CN104828854A - Method for preparing high purity silver nitrate from crude silver powder - Google Patents
Method for preparing high purity silver nitrate from crude silver powder Download PDFInfo
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- CN104828854A CN104828854A CN201510196141.XA CN201510196141A CN104828854A CN 104828854 A CN104828854 A CN 104828854A CN 201510196141 A CN201510196141 A CN 201510196141A CN 104828854 A CN104828854 A CN 104828854A
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Abstract
The invention relates to a method for preparing high purity silver nitrate from crude silver powder. The method comprises that excess crude silver powder and nitric acid subjected to distillation purification undergo a continuous reaction at a temperature of 30-50 DEG C to produce silver nitrate solution with pH greater than or equal to 4, wherein a refined nitric acid concentration is controlled in a range of 65-75% and a mole ratio of silver to nitric acid is 1: 0.65-0.85. The electrolysis crude silver powder is directly dissolved by nitric acid so that a silver nitrate solution is obtained, the silver nitrate solution is directly added into a high purity water adjustment system with pH greater than or equal to 5, the mixed solution undergoes a hydrolysis reaction, base metal impurities in the system are removed, the filtrate subjected to precision filtration is subjected to evaporation and crystallization, and the crystals are dried to form high purity silver nitrate products.
Description
Technical field
The present invention relates to the preparation method of silver deep processed product basic material Silver Nitrate finished product, belong to silver field of deep, specifically a kind of raw Ag powder prepares the processing method of high purity silver nitrate.
Background technology
Silver Nitrate is as a kind of main Chemicals of silver, have a wide range of applications in a lot of field, Silver Nitrate is also the raw material of many silver deep processed products simultaneously, is the basis producing the high added value silver fine chemical product such as various sensitive materials, silver catalyst, contact material, anti-biotic material, silver suboxide and super fine silver powder and silver slurry.
The production of tradition Silver Nitrate obtains product with purity 99.99% silver ingot through nitric acid dissolve, evaporation, crystallization, and raw materials cost is high, production efficiency is low.
About the preparation method of Silver Nitrate, domestic production mode is similar, in the production of photographic-grade Silver Nitrate, just have the processing method of further imurity-removal, because photographic-grade Silver Nitrate market capacity is limited, and the market outlook do not had.
The document that can mention: the 1) preparation of high-purity (99.999%) Silver Nitrate, Chen Hongbin is permitted the purple big vast * (Shanghai Educational College) of logical beautiful Liu of prosperous (Shanghai Science and Tech. United Co 200031) Liu Mei; 2) high purity silver nitrate preparation research and production practice, Cai trains troop (Central South University's Master's thesis 2009.6).
These documents adopt silver ingot or assorted silver to be raw material, traditionally strictly operate, just obtain reagent secondary (AR) Silver Nitrate.Obtain the Silver Nitrate that purity is high, adjust ph, recrystallize just can obtain high purity product further also to need to add reagent stair oxidation silver.Actual in the selection of raw material, produce the electrolysis silver bullion of the high-purity silver nitrate optimal purity more than 99.9% of argent used, guarantee product quality.
Summary of the invention
The object of the invention is to propose the processing method that a kind of raw Ag powder prepares high purity silver nitrate, adopt the mode direct production high-purity silver nitrate product of nitric acid dissolve, purification of water, to enhance productivity and metal recovery rate, reduce production cost.
For achieving the above object, a kind of raw Ag powder of the present invention prepares the processing method of high purity silver nitrate, and implementation method comprises:
The detection of (I) raw Ag powder: get silver powder and add in reactor, controls temperature in the kettle 30-50 DEG C, is interrupted the nitric acid after adding distilation, and controlling silver with the mol ratio of nitric acid is 1:0.65-0.85, sustained reaction, until the gas of reddish-brown disappears;
The silver nitrate solution that (II) is obtained by reacting surveys pH value, if pH >=4 proceed to next procedure; If pH < 4, appropriate silver powder need be added and consume residual acid further, make system pH >=4 carry out next step operation again;
(III) above-mentioned solution directly adds high purity water and is hydrolyzed, add pure water to be hydrolyzed, control pH value of solution > 5, density 1.75-1.80, obtain pure silver nitrate solution, obtain the silver nitrate solution clarified through a sedimentation, filtration, secondary settlement; Evaporative crystallization after filter ageing, centrifugal, drying obtains Silver Nitrate product.
A kind of raw Ag powder of the present invention prepares the processing method of high purity silver nitrate, and its beneficial effect is: adopt electrolytic silver powder directly to prepare Silver Nitrate, avoid shrend or the planing of silver ingot, reduce the loss of silver powder refining and ingot casting, improve metal recovery rate; The reaction later stage wants accurate hierarchy of control pH value, if system pH >=4 subsequent job is difficult to control, can not work continuously, and increases materials consumption, reduces working efficiency; Silver Nitrate filtrate directly adds high purity water and to be hydrolyzed removing base metal impurity, does not introduce other impurity, and purifying method is simply effective, enhances productivity and metal recovery rate, reduces production cost.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention;
Fig. 2 product detected result in kind.
