CN1387763A - Composite nano germicide and its prepn - Google Patents
Composite nano germicide and its prepn Download PDFInfo
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Abstract
The present invention relates to nano scale composite antibacterial agent and its preparation method, it is characterized in that during the preparation of nano scale zinc oxide, water soluble metallic salt is added, and uses organic modifier to proceed modification, and passes through the processes of coprecipitation, washing, drying, calcination etc. to obtain the nano grade antibacterial agent. The invented nano composite antibacterial agent is excellent in anti bacterial performance and possesses the advantages of fast, high effect, broad spectrum, durable, no resistance to chemical agent etc.
Description
One, technical field:
Composite nano germicide disclosed by the invention and preparation method thereof, the metal nanometer material technical field is specifically related to a kind of composite nano germicide based on nano zine oxide and preparation method thereof.
Two, background technology
As everyone knows, noxious bacteria is human disease and unhealthful key factor.Therefore, how to eliminate and suppress noxious bacteria, be found from bacterium since one of the emphasis of various countries' scientists study.Along with the continuous development of science and technology, various anti-biotic materials emerge in an endless stream, and substantially can be divided into inorganic antiseptic and organic antibacterial agent, and traditional inorganic antiseptic is poisonous mostly or be corrosive, and poor stability, have limited the use of inorganic antiseptic.Organic antibacterial agent because of its efficiently fast sterilization idiocratic obtain market favor, in industries such as food production, medical environment, breed, use in a large number.But also more and more higher to the degree of concern of health along with people's living standard improves constantly, green and environmental protection becomes focus, recognizes that a large amount of use organic antibacterial agents have certain harm to human body and environment, and its consumption begins to be restricted; Simultaneously, market constantly enlarges the demand field of anti-biotic material, products such as fiber, plastics, pottery, glass, coating, rubber have been proposed antibiotic requirement, and organic antibacterial agent can not satisfy market demands because of himself characteristics poor chemical stability, poor heat resistance.In recent years, inorganic new material development is rapid, and the especially appearance of nano material is for the rise of inorganic antiseptic is taken a firm foundation.The nano inorganic antimicrobial agent report is a lot, be to go up loaded with nano level silver, zinc, copper, rare earth element etc. mostly at inorganic carrier material (as molecular sieve, imvite, calcium carbonate etc.), its shortcoming is that carrier material does not have antibiotic property, and antibiotic effective ingredient is few, and the antibacterial agent consumption is big; In patent CN1341358A, disclose a kind of by water-based amino acid silver, amino-acid zinc with and decompose the nanometer metallic silver that generates, nano zine oxide antibacterial agent as material of main part.The present invention is with its difference: 1, the preparation method is different, and the present invention prepares on patent ZL98 1 16820.5 bases; 2, use the material difference, outside desilver, the zinc, the present invention has used copper, titanium, calcium, rare earth metal salt, organic modifiers etc.; 3, the present invention is inorganic and organic compound.
The present invention chooses nano zine oxide as main body in numerous anti-biotic materials, according to different environments for use and requirement, technology of preparing by patent ZL98 1 16820.5, in its preparation process, the silver that adds different proportion, copper, calcium, titanium, the water soluble salt of rare earth metal, organic modifiers etc., make itself and nano zine oxide form intermolecular the combination, this antibacterial agent has overcome the part shortcoming of traditional inorganic antiseptic, have nontoxic, fast, long-acting, wide spectrum, do not produce drug resistance, its excellent warm tolerance particularly, chemical stability, by at fiber, plastics, pottery, on probation in the paint field, antibacterial effect is good.
Silver, copper, zinc are as traditional inorganic antibacterial material, when contacting with bacterium, metal ion slowly releases, because metal ion tool oxidation-reduction quality, and can react with organic matter (thio group, carboxyl, hydroxyl), can combine with bacterial cell membrane and memebrane protein, destroy its structure, enter the enzyme that destroys electron transport system behind the cell and with the DNA reaction, reach the sterilization purpose.Composite nano germicide of the present invention except that having inorganic antibacterial effects such as conventional silver, copper, zinc, rare earth element, because particle diameter reaches nanoscale, has nano particle distinctive 1) small-size effect; 2) surface interface effect; 3) quantum size effect; The composite nano germicide that the present invention sets forth is not the stack of several inorganic antibacterial material antimicrbial powers, because zinc oxide combines on molecular level with other elements, has extremely strong synergistic effect.The photocatalysis characteristic of nano zine oxide improves its sterilizing ability and efficient for other surface atoms provide more energy greatly.Combine with a small amount of organic modifiers again on this basis, make it have organic antibacterial agent characteristics rapidly and efficiently, these all embody the anti-microbial property and the effect of this antibacterial agent excellence.
