CN1480039A - Material for filtering and killing pathogenic microorganism and its preparing method - Google Patents
Material for filtering and killing pathogenic microorganism and its preparing method Download PDFInfo
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- CN1480039A CN1480039A CNA031318673A CN03131867A CN1480039A CN 1480039 A CN1480039 A CN 1480039A CN A031318673 A CNA031318673 A CN A031318673A CN 03131867 A CN03131867 A CN 03131867A CN 1480039 A CN1480039 A CN 1480039A
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- 239000000463 material Substances 0.000 title claims abstract description 64
- 230000002147 killing effect Effects 0.000 title claims abstract description 7
- 244000000010 microbial pathogen Species 0.000 title claims description 31
- 238000000034 method Methods 0.000 title claims description 10
- 238000001914 filtration Methods 0.000 title description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims abstract description 51
- 229910052740 iodine Inorganic materials 0.000 claims abstract description 51
- 239000011630 iodine Substances 0.000 claims abstract description 51
- 239000000835 fiber Substances 0.000 claims abstract description 43
- 229920001661 Chitosan Polymers 0.000 claims abstract description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 57
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 49
- 229920002472 Starch Polymers 0.000 claims description 29
- 235000019698 starch Nutrition 0.000 claims description 29
- 239000008107 starch Substances 0.000 claims description 29
- 239000004744 fabric Substances 0.000 claims description 21
- ZRSNZINYAWTAHE-UHFFFAOYSA-N p-methoxybenzaldehyde Chemical compound COC1=CC=C(C=O)C=C1 ZRSNZINYAWTAHE-UHFFFAOYSA-N 0.000 claims description 20
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 229920002101 Chitin Polymers 0.000 claims description 18
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 18
- 230000001112 coagulating effect Effects 0.000 claims description 14
- 229920000742 Cotton Polymers 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- NOOLISFMXDJSKH-UTLUCORTSA-N (+)-Neomenthol Chemical compound CC(C)[C@@H]1CC[C@@H](C)C[C@@H]1O NOOLISFMXDJSKH-UTLUCORTSA-N 0.000 claims description 10
- NOOLISFMXDJSKH-UHFFFAOYSA-N DL-menthol Natural products CC(C)C1CCC(C)CC1O NOOLISFMXDJSKH-UHFFFAOYSA-N 0.000 claims description 10
- 229940041616 menthol Drugs 0.000 claims description 10
- 230000006837 decompression Effects 0.000 claims description 9
- 238000007872 degassing Methods 0.000 claims description 9
- 235000011187 glycerol Nutrition 0.000 claims description 9
- 239000012535 impurity Substances 0.000 claims description 9
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 claims description 8
- 238000009987 spinning Methods 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 238000006386 neutralization reaction Methods 0.000 claims description 5
- 230000000536 complexating effect Effects 0.000 claims description 4
- 239000006210 lotion Substances 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 239000004310 lactic acid Substances 0.000 claims description 3
- 235000014655 lactic acid Nutrition 0.000 claims description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- 230000006196 deacetylation Effects 0.000 claims description 2
- 238000003381 deacetylation reaction Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 5
- 239000012528 membrane Substances 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 230000001717 pathogenic effect Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 32
- 230000000844 anti-bacterial effect Effects 0.000 description 16
- 239000002131 composite material Substances 0.000 description 13
- 241000191967 Staphylococcus aureus Species 0.000 description 9
- 241000894006 Bacteria Species 0.000 description 8
- 231100000331 toxic Toxicity 0.000 description 8
- 230000002588 toxic effect Effects 0.000 description 8
- 241000222122 Candida albicans Species 0.000 description 7
- 229940095731 candida albicans Drugs 0.000 description 7
- 229920002521 macromolecule Polymers 0.000 description 7
- 230000001954 sterilising effect Effects 0.000 description 6
- 239000004753 textile Substances 0.000 description 6
- 241000700605 Viruses Species 0.000 description 5
- 231100000572 poisoning Toxicity 0.000 description 5
- 230000000607 poisoning effect Effects 0.000 description 5
- 239000007921 spray Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000000645 desinfectant Substances 0.000 description 4
- 230000002045 lasting effect Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
