CN101088679A - Prepn process of micro silver powder - Google Patents
Prepn process of micro silver powder Download PDFInfo
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- CN101088679A CN101088679A CN200710049490.4A CN200710049490A CN101088679A CN 101088679 A CN101088679 A CN 101088679A CN 200710049490 A CN200710049490 A CN 200710049490A CN 101088679 A CN101088679 A CN 101088679A
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Abstract
The chemical reaction process for preparing silver micropowder includes the following steps: dissolving silver nitrate in deionized water and diluting to 200 g/l concentration, adding 200-300 g/l concentration alkaline solution of NaOH, KOH, Na2CO3 or K2CO3 at 20-45 deg.c, adding organic reductant formic acid, formaldehyde, ethylene glycol or glycerin under low speed stirring at 50-85 rpm to produce silver micropowder of 5-10 micron size, filtering, washing, and stoving to obtain the silver micropowder product. The process has the advantages of simplicity, low production cost and controllability of the average silver micropowder size.
Description
Technical field
The invention belongs to a kind of method of utilizing chemical reaction to prepare silver material, particularly a kind of preparation method of micro silver powder.
Background technology
At present, the preparation method of nano-silver powder mainly contains physics method and chemical method.The physics method generally adopts vacuum evaporation one condensation method, vacuum sputtering and plasma sputtering method, has that equipment investment is big, productive rate is low, energy consumption is big and shortcoming such as cost height.Chemical method generally is to be raw material with the silver nitrate, adding ammoniacal liquor makes silver ion complexation form silver ammino ion to reduce the concentration of the silver ion in the solution, use hydrogen peroxide, hydrazine hydrate, triethanolamine, natrium citricum, ascorbic acid etc. silver to be precipitated out then as reducing agent, but the application of ammoniacal liquor makes the operating environment variation, the condition harshness easily produces quick-fried silver.
Summary of the invention
The purpose of this invention is to provide a kind of is raw material and do not use ammoniacal liquor to prepare the method for micro silver powder with the silver nitrate, and can obtain the micro silver powder of different average grain diameters by the different proportion of control reactant.
Purpose of the present invention realizes by following technical proposals:
The preparation method of micro silver powder, with the silver nitrate is that raw material through chemical reaction prepares micro silver powder, concrete steps are: earlier with silver nitrate with deionized water dissolving and be diluted to 200 grams per liters, be under 20～45 ℃ of conditions in temperature then, add alkaline matter in the above-mentioned liquor argenti nitratis ophthalmicus that makes, under the situation of stirring at low speed, pouring into organic reducing agent again, to generate average grain diameter be 5～10 microns micro silver powder, filter then, wash, dry, obtain finished product.
More specifically, described alkaline matter is NaOH, KOH, Na
2CO
3, K
2CO
3Any.
Described alkaline matter is that concentration is the solution of 200～300 grams per liters.
Described organic reducing agent can be any of formic acid, formaldehyde, ethylene glycol or glycerine.
The speed of described stirring at low speed is 50～85 rev/mins.
The temperature of described oven dry is 60～80 ℃.
Described alkaline matter adds in the liquor argenti nitratis ophthalmicus in two steps, earlier a part of alkaline matter is joined in the liquor argenti nitratis ophthalmicus, after adding organic reducing agent, more remaining alkaline matter is joined in the liquor argenti nitratis ophthalmicus that adds organic reducing agent, obtain the micro silver powder of different average grain diameters.
