CN102513544B - Method for preparing nanometer silver sol - Google Patents
Method for preparing nanometer silver sol Download PDFInfo
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- CN102513544B CN102513544B CN201110414696.9A CN201110414696A CN102513544B CN 102513544 B CN102513544 B CN 102513544B CN 201110414696 A CN201110414696 A CN 201110414696A CN 102513544 B CN102513544 B CN 102513544B
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- sodium borohydride
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Abstract
The invention belongs to the technical field of functional nanomaterials, and in particular relates to a method for preparing a nanometer silver sol. The method employs silver nitrate as a raw material, poly(diallyldimethylamine) hydrochloride (PDDA) as a dispersant and sodium borohydride as a reducing agent, to obtain the stable and well dispersed nanometer silver sol at room temperature. The method of the invention has the advantages of utilizing PDDA as the dispersant and obtaining the stable and well dispersed nanometer silver sol at room temperature. The method is simple in process and easy to operate.
Description
Technical field
The invention belongs to nano-functional material technical field, refer in particular to a kind of method of preparing nano silver colloidal sol, employing silver nitrate is raw material, and polydiene propyl-dimethyl amine hydrochlorate (PDDA) is dispersant, sodium borohydride is reducing agent, and room temperature prepares the nano silver colloidal sol of stable and excellent dispersion.
Background technology
Nano Silver (30 ~ 80 nm) has the special nature that many macroscopic material such as the skin effect, volume (small size) effect, quantum size effect, macro quanta tunnel effect of nano material do not have, and can be widely used in the fields such as bactericidal deodoring materials (anti-bacteria ceramic, preservative film, fabric etc.), catalyst material, modified electrode material, antistatic material, low temperature superconducting material, electric slurry, nonlinear optical material.
The preparation method of Nano Silver has a lot, as liquid phase chemical reduction method, microemulsion method, photo-induction inducing defecation by enema and suppository, ultrasonic wave assisted Reduction method, electrochemical process etc.; Wherein liquid phase chemical reduction method is because technique is simple, easy to operate, low for equipment requirements and be widely used; But gained specific grain surface is large, belong to thermodynamic unstable system, very easily reunite and form larger-size aggregate; Organic protective agent (polyvinylpyrrolidone, polyvinyl alcohol, dodecyl sodium sulfate etc.) is commonly used for the nano silver colloidal sol that dispersant is prepared Monodispersed, but reaction system generally all needs heating; The present invention proposes a kind of novel dispersant polydiene propyl-dimethyl amine hydrochlorate, can obtain the nano silver colloidal sol of stable and Monodispersed under room temperature.
Summary of the invention
The object of the invention is to take silver nitrate as raw material, PDDA are as dispersant, sodium borohydride are reducing agent, under room temperature, prepare the nano silver colloidal sol of stable and Monodispersed.
A preparation method for nano silver colloidal sol, is raw materials usedly: AgNO
3(analyzing pure), C
8h
16it is pure that ClN(analyzes), NaBH
4(analyzing pure).
Preparation technology is:
(1) silver nitrate and PDDA are dissolved in respectively in deionized water, are configured to the solution that concentration is respectively 0.9mmol/mL and 3.6mmol/mL, two kinds of solution are uniformly mixed, in control mixed solution, the mol ratio of silver nitrate and PDDA is 1:4-12;
(2) sodium borohydride aqueous solution that the proportional arrangement concentration that is 1:3-6 by silver nitrate and sodium borohydride mol ratio is 3.6mmol/mL; Under strong agitation, mixed liquor is added dropwise to sodium borohydride reduction liquid, under room temperature, react 30-60min, obtain nano silver colloidal sol.
In step 1, silver nitrate and PDDA mol ratio are that 1:6-8 is good;
In step 3, silver nitrate and sodium borohydride mol ratio are that 1:3-4 is good.
Advantage of the present invention is to utilize PDDA for dispersant, prepares the nano silver colloidal sol of stable and Monodispersed under room temperature, and this method program is simple, easy operating.
