CN102229689B - Preparation method of absorbent resin with bacteriostasis function - Google Patents
Preparation method of absorbent resin with bacteriostasis function Download PDFInfo
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- CN102229689B CN102229689B CN 201110121713 CN201110121713A CN102229689B CN 102229689 B CN102229689 B CN 102229689B CN 201110121713 CN201110121713 CN 201110121713 CN 201110121713 A CN201110121713 A CN 201110121713A CN 102229689 B CN102229689 B CN 102229689B
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Abstract
The invention discloses a preparation method of absorbent resin with a bacteriostasis function. The method comprises the following steps that: (1) sodium hydroxide is weighed and completely dissolved in deionized water, and an acrylic acid solution is slowly added; a neutralization degree of the solution is regulated to 50 to 90%; the solution is constantly stirred, such that a reaction is completely proceeded; the neutralized liquid is cooled; (2) the neutralized liquid is added to a chitosan solution; the resulting solution is sufficiently stirred; an initiator and a cross-linking agent are added to the solution for carrying out a graft-copolymerization reaction; the resulting material is stirred in an aqueous solution at a temperature of 65 DEG C, and the material is subject to a reaction; the material is stirred until the material turns viscous; the material is then subject to the reaction for 2 to 3 hours, such that absorbent resin with a bacteriostasis function is obtained. The product prepared with the method provided by the present invention has both high water absorbance and good bacteriostasis effect.
Description
Technical field
The present invention relates to a kind of preparation method with bacteriostasis property water-absorbing resin, belong to high molecular polymer based composites field.
Background technology
Chitosan is as a kind of Nantural non-toxic, good biocompatibility, and degradable, the renewable and very rich in natural resources of originating has caused day by day that people pay attention to, and has been successfully applied to a plurality of fields such as medicine.
The different molecular weight chitosan is different to the restraining effect mechanism of different microorganisms:
(1) for Gram-negative bacteria (intestinal bacteria), mainly be because micromolecular chitosan penetrating enters in the microorganism cells, electronegative tenuigenin in the adherent cell, and throwing out occurs, upset the normal physiological activity of cell, thus kill bacteria;
(2) to gram-positive microorganism (staphylococcus aureus), mainly be because macromolecular chitosan is adsorbed on the surface of microorganism cells, form one deck polymeric membrane, stoped nutritive substance in cell, to transport, until bacterium is dead.
Chitin is one of the abundantest natural organic-compound of occurring in nature, it is next in number only to Mierocrystalline cellulose, the nitrogenous natural organic-compound of quantity maximum outside the isolating protein on it or the earth simultaneously, almost there is 8% material to be rich in chitin in the water globe product organism, comprise shrimp, crab, squid, oyster and inkfish etc., the annual chitin that produces of sea leave surpasses 8,000 ten thousand tons, these oceanic resources of development and utilization, and tool is of great significance.The product chitosan of de-acetyl chitin; chitosan is comprised of most of D-glucosamine and a small amount of 2-acetylamino-2-deoxy-D-glucose; with β-(1; 4) straight-chain polysaccharide that connected of glycosidic link; its similar is in Mierocrystalline cellulose; chitosan is because of its unique molecular structure; it is the alkaline glycosaminoglycan of only a large amount of existence in the natural polysaccharide; chemical property is more active; being easy to carry out number of chemical modifies; and be dissolved in acidic aqueous solution, have good biocompatibility and biodegradability.Chitosan is because have a protonated ammonium, can with the cytolemma effect of bacterium negative charge, disturb the bacterial cell membrane function, cause bacterial body inner cell matter to run off, upset the normal physiological metabolism of cell, thereby reach the purpose of sterilization.
Present (patent publication No.: CN101559234A) aspect the domestic water-absorbing resin that has bacteriostasis property in preparation, by water absorbing resin particle being added in the dispersion liquid that contains silver ions, zine ion, titanium oxide and composition thereof, stirring is left standstill, and drying becomes the matrix material that contains antiseptic-germicide.This kind contains the silver ions matrix material because silver ions water-soluble, soluble in water when running into water in and be not attached to the water-absorbing material surface; Need under the photochemical catalysis condition, just possess antibacterial for zine ion, titanium oxide composite material.The present invention is with chitosan grafting acrylic acid synthetic resins, and antibacterial material is in the water-absorbing material all the time, and the product that possesses biocidal property and water absorbing properties just becomes emphasis of the present invention.
