CN102101173A - Method for preparing novel large-scale oil-soluble nano silver - Google Patents
Method for preparing novel large-scale oil-soluble nano silver Download PDFInfo
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- CN102101173A CN102101173A CN2009102004519A CN200910200451A CN102101173A CN 102101173 A CN102101173 A CN 102101173A CN 2009102004519 A CN2009102004519 A CN 2009102004519A CN 200910200451 A CN200910200451 A CN 200910200451A CN 102101173 A CN102101173 A CN 102101173A
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Abstract
The invention discloses a method for preparing novel large-scale oil-soluble nano silver. The method comprises the following steps of: completely dissolving silver salt and an organic protective agent into a solvent; gradually heating the solution to 20 to 70 DEG C; after the temperature is stabilized, adding a reducing agent into a reaction system; reacting for 20 to 30 minutes continuously under stirring; gradually cooling; standing and centrifuging the cooled solution; and washing sequentially with ethanol, deionized water and acetone for multiple times repeatedly to obtain the stable nano silver. The method is simple in process, simple and convenient in operation, mild in reaction, short in reaction time, high in efficiency and suitable for large-scale production; the product has high properties; the grain diameter of the nano silver is less than 20 nm; the nano silver has high secondary dispersibility in various oil agents; preparation cost and energy consumption are low; no harmful waste is generated; and the modernized production requirements, namely 'green production, environmental friendliness and energy conservation' are met.
Description
Affiliated technical field
The present invention relates to a kind of oil solubility nanometer silvery Preparation Method, especially design good dispersion in a kind of preparation oil-based solvent, be fit to the preparation method of the oil solubility nanometer silver of large-scale production.
Background technology
Since the eighties in 20th century, nanosecond science and technology show application potential widely at aspects such as material, information, the energy, environment, life, military affairs, manufacturings, for 21 century hi-tech development and human living standard's raising bring huge opportunity, become 21 century countries in the world and seize the key strategy field of high-tech and global economy commanding elevation.
Nano Silver has shown the characteristic of many excellences as the monobasic in the nano material family.Outstanding electricity, optics, antibiotic and catalysis makes Nano Silver in electronics industry, anti-biotic material, fields such as organic catalysis and energy-conserving and environment-protective have obtained extensive approval.At present, the preparation method of preparation nano-silver powder has a lot, mainly contains chemical reduction method, electrolysis, mechanical milling method, gas phase vapor method, the auxilliary photograph of ray, hydrothermal crystallization combination method, plasma method.Disclose a kind of preparation method and its usage of reducing nano-silver by phosphate in the Chinese patent 200910043855.1, this method is to be reducing agent and solvent with the liquid phosphorus acid esters, adds to cooperate stabilizing agent.With macromolecule and little stabilizer molecule, add silver salt then ,-10～200 ℃ of reactions down, thus the molten or water-soluble nano silver colloid of preparation oil.Because reducing agent and solvent that this method adopts are one, thus when reaction control difficulty, the product cut size wider distribution, of low quality.The reaction temperature height of this method is difficult to guarantee the stability of Nano Silver, and monodispersity, and energy resource consumption is big.Chinese patent 200810046690.9 discloses a kind of preparation method of spherical nano-silver powder, it is characterized in that it comprises the steps: 1) spray pyrolysis: a. is silver nitrate and one of following three kinds: 1. magnesium nitrate, 2. nickel nitrate, 3. copper nitrate, soluble in waterly be mixed with the aqueous solution that concentration is 10～40wt.%, the mol ratio of silver ion and magnesium ion, nickel ion or copper ion is 0.05～1: 4 in the solution; Spray pyrolysis then; B. in the presence of dispersant and protective agent, add ultrasonic dispersion in the absolute ethyl alcohol, get mixture; 2) preparation of spherical nano-silver powder: a. is added drop-wise to acid solution in the mixture, and regulating the pH value is 3～5, must contain the suspension of spherical nano-silver powder; B. suction filtration, washing, drying obtain spherical nano-silver powder.This method processing step is many, and product cut size is big, and redispersible is poor, is difficult to satisfy the requirement of modern industry.
Summary of the invention
The present invention is directed to the problem that exists in the background technology, proposed a kind of raw material and be easy to get, process equipment is simple, and rapidly and efficiently, purity is higher, the method for the mass preparation high stable oil solubility nanometer silver of energy-conserving and environment-protective.This kind novel nano-copper preparation method is characterized in that: said method comprising the steps of:
A: silver salt and organic protective agent are dissolved in the solvent, are warming up to 20-70 ℃ gradually, behind the temperature stabilization reducing agent is added in the reaction system, continue afterwards after stirring reaction 20-30 minute, gradually cooling.
