CN111924869A - Silver nitrate lead-removing purification process - Google Patents
Silver nitrate lead-removing purification process Download PDFInfo
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- CN111924869A CN111924869A CN202010824970.9A CN202010824970A CN111924869A CN 111924869 A CN111924869 A CN 111924869A CN 202010824970 A CN202010824970 A CN 202010824970A CN 111924869 A CN111924869 A CN 111924869A
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- silver nitrate
- silver
- lead
- filtrate
- membrane
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G5/00—Compounds of silver
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention aims to provide a silver nitrate lead-removing purification process which has high lead-removing efficiency, high product purity, low production cost and simple and convenient operation.
Description
Technical Field
The invention relates to a silver nitrate purification process, in particular to a silver nitrate lead-removing purification process.
Background
The rapid development of the electronic information industry, the specific gravity of the silver used in the electronic industry is higher and higher, and the popularization of the photovoltaic technology, which is one of the clean energy technologies, greatly drives the industrial application of the silver. The silver nitrate is used as a main raw material of industrial silver, the domestic production and sales volume is increased year by year, the content of impurities in the silver nitrate is one of important standards for evaluating the quality of the silver nitrate, in the electronic industry, the content of the impurities of the silver nitrate has an important influence on the quality of downstream products produced by using the silver nitrate as a raw material, and the content of lead is one of important indexes.
The production of silver nitrate mainly adopts an acidolysis method, namely silver and nitric acid are used as raw materials, and the silver and the nitric acid carry out redox reaction to generate the silver nitrate. The main process flow comprises oxidation, hydrolysis, evaporation, concentration, crystallization and drying, impurities in the finished silver nitrate mainly come from raw materials, most of impurities such as iron, copper and the like in the raw materials can be removed through hydrolysis, but lead impurities mainly contain Pb in the production of the silver nitrate2+The existing method is not easy to remove by a hydrolysis process under the condition of lower pH value, and is the key for influencing the product quality. Therefore, the quality of the silver nitrate product greatly depends on the quality of raw materials, the standard requirement of the existing raw material silver in the national standard No. 1 silver on lead in the silver is less than 20ppm, and the requirement of the variety with the largest demand in the silver nitrate product standard on lead in the analytically pure silver nitrate is less than 10ppm, so that the quality of the silver nitrate is greatly influenced by the quality of the lead removing process.
The existing measures for controlling lead in silver nitrate production comprise the following methods: firstly, the requirement on the lead content in the raw material silver is improved, namely the lower the lead content in the silver used for silver nitrate production, the better the lead content; and secondly, reducing the lead content in the product by adopting a multi-crystallization mode or reducing the crystallization rate.
Although qualified analytically pure silver nitrate can be produced by adopting the method, the yield of superior pure silver nitrate is low, and the quality control of the product is mainly controlled by inspecting the finished product. The following problems exist from the viewpoint of economy, energy conservation and environmental protection:
put forward high demand for silver quality which is one of main raw material, and for producing analytically pure silver nitrate
In addition, the control requirement of the raw material silver is far higher than that of the national standard No. 1 silver, so that the raw material supply is limited, and the price of the raw material has no permitted space;
secondly, the finished product rate of products is reduced, no process monitoring means is provided, the product quality is not controllable, and the yield is improved
The product processing cost improves the raw material and finished product detection control difficulty.
Silver nitrate is used as an important chemical raw material in the electronic industry, has the characteristic of light material weight and work weight, and is important in cost control and product delivery timeliness and capital turnover rate in production and operation, and product quality and technical and economic indexes are key points in operation.
Disclosure of Invention
The invention aims to provide a lead-removing agent with high lead-removing efficiency, high product purity, low production cost and simple operation
A convenient and easy silver nitrate lead-removing purification process.