Accompanying drawing explanation
Fig. 1
?the TEM photo of example 1 gained nano silver colloidal sol;
The TEM photo of Fig. 2 example 2 gained nano silver colloidal sols;
The TEM photo of Fig. 3 example 3 gained nano silver colloidal sols;
The TEM photo of Fig. 4 example 4 gained nano silver colloidal sols;
The TEM photo of Fig. 5 example 5 gained nano silver colloidal sols.
The specific embodiment
embodiment 1
First silver nitrate and PDDA are dissolved in respectively in deionized water for 1:4 in molar ratio, being configured to 10mL concentration is the PDDA aqueous solution that 0.9mmol/mL silver nitrate aqueous solution and 10mL concentration are 3.6mmol/mL; Then the ratio that is 1:6 in silver nitrate and sodium borohydride mol ratio is dissolved in sodium borohydride in deionized water, the reducing solution that configuration 15mL concentration is 3.6mmol/mL; Under magnetic agitation, silver nitrate/PDDA mixed liquor is added dropwise in sodium borohydride reduction liquid, under room temperature, react 30min, obtain nano silver colloidal sol.
embodiment 2
First silver nitrate and PDDA are dissolved in respectively in deionized water for 1:8 in molar ratio, being configured to 10mL concentration is the PDDA aqueous solution that 0.9mmol/mL silver nitrate aqueous solution and 20mL concentration are 3.6mmol/mL; Then the ratio that is 1:4 in silver nitrate and sodium borohydride mol ratio is dissolved in sodium borohydride in deionized water, the reducing solution that configuration 10mL concentration is 3.6mmol/mL; Under magnetic agitation, silver nitrate/PDDA mixed liquor is added dropwise in sodium borohydride reduction liquid, under room temperature, react 30min, obtain nano silver colloidal sol.
embodiment 3
First silver nitrate and PDDA are dissolved in respectively in deionized water for 1:6 in molar ratio, being configured to 10mL concentration is the PDDA aqueous solution that 0.9mmol/mL silver nitrate aqueous solution and 15mL concentration are 3.6mmol/mL; Then the ratio that is 1:4 in silver nitrate and sodium borohydride mol ratio is dissolved in sodium borohydride in deionized water, the reducing solution that configuration 10mL concentration is 3.6mmol/mL; Under magnetic agitation, silver nitrate/PDDA mixed liquor is added dropwise in sodium borohydride reduction liquid, under room temperature, react 40min, obtain nano silver colloidal sol.
embodiment 4
First silver nitrate and PDDA are dissolved in respectively in deionized water for 1:8 in molar ratio, being configured to 10mL concentration is the PDDA aqueous solution that 0.9mmol/mL silver nitrate aqueous solution and 20mL concentration are 3.6mmol/mL; Then the ratio that is 1:3 in silver nitrate and sodium borohydride mol ratio is dissolved in sodium borohydride in deionized water, the reducing solution that configuration 7.5mL concentration is 3.6mmol/mL; Under magnetic agitation, silver nitrate/PDDA mixed liquor is added dropwise in sodium borohydride reduction liquid, under room temperature, react 40min, obtain nano silver colloidal sol.
embodiment 5
First silver nitrate and PDDA are dissolved in respectively in deionized water for 1:12 in molar ratio, being configured to 10mL concentration is the PDDA aqueous solution that 0.9mmol/mL silver nitrate aqueous solution and 30mL concentration are 3.6mmol/mL; Then the ratio that is 1:4 in silver nitrate and sodium borohydride mol ratio is dissolved in sodium borohydride in deionized water, the reducing solution that configuration 10mL concentration is 3.6mmol/mL; Under magnetic agitation, silver nitrate/PDDA mixed liquor is added dropwise in sodium borohydride reduction liquid, under room temperature, react 30min, obtain nano silver colloidal sol.