B: centrifugal behind the solution left standstill with cooling, then, can obtain stabilized nano silver with using ethanol and deionized water and acetone cyclic washing for several times successively.
A kind of preparation method of novel large-scale oil solubility nanometer silver is characterized in that: employed silver salt is a silver acetate among the present invention, silver nitrate, complex a kind of or several of silver such as silver sulfate or shitosan silver;
A kind of preparation method of novel large-scale oil solubility nanometer silver is characterized in that: employed reducing agent is a sodium borohydride among the present invention, hydrazine hydrate, inferior sodium phosphate, one or several in the vitamin C;
A kind of used reducing agent of preparation method of novel large-scale oil solubility nanometer silver, it is characterized in that: the reducing agent that is adopted and the mol ratio of mantoquita are 1-8: 1;
A kind of preparation method of novel large-scale oil solubility nanometer silver, it is characterized in that: employed protective agent can be 12～octadecanoid acid among the present invention, alkane alcohol, alkanethiol, neopelex, DTAC, softex kw, polyethylene glycol, polyvinylpyrrolidone (PVP), one or more in the protective agents such as polyvinyl alcohol;
A kind of described protective agent of preparation method of novel large-scale oil solubility nanometer silver, it is characterized in that: the protective agent that is adopted and the mol ratio of silver salt are 0.1～10: 1;
A kind of preparation method of novel large-scale oil solubility nanometer silver is characterized in that: employed solvent can be a deionized water among the present invention, ethanol, and ethylene glycol,, isopropyl alcohol, one or more in many alcohols solvents such as glycerine or diglycol;
A kind of oil solubility nanometer silver of novel large-scale preparation, it is characterized in that: the gained nano-silver powder can be used as additive and uses, can be antibiotic with the compound preparation of macromolecular material, the antibiotic plastic of conducting function, coating, fiber, rubber, adhesive also can be used as auxiliary agent and uses, preparation lubricating oil, etc.
Beneficial effect of the present invention:
1, this method does not need the protection and the ultrasonic device of inert gas, and it is convenient to implement, and technology is simple
2, this method reaction condition gentleness, the reaction time is short, and the efficient height is fit to large-scale production.
3, the oil solubility nanometer silver granuel footpath of this method preparation is little, narrowly distributing, and output is big, and stability is high,
4, this invented technology cost is low, does not have bazardous waste to produce, and energy resource consumption is few, meets the requirement of modernization " energy-conserving and environment-protective, green production ".
Description of drawings
The present invention is further described below in conjunction with drawings and Examples.
Fig. 1 is an oil solubility nanometer silver XRD test collection of illustrative plates, and Fig. 2 is the transmission electron microscope photo (TEM) of product oil solubility nanometer silver.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Example 1: the 0.01mol silver acetate is dissolved in the 100ml ethanol, adds 5ml oleic acid and 0.5g Macrogol 2000, stirring and dissolving is warming up to 50 degree.Slowly add the 10ml hydrazine hydrate solution, vigorous stirring, solution becomes buff gradually, and the generation of expression Nano Silver stops heating after 20 minutes.Centrifugal behind the solution left standstill with cooling, and use deionized water, ethanol and acetone cyclic washing promptly obtain the purity height more than three times, the stable good good Nano Silver of oil-soluble.
Example 2: the 0.01mol silver nitrate is dissolved in the 100ml diglycol, adds 0.5g softex kw and 0.8g polyvinyl alcohol 30g, be warming up to 100 degree.The 0.02mol inferior sodium phosphate is dissolved in the 50ml diglycol, slowly is added to vigorous stirring in the above-mentioned solution, solution becomes aubergine, and the expression Nano Silver generates, and stops heating after 20 minutes.Subsequent operation is with embodiment 1.
Example 3: in 0.01mol silver nitrate dissolving 100ml ethylene glycol, add 0.6g DTAC and 2g hexadecane, be warming up to 60 degree.The 0.01mol sodium borohydride is dissolved in the 50ml ethylene glycol, slowly is added to vigorous stirring in the above-mentioned solution, the solution turned yellow look, expression nanometer copper generates, and stops reaction after 20 minutes.Subsequent operation is with embodiment 1.
Claims (8)
1. the preparation method of a novel large-scale oil solubility nanometer silver is characterized in that: said method comprising the steps of:
A: silver salt and organic protective agent are dissolved in the solvent, are warming up to 20-70 ℃ gradually, behind the temperature stabilization reducing agent is added in the reaction system, continue afterwards after stirring reaction 20-30 minute, gradually cooling.
