CN100519015C - Chemical reduction process of preparing silver powder - Google Patents
Chemical reduction process of preparing silver powder Download PDFInfo
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- CN100519015C CN100519015C CNB2006100276695A CN200610027669A CN100519015C CN 100519015 C CN100519015 C CN 100519015C CN B2006100276695 A CNB2006100276695 A CN B2006100276695A CN 200610027669 A CN200610027669 A CN 200610027669A CN 100519015 C CN100519015 C CN 100519015C
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Abstract
The chemical reduction process of preparing silver powder includes the following steps: adding silver oxide or silver carbonate as the precursor into pure water in high speed stirring at 2500-3000 rpm for 10-15 min, lowering the stirring speed to 500-800 rpm, adding reductant to react, filtering the resultant, washing and stoving to obtain silver powder. Compared with available technology, the present invention has the features of waste water with no nitrate radical and pH 6-9 and capable of being drained directly, and no waste gas pollution.
Description
Technical field
The present invention relates to a kind of preparation field of metal powder material, particularly a kind of free of contamination chemical reduction method prepares the technology of silver powder.
Background technology
The silver slurry is the most important material of electronics industry, development along with microelectric technique, the development of the precise treatment of printed circuit and electronic component, miniaturization and nanometer technology is made various conductive paste (paste, agent) with powder (especially aluminium powder), is widely used in the coating of printed wire.As the silver powder of conductive paste (paste, agent) filler, then be important key material, should be pure, thin again to its requirement, also want good dispersion, also to consider whether can cause environmental pollution problems simultaneously.
Along with developing rapidly of China's electronics industry, raw-material demands such as super fine silver powder will sharply be increased, only the market capacity of nano-silver powder is estimated just to reach 500,000 tons/year, and the trend that continues expansion is arranged.Yet because the super fine silver powder technology of preparing of China is started late, integral level is lower, still lacks the super fine silver powder manufacturing enterprise of the scale of going up so far.Produce the needed silver slurry of high-grade electronic component, the still main at present dependence on import of silver powder in the native land.Therefore, raw-material production domesticization as early as possible such as silver powder has become electronic component enterprise and has reduced production costs, improved one of key factor of export competitiveness.
The preparation of silver powder is presoma mostly with the silver nitrate at present, adopts chemistry or physical method to be prepared from, and contains a large amount of nitrate anions in the waste water of reaction back, brings very big difficulty for the processing of waste water.It is that reducing agent adopts chemical reduction method to make with hydrogen peroxide, benzaldehyde etc. that the researcher is also arranged, but their agents useful for same is often somewhat expensive, and has bigger toxicity, as the used reducing agent of U.S. Pat .Pat.4407674 and China Zhongnan Polytechnic Univ is benzaldehyde, have cyanide to produce in the system, not only operation is many, and the reaction process process control is loaded down with trivial details, and inclement condition in the preparation process, also can bring environmental pollution.
Summary of the invention
Purpose of the present invention is exactly a kind of technology that adopts chemical reduction method to prepare silver powder that provides for the weak point that overcomes above-mentioned prior art existence.
Purpose of the present invention can be achieved through the following technical solutions: a kind of technology that adopts chemical reduction method to prepare silver powder, it is characterized in that, this process using silver oxide or silver carbonate are predecessor, silver oxide or silver carbonate are added in the pure water of high-speed stirred, keep mixing speed 2500-3000 rev/min, 10～15 minutes time, mixing speed is reduced to 500-800 rev/min then, adding reducing agent again reacts, until reacting completely, products therefrom obtains silver powder after filtering, wash, drying.
Described reducing agent is a hydrazine hydrate.
Before the described reaction the preferred 2700-2800 of mixing speed rev/min, preferred 14～15 minutes of time, the preferred 600-700 of the mixing speed in the described course of reaction rev/min.
The reaction mol ratio of described silver oxide or silver carbonate and reducing agent is 1:2, reducing agent excessive by weight 5%.