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- 241000233866 Fungi Species 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000003899 bactericide agent Substances 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 3
- 238000012958 reprocessing Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CPKVUHPKYQGHMW-UHFFFAOYSA-N 1-ethenylpyrrolidin-2-one;molecular iodine Chemical compound II.C=CN1CCCC1=O CPKVUHPKYQGHMW-UHFFFAOYSA-N 0.000 description 2
- 229920000153 Povidone-iodine Polymers 0.000 description 2
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- 150000001875 compounds Chemical class 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
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- 238000005516 engineering process Methods 0.000 description 2
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- 239000000796 flavoring agent Substances 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- 230000002070 germicidal effect Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229960001621 povidone-iodine Drugs 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 239000000052 vinegar Substances 0.000 description 2
- 235000021419 vinegar Nutrition 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 1
- 108010054033 Chitin deacetylase Proteins 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 206010020751 Hypersensitivity Diseases 0.000 description 1
- 229920000881 Modified starch Polymers 0.000 description 1
- 239000004368 Modified starch Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 208000026935 allergic disease Diseases 0.000 description 1
- 230000007815 allergy Effects 0.000 description 1
- -1 amino, carboxyl Chemical group 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 244000144987 brood Species 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
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- 230000010534 mechanism of action Effects 0.000 description 1
- 235000019426 modified starch Nutrition 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
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- 230000000269 nucleophilic effect Effects 0.000 description 1
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- 238000011056 performance test Methods 0.000 description 1
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical class N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 1
- 235000019345 sodium thiosulphate Nutrition 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
A filter material for killing pathogenic microbes is prepared from chitosan membrane and fibre or fibrous product containing iodine (1-42 wt.%). Its advantages are high effect and long service life up to 20 days.
Description
One, technical field
Material is killed in the pathogenic microorganism filter that the present invention relates to shitosan and iodine composition.
Two, background technology
Iodine is a kind of bacterium, brood cell, fungi and spore thereof, virus and protozoon all to be had the broad-spectrum disinfectant of killing action rapidly.Its mechanism of action is the cytoplasmic movable gene of energy oxidizing bacteria, or combines and make it that irreversible denaturation takes place with the amino of virus protein outward.Its sterilizing power is than the strong 3-6 of chlorine-containing disinfectant times, even under cryogenic conditions, iodine possesses sterilizing power equally.Therefore abroad especially European and American countries be described as bactericide between second and be designated as disinfectant,legal.Yet also there are some shortcomings in iodine as disinfectant, is difficult for removing, has certain excitant and allergy etc. [referring to Chinese Disinfection magazine 1992,9 (3): 198-202] if any peculiar smell, volatile, easy xanthochromia.For this reason, people are carrying out research to the effect form of iodine always and are being improved.Povidone iodine system combines a kind of amorphous compound that forms by polyvinylpyrrolidone with iodine, contain available iodine 9%-12%.Be characterized in improving the solvability of iodine in water, had stable in properties, nonirritant and volatility, effect and relax advantages such as lasting, but because soluble in water, easy wash-out, therefore easy dyeing has limited its extensive use.Publication number is that 1366820 Chinese invention patent has been introduced a kind of high Polymer iodophor sterilant, and it is a kind of brown or black pearly-lustre orbicule.Its method and characteristics and povidone iodine are similar, and difference is that its content of iodine can reach 50%[referring to Chinese invention patent application number: 01120287.4].
