CN102513544A - Method for preparing nanometer silver sol - Google Patents
Method for preparing nanometer silver sol Download PDFInfo
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- CN102513544A CN102513544A CN2011104146969A CN201110414696A CN102513544A CN 102513544 A CN102513544 A CN 102513544A CN 2011104146969 A CN2011104146969 A CN 2011104146969A CN 201110414696 A CN201110414696 A CN 201110414696A CN 102513544 A CN102513544 A CN 102513544A
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- sodium borohydride
- silver nitrate
- colloidal sol
- pdda
- nano silver
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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 the nano-functional material technical field; Refer in particular to a kind of method for preparing nano silver colloidal sol, the employing silver nitrate is a raw material, and polydiene propyl-dimethyl amine hydrochlorate (PDDA) is a dispersant; Sodium borohydride is a reducing agent, and room temperature preparation obtains the nano silver colloidal sol of stable and excellent dispersion.
Background technology
Nano Silver (30 ~ 80 nm) has the special natures that many macroscopic material did not have such as the skin effect, volume (small size) effect, quantum size effect, macro quanta tunnel effect of nano material, can be widely used in 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, like liquid phase chemical reduction method, microemulsion method, photo-induction inducing defecation by enema and suppository, the auxiliary reducing process of ultrasonic wave, electrochemical process etc.; Wherein the liquid phase chemical reduction method is because technology is simple, easy to operate, low for equipment requirements and be widely used; But the gained specific grain surface is big, belongs to thermodynamic unstable system, very easily reunites with forming larger-size aggregate; Organic protective agent (polyvinylpyrrolidone, polyvinyl alcohol, dodecyl sodium sulfate etc.) is commonly used makes the nano silver colloidal sol that the dispersant preparation all disperses, but reaction system generally all need heat; The present invention proposes a kind of novel dispersant polydiene propyl-dimethyl amine hydrochlorate, can obtain nano silver colloidal sol stable and that all disperse under the room temperature.
Summary of the invention
The objective of the invention is to the silver nitrate is that raw material, PDDA are that dispersant, sodium borohydride are reducing agent, prepares nano silver colloidal sol stable and that all disperse under the room temperature.
A kind of preparation method of nano silver colloidal sol raw materials usedly is: AgNO
3(analyzing pure), C
8H
16ClN (analyzing pure), NaBH
4(analyzing pure).
Preparation technology is:
(1) silver nitrate and PDDA are dissolved in respectively in the deionized water, are configured to the solution that concentration is respectively 0.9mmol/mL and 3.6mmol/mL, two kinds of solution stirring are mixed, the mol ratio of silver nitrate and PDDA is 1:4-12 in the control mixed solution;
(2) be that the proportional arrangement concentration of 1:3-6 is the sodium borohydride aqueous solution of 3.6mmol/mL by silver nitrate and sodium borohydride mol ratio; Under strong agitation, mixed liquor is added dropwise to sodium borohydride reduction liquid, react 30-60min under the room temperature, obtain nano silver colloidal sol.
Silver nitrate and PDDA mol ratio are that 1:6-8 is good in the step 1;
Silver nitrate and sodium borohydride mol ratio are that 1:3-4 is good in the step 3.
Advantage of the present invention is to utilize PDDA to be dispersant, prepares nano silver colloidal sol stable and that all disperse under the room temperature, and this method program is simple, easy operating.
Description of drawings
Fig. 1
The TEM photo of instance 1 gained nano silver colloidal sol;
The TEM photo of Fig. 2 instance 2 gained nano silver colloidal sols;
The TEM photo of Fig. 3 instance 3 gained nano silver colloidal sols;
The TEM photo of Fig. 4 instance 4 gained nano silver colloidal sols;
The TEM photo of Fig. 5 instance 5 gained nano silver colloidal sols.
The specific embodiment
Embodiment 1
At first silver nitrate and PDDA are dissolved in respectively in the deionized water for 1:4 in molar ratio, being configured to 10mL concentration is that 0.9mmol/mL silver nitrate aqueous solution and 10mL concentration are the PDDA aqueous solution of 3.6mmol/mL; Be that the ratio of 1:6 is dissolved in sodium borohydride in the deionized water in silver nitrate and sodium borohydride mol ratio then, configuration 15mL concentration is the reducing solution of 3.6mmol/mL; Under magnetic agitation, silver nitrate/PDDA mixed liquor is added dropwise in the sodium borohydride reduction liquid, react 30min under the room temperature, obtain nano silver colloidal sol.
Embodiment 2
At first silver nitrate and PDDA are dissolved in respectively in the deionized water for 1:8 in molar ratio, being configured to 10mL concentration is that 0.9mmol/mL silver nitrate aqueous solution and 20mL concentration are the PDDA aqueous solution of 3.6mmol/mL; Be that the ratio of 1:4 is dissolved in sodium borohydride in the deionized water in silver nitrate and sodium borohydride mol ratio then, configuration 10mL concentration is the reducing solution of 3.6mmol/mL; Under magnetic agitation, silver nitrate/PDDA mixed liquor is added dropwise in the sodium borohydride reduction liquid, react 30min under the room temperature, obtain nano silver colloidal sol.