Summary of the invention
The object of the present invention is to provide a kind of preparation method with water-absorbing resin of bacteriostasis property.Product by preparation method of the present invention preparation possess high-hydroscopicity can the time also possess good fungistatic effect.
In order to reach above-mentioned purpose, solution of the present invention is:
A kind of preparation method with bacteriostasis property water-absorbing resin, comprise following processing step: 1) take by weighing potassium hydroxide fully dissolving in deionized water, slowly add acrylic acid solution, wherein the ratio of potassium hydroxide and acrylic acid add-on is potassium hydroxide: vinylformic acid=(40～73.5): 100 by weight; The adjusting degree of neutralization is 50-90%, does not stop to stir to make to react completely, and the cooling neutralizer is for subsequent use; 2) in the chitosan lysate, add neutralizer, adding initiator, linking agent carry out graft copolymerization after fully stirring, wherein the ratio of the add-on of chitosan, neutralizer, initiator and linking agent is chitosan: neutralizer: initiator: linking agent=(0.1～3.75g): (40～73.5g): (0.0625～0.5g): (0.0125～0.118g) by weight; Stirring reaction in 65 ℃ of aqueous solution reacts to thick the stopping of product and stirs, and continues the water-absorbing resin that reaction 2～3h can obtain having bacteriostasis property.
The ratio of described potassium hydroxide and acrylic acid add-on, be preferably by weight potassium hydroxide: vinylformic acid=62.5: 100, the ratio of the add-on of chitosan, neutralizer, initiator and linking agent is preferably chitosan: neutralizer: initiator by weight: linking agent=2.0: 62.5: 0.25: 0.025.
Described have bacteriostasis property water-absorbing resin product and put in 65 ℃ of baking ovens and dry to constant mass, then pulverizes and obtain powdery product.
Described chitosan lysate is take the chitosan of deacetylation 50.0--95.0% as raw material, and the acid adding solution stirring is the chitosan lysate to abundant dissolving; The ratio of chitosan and the add-on of acid solution wherein, by weight, chitosan: acid solution=1: 100.
The concentration of described acid solution is 1.0mol/L, and adopts a kind of in acetic acid, oxalic acid, vinylformic acid, citric acid or the hydrochloric acid.
Described initiator adopts Potassium Persulphate and sodium bisulfite.
Described linking agent adopts N,N methylene bis acrylamide.
Beneficial effect of the present invention is: the preparation method of a kind of chitosan grafting acrylic acid water-absorbing resin of the present invention, take vinylformic acid as matrix, with the chitosan grafting acrylic acid water-absorbing resin, this material also possesses good fungistatic effect when possessing the high-hydroscopicity energy, the resin water absorbent rate is 685g/g, bacteriostasis rate to intestinal bacteria and staphylococcus aureus reaches more than 70%, can be applied to health field, as being used for the sanitary care articles such as baby diaper, adult-incontinence diaper, sanitary napkin.
Description of drawings
Fig. 1 is process flow sheet of the present invention;
Fig. 2 is that chitosan resin is to intestinal bacteria (bacteria concentration 10
-7) antibacterial rear bacterium colony figure;
Fig. 3 be not chitosan-containing resin blank test to intestinal bacteria (bacteria concentration 10
-7) antibacterial rear bacterium colony figure;
Fig. 4 is that chitosan resin is to staphylococcus aureus (bacteria concentration 10
-7) antibacterial rear bacterium colony figure;
Fig. 5 is that the blank test of not chitosan-containing resin is to staphylococcus aureus (bacteria concentration 10
-7) antibacterial rear bacterium colony figure.
Embodiment
Embodiment 1
As shown in Figure 1, the present embodiment takes by weighing the fully dissolving in deionized water of 40g potassium hydroxide, slowly adds 100g vinylformic acid, and regulating degree of neutralization is 50%, does not stop to stir to make to react completely, and the cooling neutralizer is for subsequent use; Take by weighing the chitosan of 0.1g deacetylation 50.0--95.0%, add the 100g acetum and be stirred to abundant dissolving afterwards for the chitosan lysate, the concentration of acetum is 1.0mol/L.In the chitosan lysate, add the 40g neutralizer, add 0.0625g Potassium Persulphate and sodium bisulfite after fully stirring as initiator, 0.0125g N, the N-methylene-bisacrylamide is as linking agent, stirring reaction in 65 ℃ of aqueous solution, react to thick the stopping of product and stir, continue reaction 2～3h and can obtain product; Product put in 65 ℃ of baking ovens dry to constant mass, then pulverize and obtain Powdered super absorbent resin fat prod.Measure the synthetic resins performance, its water absorbent rate is 440g/g.