Three, summary of the invention
The objective of the invention is provides a kind of composite nano germicide and preparation method thereof to society, for contribution is done some in the life that improves people.
Technical scheme of the present invention comprises this receive the technical scheme of complex antimicrobials and the technical scheme that its system each side goes.
This composite nano germicide of the present invention, be based on nano zine oxide, technology of preparing by patent ZL98 1 16820.5, adopt the process of a whole set of preparation nanoscale complex antimicrobials, according to different environments for use and requirement, in preparation process, add different slaine, organic modifiers,, be prepared into the nano-complex antibacterial agent by chemical coprecipitation, filtration, washing, drying, calcining system process and operational procedure.Technical characterstic is: this composite nano germicide is based on nano zine oxide, the composite components that adds in its preparation process comprises: at least a in the water soluble salt of silver, copper, calcium, titanium, rare earth lanthanum, cerium, rubidium, thorium, or adding at least a in the cationic surfactant, glutaraldehyde, non-ionic surface active agent of organic modifiers, the each component ratio prescription of this composite nano germicide is: nano zine oxide: at least a composite components=40-99.99%: 0.01-60%.Each component ratio summation must satisfy 100% (percentage by weight).
Aforesaid composite nano germicide, the detailed technology main points have: the water soluble salt of a, the silver that is added, copper, calcium, titanium, rare earth lanthanum, cerium, rubidium, thorium can be their sulphate, nitrate, hydrochloride, phosphate, carbonate, the amino-acid salt of organic acid salt, soap, acetate, benzoate etc.B, the organic modifiers that is added are: glutaraldehyde, cationic quaternary ammonium salt, cation imidazoline, AEO9, the AEO10 of non-ionic surface active agent, TX-10.Can add in c, the described composite nano germicide at least a, 13 kinds of slaines and organic modifiers at the most.
The preparation method of this composite nano germicide, it is the process of a whole set of preparation composite nano germicide, according to different environments for use and requirement, in the nano zine oxide preparation process, add different metallic salts, organic modifiers, through chemical coprecipitation, filter, washing, dry, the technological operation rules of calcining, make composite nano germicide, technical characterstic is: a, this composite nano germicide is main component with nano zine oxide, can add silver, copper, calcium, titanium, rare earth lanthanum, cerium, rubidium, the water soluble salt of thorium, the glutaraldehyde of organic modifiers, cation, at least a in the non-ionic surface active agent.The component formula rate of this composite nano germicide is: nano zine oxide: at least a composite components=40-99.99%: 0.01%-60%.Each component ratio summation must satisfy 100% (percentage by weight).The preparation method of b, this composite nano germicide: each component and deal are got all the ready by necessary requirement, earlier zinc oxide is made zinc ammonia complex liquid, compound adds deionized water respectively and is made into the aqueous solution, under stirring condition, each slaine compound water solution is added in the zinc ammonia complex liquid, solution temperature is controlled at 40-120 ℃, regulate pH value at 4-11, make it chemical coprecipitation, can add organic this property agent again, the technological operation rules of washing after filtration,, drying, calcining, make composite nano germicide, be up to the standards, preserve standby.
The preparation method of composite nano germicide as mentioned above, the detailed technology main points have: the water soluble salt of a, the silver that is added, copper, calcium, titanium, rare earth lanthanum, cerium, rubidium, thorium can be their sulphate, nitrate, hydrochloride, phosphate, carbonate, organic acid salt: amino-acid salt, soap, acetate, benzoate etc.B, the organic modifiers that is added are: cationic quaternary ammonium salt, cation imidazoline, glutaraldehyde, AEO9, the AEO10 of non-ionic surface active agent, TX-10.Can add in the raw material of c, described composite nano germicide at least a, 13 kinds of slaines and organic modifiers at the most.
