021-06-25 | 晋大纳米科技（厦门）有限公司 | Preparation method of quaternary ammonium salinization modified soluble chitosan antibacterial agent, antibacterial agent and antibacterial fiber |
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