Embodiment 2
As shown in Figure 1, the present embodiment takes by weighing the fully dissolving in deionized water of 62.5g potassium hydroxide, slowly adds 100g vinylformic acid, regulates degree of neutralization 80%, does not stop to stir to make to react completely, and the cooling neutralizer is for subsequent use; Take by weighing the chitosan of 2.0g deacetylation 50.0--95.0%, add 100g vinylformic acid or citric acid solution and be stirred to abundant dissolving afterwards for the chitosan lysate, the concentration of vinylformic acid or citric acid solution is 1.0mol/L.In the chitosan lysate, add the 62.5g neutralizer, add 0.25g Potassium Persulphate and sodium bisulfite after fully stirring as initiator, 0.025g N, the N-methylene-bisacrylamide is as linking agent, stirring reaction in 65 ℃ of aqueous solution, react to thick the stopping of product and stir, continue reaction 2～3h and can obtain product; Product put in 65 ℃ of baking ovens dry to constant mass, then pulverize and obtain Powdered super absorbent resin fat prod.Measure the synthetic resins performance, it is water absorbent rate 804g/g.
Embodiment 3
As shown in Figure 1, the present embodiment takes by weighing the fully dissolving in deionized water of 73.5g potassium hydroxide, slowly adds 100g vinylformic acid, regulates degree of neutralization 90%, does not stop to stir to make to react completely, and the cooling neutralizer is for subsequent use; Take by weighing the chitosan of 3.75g deacetylation 50.0--95.0%, add the 100g hydrochloric acid soln and be stirred to abundant dissolving afterwards for the chitosan lysate, the concentration of hydrochloric acid soln is 1.0mol/L.In the chitosan lysate, add the 73.5g neutralizer, add 0.5g Potassium Persulphate and sodium bisulfite after fully stirring as initiator, 0.118g N, the N-methylene-bisacrylamide is as linking agent, stirring reaction in 65 ℃ of aqueous solution, react to thick the stopping of product and stir, continue reaction 2～3h and can obtain product; Product put in 65 ℃ of baking ovens dry to constant mass, then pulverize and obtain Powdered super absorbent resin fat prod.Measure the synthetic resins performance, it is water absorbent rate 850g/g.
Embodiment 4
Resin bacteriostasis property determination test:
Prepare respectively to contain colibacillary Bacteria liquid and contain the thin bacterium bacterial concentration of streptococcus aureus and (with the dilution of bacterium liquid be respectively: 10
-1～10
-9m
-1Concentration), make initial bacterium liquid contain bacterial concentration approximately 10
-7Ml
-1The order of magnitude, resin sample 0.10g, 18ml normal saline solution and the 1ml LB substratum that will prepare according to the method for embodiment 2 add in the Erlenmeyer flask of 50ml, add the cultured bacterium liquid of 1ml behind the autoclaving, put (37 ℃ of shaking tables, 150rpm) 8h is cultivated in concussion, pipettes 0.5ml bacterium liquid and do 10 from Erlenmeyer flask
-6, 10
-7Dilution after spread plate, each extent of dilution is coated with three culture dish, cultivates 24h in 37 ℃ of incubators, observes the bacterial growth situation, by formula η=(N
1-N
2)/N
1Calculate the resin bacteriostasis rate, wherein N
1Average colony number on the expression blank culture dish, N
2Expression adds resin sample and contains the average colony number of bacterium liquid on culture dish after processing, and calculates the resin bacteriostasis rate.Blank is identical with aforesaid operations but do not add resin.Shown in Fig. 1,2,3,4, Fig. 2 is that chitosan resin is to intestinal bacteria (bacteria concentration 10
-7) antibacterial rear bacterium colony figure; Fig. 3 be not chitosan-containing resin blank test to intestinal bacteria (bacteria concentration 10
-7) antibacterial rear bacterium colony figure; Fig. 4 is that chitosan resin is to staphylococcus aureus (bacteria concentration 10
-7) antibacterial rear bacterium colony figure; Fig. 5 is that the blank test of not chitosan-containing resin is to staphylococcus aureus (bacteria concentration 10
-7) antibacterial rear bacterium colony figure.By calculating colibacillary bacteriostasis rate is reached 76～88%; Bacteriostasis rate to streptococcus aureus is 72～77%.