Embodiment
Embodiment 1
500 kilograms of raw Ag powder are added in 1000L steel lining titanium reactor, interruption adds 420L65% and refines nitric acid, 4-5 hour is reacted under temperature 30-50 DEG C of condition, when question response slows down, open and stir and heat up, when system does not have oxynitride to produce, during survey system pH >=4, control temperature 75-80 DEG C, add pure water to be hydrolyzed, control pH value of solution > 5, density 1.75-1.80, obtain pure silver nitrate solution, obtain the silver nitrate solution clarified through a sedimentation, filtration, secondary settlement; Evaporative crystallization after filter ageing, centrifugal, drying obtains Silver Nitrate product.
Embodiment 2
1000 kilograms of raw Ag powder are added in 2500L steel lining titanium reactor, interruption adds 840L65% and refines nitric acid, 4-5 hour is reacted under temperature 30-50 DEG C of condition, when question response slows down, open and stir and heat up, when system does not have oxynitride to produce, during survey system pH >=4, control temperature 75-80 DEG C, add pure water to be hydrolyzed, control pH value of solution > 5, density 1.75-1.80, obtain pure silver nitrate solution, obtain the silver nitrate solution clarified through a sedimentation, filtration, secondary settlement; Evaporative crystallization after filter ageing, centrifugal, drying obtains Silver Nitrate product.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (2)
1. prepare a processing method for high purity silver nitrate with raw Ag powder, it is characterized in that: described method comprises the following steps:
The detection of (I) raw Ag powder: get silver powder and add in reactor, controls temperature in the kettle 30-50 DEG C, adds the nitric acid after distilation, and controlling silver with the mol ratio of nitric acid is 1:0.65-0.85, sustained reaction, until the gas of reddish-brown disappears;
The silver nitrate solution that (II) is obtained by reacting surveys pH value, if pH >=4 proceed to next procedure; If pH < 4, appropriate silver powder need be added and consume residual acid further, make system pH >=4 carry out next step operation again;
(III) above-mentioned solution directly adds high purity water and is hydrolyzed, add pure water to be hydrolyzed, control pH value of solution > 5, density 1.75-1.80, obtain pure silver nitrate solution, obtain the silver nitrate solution clarified through a sedimentation, filtration, secondary settlement; Evaporative crystallization after filter ageing, centrifugal, drying obtains Silver Nitrate product.
2. a kind of raw Ag powder prepares the processing method of high purity silver nitrate as claimed in claim 1, it is characterized in that: described in add 65% refining nitric acid be that interruption adds, add speed 7-8.75 L/5 minute.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510196141.XA CN104828854A (en) | 2015-04-23 | 2015-04-23 | Method for preparing high purity silver nitrate from crude silver powder |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510196141.XA CN104828854A (en) | 2015-04-23 | 2015-04-23 | Method for preparing high purity silver nitrate from crude silver powder |
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| CN104828854A true CN104828854A (en) | 2015-08-12 |
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| CN201510196141.XA Pending CN104828854A (en) | 2015-04-23 | 2015-04-23 | Method for preparing high purity silver nitrate from crude silver powder |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109970094A (en) * | 2019-04-23 | 2019-07-05 | 金川集团股份有限公司 | A kind of prepare inhales the process that wave screen covers special package material silver nitrate |
| CN110387563A (en) * | 2019-07-26 | 2019-10-29 | 紫金矿业集团黄金冶炼有限公司 | A kind of industrial production process of 5N high purity silver |
| CN109775745B (en) * | 2019-03-20 | 2021-06-29 | 金川集团股份有限公司 | Preparation method of silver nitrate for wave-absorbing shielding special-purpose material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1261750B1 (en) * | 2000-01-28 | 2004-04-28 | Umicore | Wet process for refining silver bullion including gold separation |
| CN102660684B (en) * | 2012-04-18 | 2013-07-31 | 金华冠华水晶有限公司 | Method for purifying silver by using wastewater of silver plating production line of rhinestone and method for preparing high-purity silver nitrate |
-
2015
- 2015-04-23 CN CN201510196141.XA patent/CN104828854A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1261750B1 (en) * | 2000-01-28 | 2004-04-28 | Umicore | Wet process for refining silver bullion including gold separation |
| CN102660684B (en) * | 2012-04-18 | 2013-07-31 | 金华冠华水晶有限公司 | Method for purifying silver by using wastewater of silver plating production line of rhinestone and method for preparing high-purity silver nitrate |
Non-Patent Citations (4)
| Title |
|---|
| 宋元宁: "以粗银为原料制备分析纯硝酸银的工艺探讨", 《有色矿冶》 * |
| 张钦发等: "含银废料中银的综合回收和利用工艺方法", 《有色金属》 * |
| 王吉华等: "粗银直接制备试剂碳酸银的工艺研究", 《云南化工》 * |
| 陈鸿彬: "高纯（99.999%）硝酸银的制备", 《化学世界》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109775745B (en) * | 2019-03-20 | 2021-06-29 | 金川集团股份有限公司 | Preparation method of silver nitrate for wave-absorbing shielding special-purpose material |
| CN109970094A (en) * | 2019-04-23 | 2019-07-05 | 金川集团股份有限公司 | A kind of prepare inhales the process that wave screen covers special package material silver nitrate |
| CN109970094B (en) * | 2019-04-23 | 2021-08-27 | 金川集团股份有限公司 | Process method for preparing silver nitrate for wave-absorbing shielding special material |
| CN110387563A (en) * | 2019-07-26 | 2019-10-29 | 紫金矿业集团黄金冶炼有限公司 | A kind of industrial production process of 5N high purity silver |
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Application publication date: 20150812 |
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