B: centrifugal behind the solution left standstill with cooling, then, can obtain stabilized nano silver with using ethanol and deionized water and acetone cyclic washing for several times successively.
2. according to the preparation method of claim item 1 described a kind of novel large-scale oil solubility nanometer silver, it is characterized in that: employed mantoquita is a silver acetate among the present invention, silver nitrate, one or several of the complex of silver such as silver sulfate or shitosan silver;
3. according to the preparation method of claim item 1 described a kind of novel large-scale oil solubility nanometer silver, it is characterized in that: employed reducing agent is a sodium borohydride among the present invention, hydrazine hydrate, inferior sodium phosphate, one or several in the vitamin C;
4. according to claim item 1 and 3 described reducing agents, it is characterized in that: the reducing agent that is adopted and the mol ratio of silver salt are 1-8: 1;
5. according to the preparation method of claim item 1 described a kind of novel large-scale oil solubility nanometer silver, it is characterized in that: employed protective agent can be 12～octadecanoid acid among the present invention, alkane alcohol, alkanethiol, neopelex, DTAC, softex kw, polyethylene glycol, polyvinylpyrrolidone (PVP), one or more in the protective agents such as polyvinyl alcohol;
6. according to claim item 1 and 5 described protective agents, it is characterized in that: the protective agent that is adopted and the mol ratio of silver salt are 0.1-10: 1;
7. according to the preparation method of claim item 1 described a kind of novel large-scale oil solubility nanometer silver, it is characterized in that: employed solvent can be a deionized water among the present invention, ethanol, ethylene glycol,, isopropyl alcohol, one or more in many alcohols solvents such as glycerine or diglycol;
8. according to claim item 1～7 described a kind of novel large-scale oil solubility nanometer silver, it is characterized in that: the gained nano-silver powder can be used as additive and uses, can be antibiotic with the compound preparation of macromolecular material, the antibiotic plastic of conducting function, coating, fiber, rubber, adhesive also can be used as auxiliary agent and uses, the lubricated wet goods of preparation.
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102310200A (en) * | 2011-08-24 | 2012-01-11 | 明基材料有限公司 | Nano silver particle forming method |
| CN102513543A (en) * | 2011-12-06 | 2012-06-27 | 上海工程技术大学 | Microwave heating reduction technology for preparing superfine silver powder |
| CN103042225A (en) * | 2012-11-05 | 2013-04-17 | 中科院广州化学有限公司 | Linear nano silver and preparation method and application thereof |
| CN103121100A (en) * | 2013-02-07 | 2013-05-29 | 东华大学 | A method for converting nano-silver particles covered by oleic acid to aqueous phase |
| CN104028775A (en) * | 2014-06-19 | 2014-09-10 | 中国航空工业集团公司北京航空材料研究院 | Preparation method for monodisperse uniform-particle-size silver nanoparticles |
| CN104530676A (en) * | 2014-12-11 | 2015-04-22 | 陈艳艳 | Preparation method of antibacterial plastic, antibacterial plastic and application thereof |
| CN104999091A (en) * | 2015-08-22 | 2015-10-28 | 钱景 | Nano-silver particles and preparation thereof |
| CN105478796A (en) * | 2015-12-23 | 2016-04-13 | 广东省微生物研究所 | Method for preparing nano-silver through tea tree essential oil and nano-silver solution prepared through method |
| CN105585850A (en) * | 2015-12-22 | 2016-05-18 | 杭州师范大学 | Ag quantum dot composited anti-static organic silicon rubber as well as preparation method and application thereof |
| CN108015299A (en) * | 2017-11-06 | 2018-05-11 | 珠海纳金科技有限公司 | Nano-Ag particles and preparation method thereof |
| CN108907228A (en) * | 2018-07-24 | 2018-11-30 | 郑州阿弗雷德化工科技有限公司 | Nano silver solution and its inexpensive synthetic method |
| CN109169706A (en) * | 2018-07-19 | 2019-01-11 | 大美泰康（天津）生态科技有限公司 | Complex antimicrobials and antibacterial bacteriostatic type multifunctional inorganic ecologic coating obtained |