Compared with prior art, characteristics of the present invention are: adopting silver oxide or silver carbonate is presoma, with the hydrazine hydrate is reducing agent, the gas-phase product of reaction is a nitrogen, can not produce exhaust emission, water is reaction medium, can not contain nitrate anion in the waste water after reaction finishes, the pH value can directly be discharged at 6-9.
The specific embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
Take by weighing silver oxide 2.480 gram and add in the pure water of high-speed stirred, kept 2800 rev/mins of mixing speeds 15 minutes, mixing speed is dropped to 600 rev/mins, add reducing agent hydrazine hydrate 2.104 grams and begin reaction.After reaction finishes, product is filtered, washs, dries the back obtain silver powder.Waste water after the reaction end is detected, and the pH value is 8, can directly discharge.
Embodiment 2
Take by weighing silver carbonate 3.360 gram and add in the pure water of high-speed stirred, kept 3000 rev/mins of mixing speeds 10 minutes, mixing speed is dropped to 800 rev/mins, add reducing agent hydrazine hydrate 2.104 grams and begin reaction.After reaction finishes, silver powder is filtered, washs, dries the back obtain silver powder.Waste water after the reaction end is detected, and the pH value is 7, can directly discharge.
Embodiment 3
Take by weighing silver oxide 2.480 gram and add in the pure water of high-speed stirred, kept 2500 rev/mins of mixing speeds 1 minute, mixing speed is dropped to 500 rev/mins, add reducing agent hydrazine hydrate 2.004 grams and begin reaction.After reaction finishes, product is filtered, washs, dries the back obtain silver powder.Waste water after the reaction end is detected, and the pH value is 6, can directly discharge.
Claims (3)
1. technology that adopts chemical reduction method to prepare silver powder, it is characterized in that, this process using silver oxide or silver carbonate are predecessor, silver oxide or silver carbonate are added in the pure water of high-speed stirred, keep mixing speed 2500-3000 rev/min, 10～15 minutes time, mixing speed is reduced to 500-800 rev/min then, add reducing agent again and react, until reacting completely, products therefrom obtains silver powder after filtering, wash, drying; Described reducing agent is a hydrazine hydrate.
2. a kind of technology that adopts chemical reduction method to prepare silver powder according to claim 1 is characterized in that, before the described reaction mixing speed 2700-2800 rev/min, 14～15 minutes time, the mixing speed 600-700 in the described course of reaction rev/min.
3. a kind of technology that adopts chemical reduction method to prepare silver powder according to claim 1 is characterized in that the reaction mol ratio of described silver oxide or silver carbonate and reducing agent is 1:2, reducing agent excessive by weight 5%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100276695A CN100519015C (en) | 2006-06-13 | 2006-06-13 | Chemical reduction process of preparing silver powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100276695A CN100519015C (en) | 2006-06-13 | 2006-06-13 | Chemical reduction process of preparing silver powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101088678A CN101088678A (en) | 2007-12-19 |
| CN100519015C true CN100519015C (en) | 2009-07-29 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100276695A Active CN100519015C (en) | 2006-06-13 | 2006-06-13 | Chemical reduction process of preparing silver powder |
Country Status (1)
| Country | Link |
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| CN (1) | CN100519015C (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101695757B (en) * | 2009-10-29 | 2011-10-05 | 彩虹集团公司 | Method for preparing aluminium powder with high tap density |
| CN102248176B (en) * | 2011-07-15 | 2012-08-22 | 云南铜业科技发展股份有限公司 | Preparation method of flake silver powder with low burning loss |
| CN105081343B (en) * | 2015-08-03 | 2017-08-25 | 佛山市顺德区百锐新电子材料有限公司 | A kind of manufacture method of conductive silver powder for touch-screen UV type laser engraving silver pastes |
| CN113399679A (en) * | 2021-05-08 | 2021-09-17 | 东方电气集团科学技术研究院有限公司 | Preparation method of high-tap aging-resistant superfine silver powder for electronic paste |
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2006
- 2006-06-13 CN CNB2006100276695A patent/CN100519015C/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN101088678A (en) | 2007-12-19 |
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