Shitosan is the product of chitin deacetylase base.Chitin is very abundant in natural resource, and natural growing amount can reach more than 1,000,000,000 tons on the annual earth, is a kind of natural macromolecule.Obtained at aspects such as medicine, food, cosmetics, wastewater treatment, industry and agriculturals using widely.Shitosan is a linear macromolecule, has fibre forming property.Adopt wet spinning technology, shitosan can be spun into silk.Because shitosan has functions such as broad spectrum antibacterial, anti-corrosive properties, so chitin fiber can be used as anti-bacterial fibre and researchs and develops antibiotic fabric such as underwear, underpants, socks etc. [referring to macromolecule circular 2002 (6): 57-63].But the bactericidal effect of shitosan is not too strong, and we measure the shitosan and the fixing antibacterial activity of the later shitosan of iodine under the same conditions, and experiment shows that the antibacterial activity of shitosan has only 72.5% (staphylococcus aureus).Therefore people add some bactericide and improve bactericidal effect in the fiber of shitosan, as add phthalocyanine salts [referring to: day disclosure is speciallyyed permit JP2001,303,437].Chinese invention patent (publication number: 1115254) introduce the preparation of chitosan iodine wound dressing, they apply one deck chitosan film on nonwoven, again that this shitosan is compound non-woven fabric compounded material is immersed in and adsorbs iodine in the iodine solution, as the medical dressing of wound burn.
Three, summary of the invention
The objective of the invention is to utilize the active group (amino, carboxyl, aldehyde radical etc.) of natural macromolecular material to be fixed with the nucleophilic district formation complex of natural bactericidal agent iodine, the feature of this complex is can discharge for a long time to be enough to filter the iodine that kills all kinds of pathogene.Utilize the fibre forming property and the spinnability of selected macromolecular material simultaneously, make yarn, cotton, cloth respectively and produce relevant health product thus.
Technical scheme of the present invention is as follows:
Material is killed in the filter of a kind of pathogenic microorganism, and it is that mass percent content is arranged is that material is killed in the pathogenic microorganism filter of 1～42% iodine for film, fiber or this fiber manufactured goods complexing that shitosan is made.Pathogenic microorganism filter of the present invention is killed in the material, between shitosan and the iodine coordination is arranged, and makes iodine have the function of slowly-releasing.Under 25 ℃, place and still to keep original antibacterial activity after 20 days.
Material is killed in above-mentioned pathogenic microorganism filter, and described shitosan can be that deacetylation is 50～95% shitosan.
Can contain carboxymethyl starch in the above-mentioned shitosan, the mass ratio of shitosan and carboxymethyl starch is 1: 0.05～1: 0.2, and the fiber of gained or film can be called shitosan-carboxymethyl starch composite fibre or film.Adding carboxymethyl starch can increase coordination stability with iodine, under 25 ℃, places and can still keep original antibacterial activity after 15 days.
Material is killed in above-mentioned filter, and the fiber manufactured goods that shitosan is made can be yarn, cotton or cloth.Can be made into mouth mask, airstrainer etc. and kill the bacterium equipment.
Pathogenic microorganism of the present invention filter is killed material and can be sprayed anisaldehyde and menthol solution are arranged.Anisaldehyde, menthol etc. are natural efficiently volatility germicide, are again safe flavourings.Spraying anisaldehyde and menthol solution can increase the ability of its fragrant fragrance and sterilization.
A kind of above-mentioned pathogenic microorganism filter method of material extremely for preparing, it is made up of the following step:
Step 1, described shitosan is dissolved in the diluted acid that concentration is 0.5-5%, remove by filter impurity, the decompression degassing, chitosan solution is sprayed in the coagulating bath of being made up of sodium hydroxide solution and ethanol by spinning head, make its solidificating fiber, warm water washing, stretching, the dry chitin fiber that gets, or chitosan solution is cast into mould, drying under reduced pressure is with dilute solution of sodium hydroxide neutralization, washed with de-ionized water, drying and forming-film
Step 2, chitin fiber or the yarn that chitin fiber is made, cotton or cloth that step 1 is made, the perhaps chitosan film that step 1 is made, be immersed in the solution of forming by 1～10% iodine, 0.5～2% glycerine and 98.5～88% ethanol 0.5～48 hour
Step 3, with above-mentioned chitin fiber or its yarn of making, cotton or cloth, perhaps chitosan film takes out from iodine solution, respectively with ethanol with to be washed to washing lotion colourless, drying at room temperature promptly get pathogenic microorganism filter of the present invention material extremely.