As embodiments of the present invention, described silver nitrate weight is 40 kilograms, adds in 200 liters of deionized waters to make liquor argenti nitratis ophthalmicus, and described alkaline matter is 15 kilograms of Na
2CO
3Add 60 liters of Na that deionized water makes
2CO
3Solution, described organic reducing agent are 15 liters and analyze pure formaldehyde, by following step operation, obtain the micro silver powder of different average grain diameters:
With Na
2CO
3Solution was added drop-wise in the liquor argenti nitratis ophthalmicus in 20～30 minutes fully, measured to analyze pure formaldehyde and be poured in the above-mentioned solution and react, and no longer rose up to temperature, treat that temperature descends 0.1 ℃, react completely, filter, washing is dried under 60 ℃ of conditions, obtains average grain diameter and be 5.21 microns micro silver powder;
Perhaps, with Na
2CO
390% of solution was added drop-wise in the liquor argenti nitratis ophthalmicus in 20～30 minutes, measured to analyze pure formaldehyde and be poured in the above-mentioned solution and react, and no longer rose up to temperature, treated that temperature descends 0.1 ℃, with Na
2CO
3Solution remaining 10% is poured in the above-mentioned solution again, no longer rises up to temperature, treats that temperature descends 0.1 ℃, reacts completely, and filters, and washing is dried under 70 ℃ of conditions, obtains average grain diameter and be 6.54 microns micro silver powder;
Perhaps, with Na
2CO
380% of solution was added drop-wise in the liquor argenti nitratis ophthalmicus in 20～30 minutes, measured to analyze pure formaldehyde and be poured in the above-mentioned solution and react, and no longer rose up to temperature, treated that temperature descends 0.1 ℃, with Na
2CO
3Solution remaining 20% is poured in the above-mentioned solution again, no longer rises up to temperature, treats that temperature descends 0.1 ℃, reacts completely, and filters, and washing is dried under 80 ℃ of conditions, obtains average grain diameter and be 7.48 microns micro silver powder;
Perhaps, with Na
2CO
370% of solution was added drop-wise in the liquor argenti nitratis ophthalmicus in 20～30 minutes, measured to analyze pure formaldehyde and be poured in the above-mentioned solution and react, and no longer rose up to temperature, treated that temperature descends 0.1 ℃, with Na
2CO
3Solution remaining 30% is poured in the above-mentioned solution again, no longer rises up to temperature, treats that temperature descends 0.1 ℃, reacts completely, and filters, and washing is dried under 80 ℃ of conditions, obtains average grain diameter and be 8.73 microns micro silver powder;
Perhaps, with Na
2CO
360% of solution was added drop-wise in the liquor argenti nitratis ophthalmicus in 20～30 minutes, measured to analyze pure formaldehyde and be poured in the above-mentioned solution and react, and no longer rose up to temperature, treated that temperature descends 0.1 ℃, with Na
2CO
3Solution remaining 40% is poured in the above-mentioned solution again, no longer rises up to temperature, treats that temperature descends 0.1 ℃, reacts completely, and filters, and washing is dried under 80 ℃ of conditions, obtains average grain diameter and be 9.66 microns micro silver powder.
The present invention is raw material with the silver nitrate, uses Na
2CO
3Produce transition metal salt Deng alkaline matter, directly topple over organic reducing agent with the preparation micro silver powder, have that technology is simple, production cost is low, under identical conditions, the controlled advantage of micro silver powder average grain diameter of gained, and owing to do not adopt ammoniacal liquor, operating environment is improved, be difficult for producing quick-fried silver as reactant.
The specific embodiment
Further specify the present invention below in conjunction with specific embodiment.
Embodiment 1: with making the liquor argenti nitratis ophthalmicus that concentration is 200 grams per liters in 200 liters of deionized waters of 40 kilograms of silver nitrates addings, with 15 kilograms of Na
2CO
3Add 60 liters of deionized waters and make the Na that concentration is 250 grams per liters
2CO
3Solution.
Then under 20～45 ℃ of temperature conditions, with Na
2CO
3Solution was added drop-wise in the liquor argenti nitratis ophthalmicus in 20～30 minutes fully, carry out the above-mentioned solution of stirring at low speed with 50 rev/mins speed, measuring 15 liters analyzes pure formaldehyde and is poured in the above-mentioned solution and reacts, no longer rise up to temperature, treat that temperature descends 0.1 ℃, reacts completely, filter, washing is dried under 60 ℃ of conditions, obtains average grain diameter and be 5.21 microns micro silver powder.