Claims (7)
1. preparation method with bacteriostasis property water-absorbing resin, it is characterized in that comprising following processing step: 1) take by weighing potassium hydroxide fully dissolving in deionized water, slowly add acrylic acid solution, the ratio of potassium hydroxide and acrylic acid add-on wherein, be potassium hydroxide by weight: vinylformic acid=(40～73.5): 100, the adjusting degree of neutralization is 50-90%, does not stop to stir to make to react completely, and the cooling neutralizer is for subsequent use; 2) in the chitosan lysate, add neutralizer, adding initiator, linking agent carry out graft copolymerization after fully stirring, wherein the ratio of the add-on of chitosan lysate, neutralizer, initiator and linking agent is chitosan: neutralizer: initiator: linking agent=(0.1～3.75): (40～73.5): (0.0625～0.5): (0.0125～0.118) by weight; Stirring reaction in 65 ℃ of aqueous solution reacts to thick the stopping of product and stirs, and continues reaction 2～3h and can obtain having the bacteriostasis property water-absorbing resin.
2. a kind of preparation method with bacteriostasis property water-absorbing resin as claimed in claim 1, it is characterized in that: the ratio of described potassium hydroxide and acrylic acid add-on, be potassium hydroxide by weight: vinylformic acid=62.5: 100, the ratio of the add-on of chitosan, neutralizer, initiator and linking agent is chitosan: neutralizer: initiator: linking agent=2.0: 62.5: 0.25: 0.025 by weight.
3. a kind of preparation method with bacteriostasis property water-absorbing resin as claimed in claim 1 is characterized in that: described have bacteriostasis property water-absorbing resin product and put in 65 ℃ of baking ovens and dry to constant mass, then pulverizes and obtain powdery product.
4. a kind of preparation method with bacteriostasis property water-absorbing resin as claimed in claim 1, it is characterized in that: described chitosan lysate is take the chitosan of deacetylation 50.0--95.0% as raw material, and the acid adding solution stirring is the chitosan lysate to abundant dissolving; The ratio of chitosan and the add-on of acid solution wherein, by weight, chitosan: acid solution=1: 100.
5. a kind of preparation method with bacteriostasis property water-absorbing resin as claimed in claim 4, it is characterized in that: the concentration of described acid solution is 1.0mol/L, and adopts a kind of in acetic acid, oxalic acid, vinylformic acid, citric acid or the hydrochloric acid.
6. a kind of preparation method with bacteriostasis property water-absorbing resin as claimed in claim 1 is characterized in that: described initiator employing Potassium Persulphate and sodium bisulfite.
7. a kind of preparation method with bacteriostasis property water-absorbing resin as claimed in claim 1 is characterized in that: described linking agent employing N,N methylene bis acrylamide.
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| CN104497210A (en) * | 2014-11-13 | 2015-04-08 | 苏州威尔德工贸有限公司 | Super absorbent resin used for paper diaper and production method thereof |
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| CN110123528B (en) * | 2019-04-28 | 2021-06-18 | 杭州可靠护理用品股份有限公司 | Paper diaper with excellent water absorption and locking antibacterial performance and processing technology thereof |
| CN110280110A (en) * | 2019-07-02 | 2019-09-27 | 陕西中医药大学 | A kind of chemical drier and preparation method thereof |
| CN110558104B (en) * | 2019-10-15 | 2021-11-02 | 安徽强茗塑业科技有限公司 | Grass planting grid with water storage function |
| CN113563611B (en) * | 2021-07-16 | 2022-09-06 | 浙江大学 | Biocompatible hydrogel dry powder and preparation method and application thereof |
| CN114032687A (en) * | 2021-11-12 | 2022-02-11 | 南通大学 | Preparation method and application of moisture-proof and mildew-proof resin |
| CN115581792B (en) * | 2022-11-20 | 2023-12-19 | 上海护理佳实业有限公司 | Self-adhesive high-absorption material and absorption core |
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| CN1616505A (en) * | 2004-09-30 | 2005-05-18 | 北京理工大学 | Process for preparing chitosan base macroporous high water absorptive resin |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1616505A (en) * | 2004-09-30 | 2005-05-18 | 北京理工大学 | Process for preparing chitosan base macroporous high water absorptive resin |
Non-Patent Citations (1)
| Title |
|---|
| 辛华等.壳聚糖接枝共聚制备高吸水性树脂的研究.《化工新型材料》.2010,第38卷(第6期),第71-73页. * |
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