| CN109197899A (en) * | 2017-07-05 | 2019-01-15 | 北京农学院 | A kind of novel liquid nano silver antibacterial agent and its preparation method and application |
| CN109235026A (en) * | 2018-08-23 | 2019-01-18 | 合肥普尔德医疗用品有限公司 | A kind of medical material preparation method based on antimicrobial nano silver chemical modification |
| CN109233300A (en) * | 2018-09-12 | 2019-01-18 | 深圳沐之方抗菌科技有限公司 | Preparation method, the preparation method of nano silver antimicrobials, antibiotic plastic and antibiotic plastic of nano silver antimicrobials |
| CN112273396A (en) * | 2019-07-24 | 2021-01-29 | 陈信行 | Nano silver solvent |
| CN113714508A (en) * | 2021-08-12 | 2021-11-30 | 深圳大学 | Nano silver and preparation method and application thereof |
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2009
- 2009-12-22 CN CN2009102004519A patent/CN102101173A/en active Pending
Cited By (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102310200A (en) * | 2011-08-24 | 2012-01-11 | 明基材料有限公司 | Nano silver particle forming method |
| CN102513543A (en) * | 2011-12-06 | 2012-06-27 | 上海工程技术大学 | Microwave heating reduction technology for preparing superfine silver powder |
| CN103042225A (en) * | 2012-11-05 | 2013-04-17 | 中科院广州化学有限公司 | Linear nano silver and preparation method and application thereof |
| CN103042225B (en) * | 2012-11-05 | 2015-05-13 | 中科院广州化学有限公司 | Linear nano silver and preparation method and application thereof |
| CN103121100A (en) * | 2013-02-07 | 2013-05-29 | 东华大学 | A method for converting nano-silver particles covered by oleic acid to aqueous phase |
| CN103121100B (en) * | 2013-02-07 | 2015-10-28 | 东华大学 | A kind of method of nano-Ag particles to aqueous phase shifting Coated with Oleic Acid |
| CN104028775A (en) * | 2014-06-19 | 2014-09-10 | 中国航空工业集团公司北京航空材料研究院 | Preparation method for monodisperse uniform-particle-size silver nanoparticles |
| CN104530676A (en) * | 2014-12-11 | 2015-04-22 | 陈艳艳 | Preparation method of antibacterial plastic, antibacterial plastic and application thereof |
| CN104999091A (en) * | 2015-08-22 | 2015-10-28 | 钱景 | Nano-silver particles and preparation thereof |
| CN105585850A (en) * | 2015-12-22 | 2016-05-18 | 杭州师范大学 | Ag quantum dot composited anti-static organic silicon rubber as well as preparation method and application thereof |
| CN105585850B (en) * | 2015-12-22 | 2019-03-05 | 杭州师范大学 | A kind of antistatic organic silicon rubber and the preparation method and application thereof that Ag quantum dot is compound |
| CN105478796A (en) * | 2015-12-23 | 2016-04-13 | 广东省微生物研究所 | Method for preparing nano-silver through tea tree essential oil and nano-silver solution prepared through method |
| CN105478796B (en) * | 2015-12-23 | 2018-01-05 | 广东省微生物研究所 | A kind of Nano silver solution for the method and its preparation that Nano Silver is prepared using tea tree ethereal oil |
| CN109197899A (en) * | 2017-07-05 | 2019-01-15 | 北京农学院 | A kind of novel liquid nano silver antibacterial agent and its preparation method and application |
| CN108015299A (en) * | 2017-11-06 | 2018-05-11 | 珠海纳金科技有限公司 | Nano-Ag particles and preparation method thereof |
| CN109169706A (en) * | 2018-07-19 | 2019-01-11 | 大美泰康（天津）生态科技有限公司 | Complex antimicrobials and antibacterial bacteriostatic type multifunctional inorganic ecologic coating obtained |
| CN108907228A (en) * | 2018-07-24 | 2018-11-30 | 郑州阿弗雷德化工科技有限公司 | Nano silver solution and its inexpensive synthetic method |
| CN109235026A (en) * | 2018-08-23 | 2019-01-18 | 合肥普尔德医疗用品有限公司 | A kind of medical material preparation method based on antimicrobial nano silver chemical modification |
| CN109233300A (en) * | 2018-09-12 | 2019-01-18 | 深圳沐之方抗菌科技有限公司 | Preparation method, the preparation method of nano silver antimicrobials, antibiotic plastic and antibiotic plastic of nano silver antimicrobials |
| CN109233300B (en) * | 2018-09-12 | 2021-03-16 | 深圳沐之方抗菌科技有限公司 | Preparation method of nano-silver antibacterial agent, antibacterial plastic and preparation method of antibacterial plastic |
| CN112273396A (en) * | 2019-07-24 | 2021-01-29 | 陈信行 | Nano silver solvent |
| CN113714508A (en) * | 2021-08-12 | 2021-11-30 | 深圳大学 | Nano silver and preparation method and application thereof |
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