Embodiment 2: with making the liquor argenti nitratis ophthalmicus that concentration is 200 grams per liters in 200 liters of deionized waters of 40 kilograms of silver nitrates addings, with 15 kilograms of Na
2CO
3Add 60 liters of deionized waters and make the Na that concentration is 250 grams per liters
2CO
3Solution.
Then under 20～45 ℃ of temperature conditions, with Na
2CO
390% of solution was added drop-wise in the liquor argenti nitratis ophthalmicus in 20～30 minutes fully, carry out the above-mentioned solution of stirring at low speed with 60 rev/mins speed, measuring 15 liters analyzes pure formaldehyde and is poured in the above-mentioned solution and reacts, no longer rise up to temperature, treat that temperature descends 0.1 ℃, reacts completely, filter, washing is dried under 70 ℃ of conditions, obtains average grain diameter and be 6.54 microns micro silver powder.
Embodiment 3: with making the liquor argenti nitratis ophthalmicus that concentration is 200 grams per liters in 200 liters of deionized waters of 40 kilograms of silver nitrates addings, with 15 kilograms of Na
2CO
3Add 60 liters of deionized waters and make the Na that concentration is 250 grams per liters
2CO
3Solution.
Then under 20～45 ℃ of temperature conditions, with Na
2CO
380% of solution was added drop-wise in the liquor argenti nitratis ophthalmicus in 20～30 minutes, carried out the above-mentioned solution of stirring at low speed with 70 rev/mins speed, measured 15 liters and analyzed pure formaldehyde and be poured in the above-mentioned solution and react, and no longer rose up to temperature, treated that temperature descends 0.1 ℃, with Na
2CO
3Solution remaining 20% is poured in the above-mentioned solution again, no longer rises up to temperature, treats that temperature descends 0.1 ℃, reacts completely, and filters, and washing is dried under 80 ℃ of conditions, obtains average grain diameter and be 7.48 microns micro silver powder.
Embodiment 4: with making the liquor argenti nitratis ophthalmicus that concentration is 200 grams per liters in 200 liters of deionized waters of 40 kilograms of silver nitrates addings, with 15 kilograms of Na
2CO
3Add 60 liters of deionized waters and make the Na that concentration is 250 grams per liters
2CO
3Solution.
Under 20～45 ℃ of temperature conditions, with Na
2CO
370% of solution was added drop-wise in the liquor argenti nitratis ophthalmicus in 20～30 minutes, carried out the above-mentioned solution of stirring at low speed with 75 rev/mins speed, measured 15 liters and analyzed pure formaldehyde and be poured in the above-mentioned solution and react, and no longer rose up to temperature, treated that temperature descends 0.1 ℃, with Na
2CO
3Solution remaining 30% is poured in the above-mentioned solution again, no longer rises up to temperature, treats that temperature descends 0.1 ℃, reacts completely, and filters, and washing is dried under 80 ℃ of conditions, obtains average grain diameter and be 8.73 microns micro silver powder.
Embodiment 5: with making the liquor argenti nitratis ophthalmicus that concentration is 200 grams per liters in 200 liters of deionized waters of 40 kilograms of silver nitrates addings, with 15 kilograms of Na
2CO
3Add 60 liters of deionized waters and make the Na that concentration is 250 grams per liters
2CO
3Solution.
Under 20～45 ℃ of temperature conditions, with Na
2CO
360% of solution was added drop-wise in the liquor argenti nitratis ophthalmicus in 20～30 minutes, carried out the above-mentioned solution of stirring at low speed with 85 rev/mins speed, measured 15 liters and analyzed pure formaldehyde and be poured in the above-mentioned solution and react, and no longer rose up to temperature, treated that temperature descends 0.1 ℃, with Na
2CO
3Solution remaining 40% is poured in the above-mentioned solution again, no longer rises up to temperature, treats that temperature descends 0.1 ℃, reacts completely, and filters, and washing is dried under 80 ℃ of conditions, obtains average grain diameter and be 9.66 microns micro silver powder.