The above-mentioned pathogenic microorganism filter method of material extremely for preparing, also can form by the following step:
Step 1, described shitosan is dissolved in the diluted acid that concentration is 0.5-5%, adds 0.5～2% carboxymethyl starch of chitosan mass, dissolving, remove by filter impurity, the decompression degassing, chitosan solution is sprayed in the coagulating bath of being made up of sodium hydroxide solution and ethanol by spinning head, make its solidificating fiber, warm water washing, stretching, the dry chitin fiber that gets, or chitosan solution is cast into mould, drying under reduced pressure is with dilute solution of sodium hydroxide neutralization, washed with de-ionized water, drying and forming-film
Step 2, with above-mentioned chitin fiber or its yarn of making, cotton or cloth, perhaps chitosan film is immersed in the solution of being made up of 1～10% iodine, 0.5～2% glycerine and 98.5～88% ethanol 0.5～48 hour,
Step 3, with above-mentioned chitin fiber or its yarn of making, cotton or cloth, perhaps chitosan film takes out, respectively with ethanol with to be washed to washing lotion colourless, drying at room temperature promptly get pathogenic microorganism of the present invention and filters material extremely.It is stronger that the coordination of shitosan and carboxymethyl starch and iodine is killed in the material in the filter of the pathogenic microorganism that so makes, and coordination stability is better.
In the step 1 of two above-mentioned methods, described diluted acid can be acetate, hydrochloric acid or lactic acid, and the mass ratio of coagulating bath 10% sodium hydroxide solution and ethanol is 50: 50～80: 20.
Material is killed in pathogenic microorganism filter of the present invention following characteristics:
1, still has efficient, quick-acting, the broad-spectrum sterilization power identical with iodine.We serve as the test bacterium with staphylococcus aureus, Candida albicans, and immobilization iodine reaches 99.999% and 99.973% respectively to their killing rate.And shitosan and the modified starch killing rate to staphylococcus aureus under similarity condition is respectively 72.5% and 0.5%.
2, have the function of slowly-releasing because material is killed in pathogenic microorganism of the present invention filter, so immobilization iodine have the advantage more lasting than iodine bactericidal action.Test shows that under 25 ℃ it still has same antibacterial activity after 20 days.
3, the iodine in the immobilization iodine is in the state of suppressed by vector complexing, and the iodine that is fixed is not only measured bigger, and character is more stable, and smell is little, toxicity is low, nonirritant, have cleaning, decontamination and deodorant effect concurrently.Under 25 ℃, the content by iodine in the air of this material is respectively 0.070-0.780mg/m
3, recommending the aerial threshold limit value of iodine less than ACGIH is 1mg/m
3[referring to Hazardous Chemical Substances up-to-date application manual: 146,1996 Chinese material publishing houses; Chemicals toxicity, rules, environmental data handbook: 513,1992, the China Environmental Science Press].Therefore under conventional working concentration, this material is safe to the people.
4, the depth of immobilization iodine color and available iodine content just are proportionate, and lost sterilizing power when colourless, but carrier material are recyclable, and be available above-mentioned with reusing after the quadrat method processing again.
5, the iodine with the macromolecular material complexing can discharge for a long time, has the effect of lasting pathogenic microbe killing.And anisaldehyde, menthol etc. are natural efficiently volatility germicide, are again safe flavourings.But the volatile matter of these sterilizations own not only has synergistic function with iodine, bring lasting delicate fragrance sense can for again the user of this product.
Simple, the easy row of preparation method of the present invention, cost is low.