Composite nano germicide of the present invention, except that having inorganic antibacterial effects such as conventional silver, copper, zinc, because particle diameter reaches nanoscale, it is distinctive to have a nano particle: 1) small-size effect; 2) surface interface effect; 3) quantum size effect; These all show the anti-microbial property and the effect of this antibacterial agent excellence.Be characterized in: 1, specific surface area is big, compares with traditional inorganic antiseptic, can significantly reduce consumption, and composite nano germicide is the 10%-20% of traditional inorganic antiseptic consumption.2, the surface atom quantity of nano particle is greatly more than traditional particle, and surface atom possesses very high-energy owing to lacking contiguous coordination atom, can strengthen the affinity of antibacterial agent and bacterium, improves the efficient of sterilization.3, for zinc oxide, the nanoscale particle diameter can improve photocatalytic effect greatly, under illumination condition, produce electron transition, and, produce electronics and hole at ion surface with the energy transmission, when water in the environment contacts with oxygen, generate negative oxygen ion and OH ion, negative oxygen ion has very strong sterilizing power, and the OH ion can react with most of organic matters, impel its decomposition, can strengthen sterilizing power.Be used for the ceramic coating industry, can make its product have self-cleaning power.4, the composite nano germicide of the present invention's elaboration is not the stack of several inorganic antibacterial material antimicrbial powers, because nano zine oxide combines on molecular level with other elements, has extremely strong synergistic effect.The photocatalysis characteristic of nano zine oxide improves its sterilizing ability and efficient for other surface atoms provide more energy greatly.Combine with a small amount of organic modifiers again on this basis, make it have organic antibacterial agent characteristics rapidly and efficiently, the harm of having avoided a large amount of use organic antibacterial agents to bring simultaneously.The preparation method of this nano-complex antibacterial agent is easy, easy to operate, has advance, practicality and remarkable economical and social effect, is worth using and promoting.
Four: description of drawings
Fig. 1 is a composite nano germicide preparation technology method flow block diagram.
In Fig. 1: 1, organic modifiers; 2, aqueous metal salt; 3, zinc ammonia complex liquid; 4, heated and stirred is mixed; 5, regulate the pH value chemical coprecipitation; 6, filter; 7, washing; 8, drying; 9, calcining; 10, check.
Five, concrete implementing method:
Embodiment one composite nano germicide and preparation method thereof:
1, this routine composite nano germicide, its each component ratio is: zinc oxide: copper carbonate: silver chlorate: cerous sulfate: calcium phosphate: titanium sulfate: cation imidazoline=85%: 0.1%: 1%: 1%: 9%: 1.9%: 2%, (percentage by weight), each component ratio summation is 100%.
2, the preparation method of this routine composite nano germicide: 85% zinc oxide is required preparation zinc ammonia complex liquid according to patent ZL98 1 16820.5, add 0.1% copper carbonate, 1% silver chlorate, 1% cerous sulfate, 9% calcium phosphate, 1.9% titanium sulfate in order respectively, solution is heated to 40 ℃, chemical coprecipitation when PH=8.5, add 2% cation imidazoline solutions, after filtration, washing, dry, calcining make finished product, adds in plastic products, antibacterial effect is fine.24 hours to staphylococcus aureus killing rate 100%
Embodiment two composite nano germicides and preparation method thereof:
1, this routine composite nano germicide, its each component ratio is: zinc oxide: copper acetate: silver nitrate: normal thorium sulfate: lanthanum nitrate: glutaraldehyde: non-ionic surface active agent AEO9=55%: 15%: 12%: 10%: 2%: 3%: 3%, (percentage by weight), each component ratio summation is 100%.
2, the preparation method of this routine composite nano germicide: 55% zinc oxide is required preparation zinc ammonia complex liquid according to patent ZL981 16820.5, be sequentially added into 15% copper acetate, 12% silver nitrate, 10% normal thorium sulfate, 2% lanthanum nitrate, 3% non-ionic surface active agent AEO9, solution is heated to 98 ℃, chemical coprecipitation when PH=4, add 3% glutaraldehyde, after filtration, washing, dry, calcining make finished product, adds in being coated with material products, antibacterial effect is fine.1 hour to staphylococcus aureus killing rate 100%.