Embodiment 6: with making the liquor argenti nitratis ophthalmicus that concentration is 200 grams per liters in 200 liters of deionized waters of 40 kilograms of silver nitrates addings, 12 kilograms of NaOH are added 60 liters of deionized waters make the NaOH solution that concentration is 200 grams per liters.
Under 20～45 ℃ of temperature conditions, in 20～30 minutes, be added drop-wise in the liquor argenti nitratis ophthalmicus fully NaOH solution, carry out the above-mentioned solution of stirring at low speed with 55 rev/mins speed, measure 15 liters of pure formic acid and be poured in the above-mentioned solution and react, no longer rise up to temperature, treat that temperature descends 0.1 ℃, react completely, filter, washing, under 60 ℃ of conditions, dry, obtain average grain diameter and be 5.15 microns micro silver powder.
Embodiment 7: with making the liquor argenti nitratis ophthalmicus that concentration is 200 grams per liters in 200 liters of deionized waters of 40 kilograms of silver nitrates addings, 15 kilograms of KOH are added 60 liters of deionized waters make the KOH solution that concentration is 250 grams per liters.
Under 20～45 ℃ of temperature conditions, 70% of KOH solution was added drop-wise in the liquor argenti nitratis ophthalmicus in 20～30 minutes, carry out the above-mentioned solution of stirring at low speed with 60 rev/mins speed, measuring 15 liters of ethylene glycol is poured in the above-mentioned solution and reacts, no longer rise up to temperature, treat that temperature descends 0.1 ℃, KOH solution remaining 30% is poured in the above-mentioned solution again, no longer rise up to temperature, treat that temperature descends 0.1 ℃, reacts completely, filter, washing is dried under 80 ℃ of conditions, obtains average grain diameter and be 8.68 microns micro silver powder.
Embodiment 8: with making the liquor argenti nitratis ophthalmicus that concentration is 200 grams per liters in 200 liters of deionized waters of 40 kilograms of silver nitrates addings, with 18 kilograms of K
2CO
3Add 60 liters of deionized waters and make the K that concentration is 300 grams per liters
2CO
3Solution.
Under 20～45 ℃ of temperature conditions, with K
2CO
360% of solution was added drop-wise in the liquor argenti nitratis ophthalmicus in 20～30 minutes, measured 15 liters of glycerine and was poured in the above-mentioned solution and reacts, and no longer rose up to temperature, treated that temperature descends 0.1 ℃, with K
2CO
3Solution remaining 40% is poured in the above-mentioned solution again, no longer rises up to temperature, treats that temperature descends 0.1 ℃, reacts completely, and filters, and washing is dried under 80 ℃ of conditions, obtains average grain diameter and be 9.75 microns micro silver powder.
Claims (8)
1, the preparation method of micro silver powder, with the silver nitrate is that raw material through chemical reaction prepares micro silver powder, it is characterized in that: earlier with silver nitrate with deionized water dissolving and be diluted to 200 grams per liters, be under 20～45 ℃ of conditions in temperature then, add alkaline matter in the above-mentioned liquor argenti nitratis ophthalmicus that makes, under the situation of stirring at low speed, pouring into organic reducing agent again, to generate average grain diameter be 5～10 microns micro silver powder, filter then, wash, dry, obtain finished product.
2, the preparation method of micro silver powder according to claim 1, it is characterized in that: described alkaline matter is NaOH, KOH, Na
2CO
3, K
2CO
3Any.
3, as the preparation method of micro silver powder as described in the claim 2, it is characterized in that: described alkaline matter is that concentration is the solution of 200～300 grams per liters.