Four, embodiment
The performance test of material is killed in pathogenic microorganism filter of the present invention:
1, the anti-microbial property test method of material is tested by People's Republic of China's textile industry standard FZ/T01021-92 " antibacterial fabric method for testing performance ".We are the anti-microbial property [referring to People's Republic of China (PRC) textile industry standard FZ/T 01021-92] that the test bacterium is measured material with staphylococcus aureus, Candida albicans.This shows that pathogenic microorganism of the present invention filter kills that chelated iodine can slowly release in the material, and to pathogenic microorganisms such as disease fungus, bacterium, virus performance toxic action.
2, the pathogenic microorganism of the present invention filter assay that kills iodine in the material is measured by the iodimetric titration in the Pharmacopoeia of People's Republic of China.With spirit of vinegar and potassium iodide shitosan is dissolved earlier, iodine is discharged, measure the content [referring to two pharmacopeia notes of Pharmacopoeia of People's Republic of China nineteen ninety version: 848 Chemical Industry Press] of iodine in the material then by the titration of sodium thiosulfate standard solution.
3, volatility test under the immobilization iodine room temperature: material is killed in pathogenic microorganism filter of the present invention place a glass tube, a termination of glass tube has the impinger of gas flowmeter, the absorption liquid monoiod(in)ate aqueous solutions of potassium of the logical people's iodine of the other end.Under certain flow, behind the ventilation appropriate time, absorption liquid is made developer with starch,, kill the material volatility of iodine at room temperature thereby calculate pathogenic microorganism filter of the present invention with the content of iodine in the spectrophotometry absorption liquid.It is 1mg/m that ACGIH is recommended the aerial threshold limit value of iodine
3
Embodiment 1
With shitosan with 2% (m/m, down together) after the spirit of vinegar dissolving, the content of shitosan in solution is 4% (m/m, down together), remove by filter impurity, the decompression degassing, by spinning head shitosan is sprayed into by sodium hydroxide solution and ethanol and form (mass ratio, sodium hydroxide: water: coagulating bath ethanol=7: 63: 30), make shitosan in coagulating bath, be frozen into silk, take out the shitosan silk, warm water washing, stretching, the dry chitin fiber that gets.Chitin fiber can be reprocessed into cotton, yarn, cloth, and other textile fabrics [referring to macromolecule circular 2002 (6): 57-63].
To in 2% iodohydrin solution (containing 0.5% glycerine), place 4 hours by the gauze that chitin fiber is made, and take out gauze and clean with the second alcohol and water respectively.Spray is with anisaldehyde and menthol solution after the drying at room temperature.Promptly get pathogenic microorganism filter of the present invention and kill material.This material is yellow.The content of iodine is 4.5% in the material, and the toxic action of staphylococcus aureus, Candida albicans is reached 99.999% and 99.963% respectively.By the report of pharmacopeia, if this material is brought into play so high toxic action to disease fungus and bacterium, then it also is sure to the toxic action of virus.
Under 25 ℃, the content by iodine in the air of this material is 0.070mg/m
3Utilize this antibacterial gauze to prepare medical bactericidal mask.This mouth mask is can not only the airborne pathogenic microorganism of Filtration Adsorption such as bacterium, virus, and can kill them, thus it can improve mouth mask antibacterial effect, prolong single service time of mouth mask, can also reduce the number of plies of mouth mask.The time of keeping effective poisoning concentration simultaneously can reach 15 days.
Embodiment 2
With shitosan with after 5% acetic acid,diluted (content of shitosan in solution the is 5%) dissolving, add a certain amount of carboxymethyl starch (shitosan: carboxymethyl starch=1: 0.1m/m), after waiting to dissolve, remove by filter impurity, the decompression degassing, by spinning head shitosan is sprayed into by sodium hydroxide solution and ethanol and to form (sodium hydroxide: water: ethanol=6: 54: 40,) coagulating bath, make shitosan in coagulating bath, be frozen into silk, take out the shitosan silk, warm water washing, stretching, the dry shitosan-carboxymethyl starch composite fibre that gets.Can be with this shitosan-carboxymethyl starch composite fibre reprocessing resultant yarn, cloth, and other textile fabrics [referring to macromolecule circular 2002 (6): 57-63].