Embodiment three composite nano germicides and preparation method thereof:
1, this routine composite nano germicide, its each component ratio is: zinc oxide: copper sulphate: silver nitrate: cerous sulfate: lanthanum chloride: cationic quaternary ammonium salt=55%: 15%: 15%: 10%: 2%: 3%, (percentage by weight), each component ratio summation is 100%.
2, the preparation method of this routine composite nano germicide: 55% zinc oxide is required preparation solution according to patent ZL98 1 16820.5, be sequentially added into 15% copper carbonate, 15% silver nitrate, 10% cerous sulfate, 2% lanthanum chloride, solution is heated to 75 ℃, chemical coprecipitation when PH=7, add 3% cationic quaternary ammonium salt, washing after filtration,, drying, calcining make finished product, add in textile fabrics and try out, antibacterial effect is fine.3 hours to staphylococcus aureus killing rate 100%.
Embodiment four composite nano germicides and preparation method thereof:
1, this routine composite nano germicide, its each component ratio is: zinc oxide: copper sulphate or glutaraldehyde=99.99%: 0.01%, (percentage by weight), each component ratio summation is 100%.
2, the preparation method of this routine composite nano germicide: 99.99% zinc oxide is required preparation solution according to patent ZL98 1 16820.5, be sequentially added into 0.01 copper carbonate or glutaraldehyde, solution is heated to 120 ℃, chemical coprecipitation when PH=11, washing after filtration,, drying, calcining make finished product, add in textile fabrics and try out, antibacterial effect is fine.5 hours to staphylococcus aureus killing rate 100%.
Embodiment five composite nano germicides and preparation method thereof:
1, this routine composite nano germicide, its each component ratio is: zinc oxide: calcium carbonate: copper sulphate: silver nitrate: normal thorium sulfate: cerous sulfate: lanthanum nitrate: titanium sulfate: thorium nitrate: cationic quaternary ammonium salt: cation imidazoline: glutaraldehyde: non-ionic surface active agent AEO9: TX-10=40%: 5%: 10%: 12%: 2%: 3%: 2%: 10%: 3%: 3%: 2%: 2%: 3%: 3%, (percentage by weight), each component ratio summation is 100%.
2, the preparation method of the composite nano germicide that this is routine: 40% zinc oxide is required preparation solution according to patent ZL98 1 16820.5, be sequentially added into 5% calcium carbonate, 10% copper sulphate, 12% silver nitrate, 2% normal thorium sulfate, 3% cerous sulfate, 2% lanthanum nitrate, 10% titanium sulfate, 3% thorium nitrate, solution is heated to 60 ℃, chemical coprecipitation when PH=6, add 3% cationic quaternary ammonium salt, 2% cation imidazoline, 2% glutaraldehyde, 3% non-ionic surface active agent AEO9,3% non-ionic surface active agent TX-10, after filtration, washing, dry, calcining makes finished product, add in being coated with material products, antibacterial effect is fine.0.5 hour to staphylococcus aureus killing rate 100%.
Claims (4)
1, a kind of composite nano germicide, it is based on nano zine oxide, adopted the process of a whole set of preparation nanoscale complex antimicrobials, according to different environments for use and requirement, in the nano zine oxide preparation process, add different metallic salts, organic modifiers, pass through chemical coprecipitation, filter, washing, dry, process and operational procedures such as calcining, be prepared into composite nano germicide, be characterised in that: this composite nano germicide is based on nano zine oxide, addible composite components comprises: silver, copper, calcium, titanium, rare earth lanthanum, cerium, rubidium, at least a in the water soluble salt of thorium, or the glutaraldehyde of interpolation organic modifiers, cation, at least a in the non-ionic surface active agent, the each component ratio prescription of this composite nano germicide is: nano zine oxide: at least a composite components=40-99.99% of interpolation: 0.01-60%, the summation of each component ratio must satisfy 100% (percentage by weight).