4, as the preparation method of micro silver powder as described in the claim 3, it is characterized in that: described organic reducing agent can be any of formic acid, formaldehyde, ethylene glycol or glycerine.
5, as the preparation method of micro silver powder as described in the claim 4, it is characterized in that: the speed of described stirring at low speed is 50～85 rev/mins.
6, as the preparation method of micro silver powder as described in the claim 5, it is characterized in that: the temperature of described oven dry is 60～80 ℃.
7, as the preparation method of micro silver powder as described in claim 2 or 6, it is characterized in that: described alkaline matter adds in the liquor argenti nitratis ophthalmicus in two steps, earlier a part of alkaline matter is joined in the liquor argenti nitratis ophthalmicus, after adding organic reducing agent, again remaining alkaline matter is joined in the liquor argenti nitratis ophthalmicus that adds organic reducing agent, obtain the micro silver powder of different average grain diameters.
8, as the preparation method of micro silver powder as described in the claim 7, it is characterized in that: described silver nitrate weight is 40 kilograms, adds in 200 liters of deionized waters to make liquor argenti nitratis ophthalmicus, and described alkaline matter is 15 kilograms of Na
2CO
3Add 60 liters of Na that deionized water makes
2CO
3Solution, described organic reducing agent are 15 liters and analyze pure formaldehyde, by following step operation, obtain the micro silver powder of different average grain diameters,
A. with Na
2CO
3Solution was added drop-wise in the liquor argenti nitratis ophthalmicus in 20～30 minutes fully, measured to analyze pure formaldehyde and be poured in the above-mentioned solution and react, and no longer rose up to temperature, treat that temperature descends 0.1 ℃, react completely, filter, washing is dried under 60 ℃ of conditions, obtains average grain diameter and be 5.21 microns micro silver powder;
B. or, with Na
2CO
390% of solution was added drop-wise in the liquor argenti nitratis ophthalmicus in 20～30 minutes, measured to analyze pure formaldehyde and be poured in the above-mentioned solution and react, and no longer rose up to temperature, treated that temperature descends 0.1 ℃, with Na
2CO
3Solution remaining 10% is poured in the above-mentioned solution again, no longer rises up to temperature, treats that temperature descends 0.1 ℃, reacts completely, and filters, and washing is dried under 70 ℃ of conditions, obtains average grain diameter and be 6.54 microns micro silver powder;
C. or, with Na
2CO
380% of solution was added drop-wise in the liquor argenti nitratis ophthalmicus in 20～30 minutes, measured to analyze pure formaldehyde and be poured in the above-mentioned solution and react, and no longer rose up to temperature, treated that temperature descends 0.1 ℃, with Na
2CO
3Solution remaining 20% is poured in the above-mentioned solution again, no longer rises up to temperature, treats that temperature descends 0.1 ℃, reacts completely, and filters, and washing is dried under 80 ℃ of conditions, obtains average grain diameter and be 7.48 microns micro silver powder;
D. or, with Na
2CO
370% of solution was added drop-wise in the liquor argenti nitratis ophthalmicus in 20～30 minutes, measured to analyze pure formaldehyde and be poured in the above-mentioned solution and react, and no longer rose up to temperature, treated that temperature descends 0.1 ℃, with Na
2CO
3Solution remaining 30% is poured in the above-mentioned solution again, no longer rises up to temperature, treats that temperature descends 0.1 ℃, reacts completely, and filters, and washing is dried under 80 ℃ of conditions, obtains average grain diameter and be 8.73 microns micro silver powder;
E. or, with Na
2CO
360% of solution was added drop-wise in the liquor argenti nitratis ophthalmicus in 20～30 minutes, measured to analyze pure formaldehyde and be poured in the above-mentioned solution and react, and no longer rose up to temperature, treated that temperature descends 0.1 ℃, with Na
2CO
3Solution remaining 40% is poured in the above-mentioned solution again, no longer rises up to temperature, treats that temperature descends 0.1 ℃, reacts completely, and filters, and washing is dried under 80 ℃ of conditions, obtains average grain diameter and be 9.66 microns micro silver powder.