The gauze that shitosan-the carboxymethyl starch composite fibre is made was placed 6 and 12 hours in 5% iodohydrin solution (containing 0.5% glycerine), taken out gauze and clean with the second alcohol and water respectively.Spray promptly gets pathogenic microorganism filter of the present invention with anisaldehyde and menthol solution and kills material after the drying at room temperature.This material is brownish red and black.The quality percentage composition of iodine is respectively 11%, 27% in the material, and the toxic action of staphylococcus aureus, Candida albicans is reached 99.999% and 99.973% respectively.Under 25 ℃, the content by iodine in the air of this material is respectively 0.098mg/m
3And 0.212mg/m
3The time of keeping effective poisoning concentration simultaneously can reach 20 days.
Embodiment 3
With shitosan with 1% diluted hydrochloric acid dissolution after, add a certain amount of carboxymethyl starch (shitosan: carboxymethyl starch=1: 0.05m/m), after waiting to dissolve, remove by filter impurity, the decompression degassing, by spinning head shitosan is sprayed into by sodium hydroxide solution and ethanol and to form (sodium hydroxide: water: coagulating bath ethanol=5: 45: 50), make shitosan in coagulating bath, be frozen into silk, take out the shitosan silk, warm water washing, stretching, the dry shitosan-carboxymethyl starch composite fibre that gets.Can be with this shitosan-carboxymethyl starch composite fibre reprocessing resultant yarn, cloth, and other textile fabrics [referring to macromolecule circular 2002 (6): 57-63].
The gauze that shitosan-the carboxymethyl starch composite fibre is made was placed 0.5 hour in 1% iodohydrin solution (containing 2% glycerine), taken out gauze and clean with the second alcohol and water respectively.Spray promptly gets pathogenic microorganism filter of the present invention and kills material with anisaldehyde and menthol solution after the drying at room temperature.This material is yellow.The quality percentage composition of iodine is respectively 1% in the material, and the toxic action of staphylococcus aureus, Candida albicans is reached 99.999% and 99.973% respectively.Under 25 ℃, the content by iodine in the air of this material is respectively 0.098mg/m
3The time of keeping effective poisoning concentration simultaneously can reach 20 days.
Embodiment 4
With shitosan with 0.5% diluted hydrochloric acid dissolution after, add a certain amount of carboxymethyl starch (shitosan: carboxymethyl starch=1: 0.2m/m), after waiting to dissolve, remove by filter impurity, the decompression degassing, by spinning head shitosan is sprayed into the coagulating bath of being made of (sodium hydroxide: water: ethanol=8: 72: 20) sodium hydroxide solution and ethanol, make shitosan in coagulating bath, be frozen into silk, take out the shitosan silk, warm water washing, stretching, the dry shitosan-carboxymethyl starch composite fibre that gets.Can be with this shitosan-carboxymethyl starch composite fibre reprocessing resultant yarn, cloth, and other textile fabrics [referring to macromolecule circular 2002 (6): 57-63].
The gauze that shitosan-the carboxymethyl starch composite fibre is made was placed 12 hours in 5% iodohydrin solution (containing 0.5% glycerine), taken out gauze and clean with the second alcohol and water respectively.Spray promptly gets pathogenic microorganism filter of the present invention with anisaldehyde and menthol solution and kills material after the drying at room temperature.This material is brownish red and black.The quality percentage composition of iodine is respectively 27% in the material, and the toxic action of staphylococcus aureus, Candida albicans is reached 99.999% and 99.973% respectively.Under 25 ℃, the content by iodine in the air of this material is respectively 0.212mg/m
3The time of keeping effective poisoning concentration simultaneously can reach 20 days.