2, a kind of preparation method of composite nano germicide, it is the process of a whole set of preparation composite nano germicide, it is based on nano zine oxide, according to different environments for use and requirement, in the nano zine oxide preparation process, add different metallic salt, organic modifiers, through the technological operation rules of chemical coprecipitation, filtration, washing, drying, calcining, make composite nano germicide, be characterised in that:
The material component of a, this composite nano germicide is based on nano zine oxide, can add in the water soluble salt of silver, copper, calcium, titanium, rare earth lanthanum, cerium, rubidium, thorium at least a, or add in the glutaraldehyde, cation, non-ionic surface active agent of organic modifiers at least a, the each component ratio prescription of this composite nano germicide is: nano zine oxide: at least a composite components=40-99.99%: 0.01-60%, and the summation of each component ratio must satisfy 100% (percentage by weight);
The preparation method of b, this composite nano germicide: on request each material component is got all the ready, earlier zinc oxide is made zinc ammonia complex liquid, other slaines are made into the aqueous solution respectively, and each aqueous metal salt is added in the zinc ammonia complex liquid, solution temperature is controlled at 40-120 ℃, regulate pH value at 4-11, make it chemical coprecipitation, add the organic modifiers composite components again, the technological operation rules of washing after filtration,, drying, calcining, make composite nano germicide, be up to the standards, preserve standby.
3, composite nano germicide according to claim 1 is characterised in that:
A. the water soluble salt of the silver that is added, copper, calcium, titanium, rare earth lanthanum, cerium, rubidium, thorium can be their sulphate, nitrate, hydrochloride, phosphate, carbonate, organic acid salt;
B. the organic modifiers that is added can be: cationic quaternary ammonium salt, cation imidazoline, glutaraldehyde, the AEO9 of non-ionic surface active agent, AEO10, TX-10.
4, the preparation method of composite nano germicide according to claim 2 is characterised in that:
A. the water soluble salt of the silver that is added, copper, calcium, titanium, rare earth lanthanum, cerium, rubidium, thorium can be their sulphate, nitrate, hydrochloride, phosphate, carbonate, organic acid salt;
B, the organic modifiers that is added can be: cationic quaternary ammonium salt, cation imidazoline, glutaraldehyde, the AEO9 of non-ionic surface active agent, AEO10, TX-10.
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| CNB2004100124161A CN100525629C (en) | 2002-06-12 | 2002-06-12 | Nano inorganic germicide and its preparation method |
| CN 02121247 CN1387763A (en) | 2002-06-12 | 2002-06-12 | Composite nano germicide and its prepn |
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| CN1296548C (en) * | 2004-03-30 | 2007-01-24 | 东华大学 | Nano functional finishing agent for textile, preparation method and application |
| CN1295965C (en) * | 2004-09-24 | 2007-01-24 | 复旦大学 | Inorganic mesoporous antiseptic material and its preparing method |
| CN101836660A (en) * | 2010-04-06 | 2010-09-22 | 青岛科技大学 | Preparation method of composite nano-antibacterial, as well as antibacterial NL latex and antibacterial TPI rubber |
| CN102511499A (en) * | 2011-10-27 | 2012-06-27 | 浙江金海环境技术股份有限公司 | Green ecological habitat antibacterial self-cleaning material |
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| CN106139932A (en) * | 2016-06-30 | 2016-11-23 | 安徽繁盛禽业有限公司 | A kind of load Ag-ZnO is antibacterial is strengthening ultra-fine eider down powder poly-vinylidene-fluoride composite film |
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| JP2017043559A (en) * | 2015-08-27 | 2017-03-02 | 住化エンバイロメンタルサイエンス株式会社 | Antibacterial agent composition |
| CN109892326A (en) * | 2019-03-25 | 2019-06-18 | 合肥工业大学 | Silver-colored ball antibacterial agent of composite Nano containing zinc of a kind of load and preparation method thereof |
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2002
- 2002-06-12 CN CNB2004100124161A patent/CN100525629C/en not_active Expired - Fee Related
- 2002-06-12 CN CN 02121247 patent/CN1387763A/en active Pending
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| CN1296548C (en) * | 2004-03-30 | 2007-01-24 | 东华大学 | Nano functional finishing agent for textile, preparation method and application |
| CN1295965C (en) * | 2004-09-24 | 2007-01-24 | 复旦大学 | Inorganic mesoporous antiseptic material and its preparing method |
| CN101836660A (en) * | 2010-04-06 | 2010-09-22 | 青岛科技大学 | Preparation method of composite nano-antibacterial, as well as antibacterial NL latex and antibacterial TPI rubber |
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Also Published As
| Publication number | Publication date |
|---|---|
| CN100525629C (en) | 2009-08-12 |
| CN1589630A (en) | 2005-03-09 |
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