Claims (3)
1. a method of preparing nano silver colloidal sol, is characterized in that comprising the steps:
(1) silver nitrate and polydiene propyl-dimethyl amine hydrochlorate are dissolved in respectively in deionized water, be configured to the solution that concentration is respectively 0.9mmol/mL and 3.6mmol/mL, two kinds of solution are uniformly mixed, and in control mixed solution, the mol ratio of silver nitrate and polydiene propyl-dimethyl amine hydrochlorate is 1:4-12;
(2) sodium borohydride aqueous solution that the proportional arrangement concentration that is 1:3-6 by silver nitrate and sodium borohydride mol ratio is 3.6mmol/mL; Under strong agitation, mixed liquor is added dropwise to sodium borohydride reduction liquid, under room temperature, react 30-60min, obtain nano silver colloidal sol.
2. a kind of method of preparing nano silver colloidal sol as claimed in claim 1, is characterized in that: in step (1), silver nitrate and polydiene propyl-dimethyl amine hydrochlorate mol ratio are 1:6-8.
3. a kind of method of preparing nano silver colloidal sol as claimed in claim 1, is characterized in that: in step (2), silver nitrate and sodium borohydride mol ratio are 1:3-4.
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| CN201110414696.9A CN102513544B (en) | 2011-12-13 | 2011-12-13 | Method for preparing nanometer silver sol |
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| CN201110414696.9A CN102513544B (en) | 2011-12-13 | 2011-12-13 | Method for preparing nanometer silver sol |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103722181B (en) * | 2014-01-21 | 2016-01-20 | 江苏欧耐尔新型材料有限公司 | Liquid phase reduction uses dispersant to prepare the method for nano-silver powder |
| CN104490927A (en) * | 2014-12-12 | 2015-04-08 | 江苏大学 | Nano-silver composite material as well as preparation method and application thereof |
| CN108892393A (en) * | 2018-06-08 | 2018-11-27 | 安徽菲勒自动门制造有限公司 | A kind of automatically-controlled door disables the preparation method of high-strength antimicrobial textiles |
| CN110299222B (en) * | 2019-07-29 | 2020-09-18 | 中国工程物理研究院应用电子学研究所 | Visible light transparent conductive film and preparation method thereof |
| CN110438800A (en) * | 2019-08-01 | 2019-11-12 | 太仓市洪宇新材料科技有限公司 | It is a kind of with antistatic and antibacterial functions dacrons and preparation method thereof |
| CN111922359B (en) * | 2020-10-19 | 2021-01-05 | 西安宏星电子浆料科技股份有限公司 | Preparation method of pure silver nanowires |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101249566A (en) * | 2008-03-31 | 2008-08-27 | 中国科学院物理研究所 | Preparation method of monodisperse silver nano |
| CN101421032A (en) * | 2006-04-15 | 2009-04-29 | 拜尔技术服务有限责任公司 | Method for producing metal particles, metal particles produced thereby, and the use thereof |
| CN101716684A (en) * | 2009-12-18 | 2010-06-02 | 华南理工大学 | Highly dispersible spherical nano-silver powder and preparation method thereof |
| CN101731272A (en) * | 2009-12-24 | 2010-06-16 | 中国人民解放军军事医学科学院基础医学研究所 | Method for preparing antibacterial nanometer silver colloid |
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| KR20060132076A (en) * | 2005-06-17 | 2006-12-21 | 한국과학기술연구원 | Preparation method of nano-powder by chemical precipitation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101421032A (en) * | 2006-04-15 | 2009-04-29 | 拜尔技术服务有限责任公司 | Method for producing metal particles, metal particles produced thereby, and the use thereof |
| CN101249566A (en) * | 2008-03-31 | 2008-08-27 | 中国科学院物理研究所 | Preparation method of monodisperse silver nano |
| CN101716684A (en) * | 2009-12-18 | 2010-06-02 | 华南理工大学 | Highly dispersible spherical nano-silver powder and preparation method thereof |
| CN101731272A (en) * | 2009-12-24 | 2010-06-16 | 中国人民解放军军事医学科学院基础医学研究所 | Method for preparing antibacterial nanometer silver colloid |
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