Embodiment 5
Elder generation with 2% rare lactic acid dissolution, adds a certain amount of carboxymethyl starch (shitosan: carboxymethyl starch=1: 0.15m/m), remove by filter impurity, the decompression degassing with shitosan then.Be cast into mould then, drying under reduced pressure, with dilute solution of sodium hydroxide (concentration 5%) neutralization, washed with de-ionized water, 50 ℃ of drying and mouldings get shitosan-carboxymethyl starch composite membrane.
Shitosan-carboxymethyl starch composite membrane was placed 48 hours in 10% iodohydrin solution (containing 1% glycerine), taken out composite membrane and clean with the second alcohol and water respectively.Spray promptly gets pathogenic microorganism filter of the present invention with anisaldehyde and menthol solution and kills material after the drying at room temperature.This material is a black.The content of iodine is 42% in the material, and the toxic action of staphylococcus aureus, Candida albicans is reached 99.9996% and 99.997% respectively.Under 25 ℃, the content by iodine in the air of this material is 0.780mg/m
3The time of keeping effective poisoning concentration simultaneously can reach 20 days.
Claims (9)
1. material is killed in pathogenic microorganism filter, it is characterized in that it is that mass percent content is arranged is that material is killed in the pathogenic microorganism filter of 1～42% iodine for film, fiber or this fiber manufactured goods complexing that shitosan is made.
2. material is killed in filter according to claim 1, it is characterized in that described shitosan is that deacetylation is 50～95% shitosan.
3. material is killed in filter according to claim 1, it is characterized in that described shitosan contains carboxymethyl starch, and the mass ratio of shitosan and carboxymethyl starch is 1: 0.05～1: 0.2.
4. material is killed in filter according to claim 1 and 2, it is characterized in that the fiber manufactured goods that shitosan is made are yarn, cotton or cloth.
5. material is killed in filter according to claim 1 and 2, it is characterized in that killing material surface in filter is sprayed with anisaldehyde and menthol solution.
6. one kind prepares the method that material is killed in the described filter of claim 1, it is characterized in that being made up of the following step:
Step 1, described shitosan is dissolved in the diluted acid that concentration is 0.5-5%, remove by filter impurity, the decompression degassing, chitosan solution is sprayed in the coagulating bath of being made up of sodium hydroxide solution and ethanol by spinning head, make its solidificating fiber, warm water washing, stretching, the dry chitin fiber that gets, or chitosan solution is cast into mould, drying under reduced pressure is with dilute solution of sodium hydroxide neutralization, washed with de-ionized water, drying and forming-film
Step 2, with above-mentioned chitin fiber or its yarn of making, cotton or cloth, perhaps chitosan film is immersed in the solution of being made up of 1～10% iodine, 0.5～2% glycerine and 98.5～88% ethanol 0.5～48 hour,
Step 3, with above-mentioned chitin fiber or its yarn of making, cotton or cloth, perhaps chitosan film takes out, respectively with ethanol with to be washed to washing lotion colourless, drying at room temperature promptly get pathogenic microorganism of the present invention and filters material extremely.
7. one kind prepares the method that material is killed in the described filter of claim 3, it is characterized in that being made up of the following step:
Step 1, described shitosan is dissolved in the diluted acid that concentration is 0.5-5%, adds 0.5～2% carboxymethyl starch of chitosan mass, dissolving, remove by filter impurity, the decompression degassing, chitosan solution is sprayed in the coagulating bath of being made up of sodium hydroxide solution and ethanol by spinning head, make its solidificating fiber, warm water washing, stretching, the dry chitin fiber that gets, or chitosan solution is cast into mould, drying under reduced pressure is with dilute solution of sodium hydroxide neutralization, washed with de-ionized water, drying and forming-film
Step 2, with above-mentioned chitin fiber or its yarn of making, cotton or cloth, perhaps chitosan film is immersed in the solution of being made up of 1～10% iodine, 0.5～2% glycerine and 98.5～88% ethanol 0.5～48 hour,
Step 3, with above-mentioned chitin fiber or its yarn of making, cotton or cloth, perhaps chitosan film takes out, respectively with ethanol with to be washed to washing lotion colourless, drying at room temperature promptly get pathogenic microorganism of the present invention and filters material extremely.