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| CN100506440C CN100506440C (en) | 2009-07-01 |
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| 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 |
| CN102248176A (en) * | 2011-07-15 | 2011-11-23 | 云南铜业科技发展股份有限公司 | Preparation method of flake silver powder with low burning loss |
| CN103143723A (en) * | 2013-03-27 | 2013-06-12 | 深圳市中金岭南科技有限公司 | Method for preparing flake silver powder with low bulk density |
| CN103769174A (en) * | 2014-01-24 | 2014-05-07 | 济南大学 | Preparation method of silver/silver chloride composite particles |
| CN105458285A (en) * | 2015-11-30 | 2016-04-06 | 成都市天甫金属粉体有限责任公司 | Silver powder preparing technology for controlling grain size through control over adding amount of sodium hydroxide |
| CN111889695A (en) * | 2020-07-15 | 2020-11-06 | 善日(嘉善)能源科技有限公司 | Preparation method of micro-nano silver powder with controllable particle size |
| CN112614608A (en) * | 2020-12-10 | 2021-04-06 | 广东工业大学 | Low-temperature co-fired ceramic inner conductive silver paste and preparation method thereof |
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2007
- 2007-07-11 CN CNB2007100494904A patent/CN100506440C/en active Active
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| 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 |
| CN102248176A (en) * | 2011-07-15 | 2011-11-23 | 云南铜业科技发展股份有限公司 | Preparation method of flake silver powder with low burning loss |
| 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 |
| CN103143723A (en) * | 2013-03-27 | 2013-06-12 | 深圳市中金岭南科技有限公司 | Method for preparing flake silver powder with low bulk density |
| CN103143723B (en) * | 2013-03-27 | 2015-09-30 | 深圳市中金岭南科技有限公司 | A kind of method preparing the flake silver powder of low-apparent-density |
| CN103769174A (en) * | 2014-01-24 | 2014-05-07 | 济南大学 | Preparation method of silver/silver chloride composite particles |
| CN103769174B (en) * | 2014-01-24 | 2016-08-17 | 济南大学 | A kind of preparation method of silver/silver chloride composite particles |
| CN105458285A (en) * | 2015-11-30 | 2016-04-06 | 成都市天甫金属粉体有限责任公司 | Silver powder preparing technology for controlling grain size through control over adding amount of sodium hydroxide |
| CN105458285B (en) * | 2015-11-30 | 2018-07-17 | 成都市天甫金属粉体有限责任公司 | A kind of silver powder preparation process controlling grain size by controlling sodium hydroxide additive amount |
| CN111889695A (en) * | 2020-07-15 | 2020-11-06 | 善日(嘉善)能源科技有限公司 | Preparation method of micro-nano silver powder with controllable particle size |
| CN112614608A (en) * | 2020-12-10 | 2021-04-06 | 广东工业大学 | Low-temperature co-fired ceramic inner conductive silver paste and preparation method thereof |
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| CN100506440C (en) | 2009-07-01 |
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Assignee: The Great Wall Gold & Silver Refinery Assignor: CHINA BANKNOTE PRINTING AND MINTING Corp. Contract record no.: 2011510000337 Denomination of invention: Prepn process of micro silver powder Granted publication date: 20090701 License type: Exclusive License Open date: 20071219 Record date: 20111229 |
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Address after: 610000 No. 189, Golden Road, Wenjiang District, Sichuan, Chengdu Patentee after: China Banknote Printing and Minting Group Co.,Ltd. Address before: 610000 No. 189, Golden Road, Wenjiang District, Sichuan, Chengdu Patentee before: CHINA BANKNOTE PRINTING AND MINTING Corp. |
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