Embodiment 3
At first silver nitrate and PDDA are dissolved in respectively in the deionized water for 1:6 in molar ratio, being configured to 10mL concentration is that 0.9mmol/mL silver nitrate aqueous solution and 15mL concentration are the PDDA aqueous solution of 3.6mmol/mL; Be that the ratio of 1:4 is dissolved in sodium borohydride in the deionized water in silver nitrate and sodium borohydride mol ratio then, configuration 10mL concentration is the reducing solution of 3.6mmol/mL; Under magnetic agitation, silver nitrate/PDDA mixed liquor is added dropwise in the sodium borohydride reduction liquid, react 40min under the room temperature, obtain nano silver colloidal sol.
Embodiment 4
At first silver nitrate and PDDA are dissolved in respectively in the deionized water for 1:8 in molar ratio, being configured to 10mL concentration is that 0.9mmol/mL silver nitrate aqueous solution and 20mL concentration are the PDDA aqueous solution of 3.6mmol/mL; Be that the ratio of 1:3 is dissolved in sodium borohydride in the deionized water in silver nitrate and sodium borohydride mol ratio then, configuration 7.5mL concentration is the reducing solution of 3.6mmol/mL; Under magnetic agitation, silver nitrate/PDDA mixed liquor is added dropwise in the sodium borohydride reduction liquid, react 40min under the room temperature, obtain nano silver colloidal sol.
Embodiment 5
At first silver nitrate and PDDA are dissolved in respectively in the deionized water for 1:12 in molar ratio, being configured to 10mL concentration is that 0.9mmol/mL silver nitrate aqueous solution and 30mL concentration are the PDDA aqueous solution of 3.6mmol/mL; Be that the ratio of 1:4 is dissolved in sodium borohydride in the deionized water in silver nitrate and sodium borohydride mol ratio then, configuration 10mL concentration is the reducing solution of 3.6mmol/mL; Under magnetic agitation, silver nitrate/PDDA mixed liquor is added dropwise in the sodium borohydride reduction liquid, react 30min under the room temperature, obtain nano silver colloidal sol.
Claims (4)
1. method for preparing nano silver colloidal sol, it is characterized in that: the employing silver nitrate is a raw material, and polydiene propyl-dimethyl amine hydrochlorate is a dispersant, and sodium borohydride is a reducing agent, and room temperature preparation obtains stable and finely dispersed nano silver colloidal sol.
2. a kind of method for preparing nano silver colloidal sol as claimed in claim 1 is characterized in that comprising the steps:
(1) silver nitrate and PDDA are dissolved in respectively in the deionized water, are configured to the solution that concentration is respectively 0.9mmol/mL and 3.6mmol/mL, two kinds of solution stirring are mixed, the mol ratio of silver nitrate and PDDA is 1:4-12 in the control mixed solution;
(2) be that the proportional arrangement concentration of 1:3-6 is the sodium borohydride aqueous solution of 3.6mmol/mL by silver nitrate and sodium borohydride mol ratio; Under strong agitation, mixed liquor is added dropwise to sodium borohydride reduction liquid, react 30-60min under the room temperature, obtain nano silver colloidal sol.
3. a kind of method for preparing nano silver colloidal sol as claimed in claim 2 is characterized in that: silver nitrate and PDDA mol ratio are 1:6-8 in the step 1.
4. a kind of method for preparing nano silver colloidal sol as claimed in claim 2 is characterized in that: silver nitrate and sodium borohydride mol ratio are 1:3-4 in the step 3.
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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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| CN102513544B CN102513544B (en) | 2014-04-09 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103722181A (en) * | 2014-01-21 | 2014-04-16 | 江苏欧耐尔新型材料有限公司 | Method for preparing nano silver powder by using dispersing agent through liquid-phase reduction method |
| 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 |
| CN110299222A (en) * | 2019-07-29 | 2019-10-01 | 中国工程物理研究院应用电子学研究所 | A kind of visible 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 |
| CN111922359A (en) * | 2020-10-19 | 2020-11-13 | 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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| 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 |
| 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 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103722181A (en) * | 2014-01-21 | 2014-04-16 | 江苏欧耐尔新型材料有限公司 | Method for preparing nano silver powder by using dispersing agent through liquid-phase reduction method |
| 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 |
| CN110299222A (en) * | 2019-07-29 | 2019-10-01 | 中国工程物理研究院应用电子学研究所 | A kind of visible 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 |
| CN111922359A (en) * | 2020-10-19 | 2020-11-13 | 西安宏星电子浆料科技股份有限公司 | Preparation method of pure silver nanowires |
| 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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| CN102513544B (en) | 2014-04-09 |
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