8. according to claim 6 or 7 described preparation methods, it is characterized in that the diluted acid described in the step 1 is acetate, lactic acid or hydrochloric acid.
9. according to claim 6 or 7 described preparation methods, it is characterized in that the mass ratio of coagulating bath 10% sodium hydroxide solution described in the step 1 and ethanol is 50: 50～80: 20.
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Cited By (7)
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| CN102888672A (en) * | 2011-07-20 | 2013-01-23 | 李永兴 | Method for preparing chitosan fibers for textile industry from high-concentration solution prepared from composite solvent |
| CN103704908A (en) * | 2014-01-16 | 2014-04-09 | 青岛海百合生物技术有限公司 | Fine-particle-proof mask with chitosan and nano-zinc oxide and manufacturing method of fine-particle-proof mask |
| CN105999338A (en) * | 2016-05-19 | 2016-10-12 | 常州佳得顺抗菌材料科技有限公司 | Air disinfecting filter element material and preparation method thereof |
| CN107335286A (en) * | 2017-08-08 | 2017-11-10 | 成都漆彩之星环保科技有限公司 | A kind of composite air filter cotton |
| CN106008726B (en) * | 2016-05-19 | 2019-06-18 | 常州佳得顺抗菌材料科技有限公司 | High poly- iodine of starch and its preparation method and application |
| CN111535033A (en) * | 2020-04-30 | 2020-08-14 | 江阴苏达汇诚复合材料有限公司 | Preparation method and application of iodine-based antimicrobial microporous fiber material |
| WO2022120561A1 (en) * | 2020-12-08 | 2022-06-16 | 深圳先进技术研究院 | Water-soluble gel membrane having virus enrichment function, and preparation method therefor and application thereof |
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- 2003-06-12 CN CN03131867.3A patent/CN1224317C/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102888672A (en) * | 2011-07-20 | 2013-01-23 | 李永兴 | Method for preparing chitosan fibers for textile industry from high-concentration solution prepared from composite solvent |
| CN103704908A (en) * | 2014-01-16 | 2014-04-09 | 青岛海百合生物技术有限公司 | Fine-particle-proof mask with chitosan and nano-zinc oxide and manufacturing method of fine-particle-proof mask |
| CN103704908B (en) * | 2014-01-16 | 2015-09-16 | 青岛海百合生物技术有限公司 | Anti-fine particle mouth mask of a kind of chitosan-containing and nano zine oxide and preparation method thereof |
| CN105999338A (en) * | 2016-05-19 | 2016-10-12 | 常州佳得顺抗菌材料科技有限公司 | Air disinfecting filter element material and preparation method thereof |
| CN105999338B (en) * | 2016-05-19 | 2018-11-23 | 常州佳得顺抗菌材料科技有限公司 | A kind of air sterillization material for core and preparation method thereof |
| CN106008726B (en) * | 2016-05-19 | 2019-06-18 | 常州佳得顺抗菌材料科技有限公司 | High poly- iodine of starch and its preparation method and application |
| CN107335286A (en) * | 2017-08-08 | 2017-11-10 | 成都漆彩之星环保科技有限公司 | A kind of composite air filter cotton |
| CN111535033A (en) * | 2020-04-30 | 2020-08-14 | 江阴苏达汇诚复合材料有限公司 | Preparation method and application of iodine-based antimicrobial microporous fiber material |
| CN111535033B (en) * | 2020-04-30 | 2023-06-23 | 江阴苏达汇诚复合材料有限公司 | Preparation method and application of iodine antimicrobial microporous fiber material |
| WO2022120561A1 (en) * | 2020-12-08 | 2022-06-16 | 深圳先进技术研究院 | Water-soluble gel membrane having virus enrichment function, and preparation method therefor and application thereof |
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