The invention relates to a silver nitrate lead-removing purification process, which comprises the following steps:
(1) a concentration adjusting and liquid preparing process: adding a silver nitrate solution generated by the reaction of nitric acid and silver into a hydrolyzer, and adjusting the density of the silver nitrate solution to 1.5-2.0 g/cm by using water3Adjusting the pH value in the hydrolyzer to 3-5 by using silver oxide;
(2) impurity removal and filtration processes: adding an impurity removing agent carbonate into the hydrolyzer of the concentrated solution prepared in the step (1), starting a stirring device of the hydrolyzer, stirring for 2-4 h, stopping the stirring device, standing the solution in the hydrolyzer for 1-4 h, introducing the solution into a filter tank, filtering, introducing the obtained filtrate into a filtrate storage tank, and cleaning the obtained filter cake with deionized water and then removing the filter cake into a collecting bin;
(3) and (3) an inspection process: analyzing and testing the indexes of the filtrate in the filtrate storage tank obtained in the step (2), and if the lead content in the filtrate is more than or equal to 10ppm, sequentially repeating the steps (1) - (2) for a plurality of times until the lead content in the filtrate storage tank is less than 10 ppm;
(4) a precise filtering process: introducing the qualified filtrate obtained by the previous step into a membrane filtration component by a pump for filtration;
(5) an evaporation concentration process: pumping the filtrate obtained in the precise filtering process in the step (4) to an evaporation kettle for concentration;
(6) and (5) a crystal drying procedure, namely cooling and crystallizing the silver nitrate solution obtained in the evaporation and concentration procedure in the step (5), and carrying out solid-liquid separation and drying to obtain the finished product of silver nitrate.
The addition amount of the preferred impurity removing agent is 0.1-1% of the mass of the silver in the silver nitrate solution.
By adopting the technical scheme, the pH value in the hydrolyzer is adjusted by using silver oxide, a certain amount of impurity removing agent is added in the silver nitrate hydrolysis procedure, lead ions react with the lead ions to form precipitates, then the precipitates are removed together with other hydrolysis products in the later treatment, other harmful impurities are not brought in the reaction process of the impurity removing agent and the lead ions, the special impurity removing agent for removing lead, namely silver carbonate is a water-insoluble compound, and the reaction product, the redundant impurity removing agent and other hydrolysis products are filtered and discharged together with filter cakes in the reaction process, so that the impurity removal is realized, and the purity of the product is ensured.
Further, the molecular weight of the polymer membrane selected by the membrane filtration module is 1 to 10 ten thousand.
Preferably, the membrane filtration module is a hollow tubular membrane module.
Preferably, the membrane of the membrane filtration module is an organic maple membrane.
The combination of the filter tank and the membrane filter component is adopted to filter out water-insoluble substances as much as possible, thereby ensuring the high purity of the product.
In conclusion, the silver nitrate lead-removing purification process provided by the invention adopts the impurity removing agent and the process combining chemical and physical impurity removal, and has the advantages of high lead-removing efficiency, simple process flow, convenience in operation, high product purity and low production cost.
Detailed Description
The invention is further illustrated by the following examples:
the silver nitrate lead-removing purification process comprises the following steps:
(1) a concentration adjusting and liquid preparing process: adding a silver nitrate solution generated by the reaction of nitric acid and silver into a hydrolyzer, and adjusting the density of the silver nitrate solution to 1.5-2.0 g/cm by using water3In silver oxide-regulated hydrolyzersThe pH value is 3-5;
(2) impurity removal and filtration processes: adding an impurity removing agent silver carbonate into the hydrolyzer subjected to concentration adjustment and solution preparation in the step (1), starting a stirring device of the hydrolyzer, stirring for 2-4 h, stopping the stirring device, standing the solution in the hydrolyzer for 1-4 h, introducing the solution into a filter tank, filtering, introducing the obtained filtrate into a filtrate storage tank, washing the obtained filter cake with deionized water, and then removing the filter cake into a collecting bin;
(3) and (3) an inspection process: analyzing and testing the indexes of the filtrate in the filtrate storage tank obtained in the step (2), and if the lead content in the filtrate is more than or equal to 10ppm, sequentially repeating the steps (1) - (2) for a plurality of times until the lead content in the filtrate storage tank is less than 10 ppm;
(4) a precise filtering process: introducing the qualified filtrate obtained by the previous step into a membrane filtration component by a pump for filtration;
(5) an evaporation concentration process: pumping the filtrate obtained in the precise filtering process in the step (4) to an evaporation kettle for concentration;
(6) and (5) a crystal drying procedure, namely cooling and crystallizing the silver nitrate solution obtained in the evaporation and concentration procedure in the step (5), and carrying out solid-liquid separation and drying to obtain the finished product of silver nitrate.
The first embodiment is as follows:
(1) the content of silver and lead in the raw material is 8ppm, 800kg of silver nitrate aqueous solution is fed once, and the density of the silver nitrate aqueous solution in the hydrolysis procedure is 1.7g/cm3Adjusting the pH value to be 4 by using silver oxide, adding 5kg of impurity removing agent silver carbonate, reacting for 4 hours, standing for 1 hour, performing bag type filtration through a filter tank and 1 ten thousand molecular weight membrane filtration, and then sequentially performing concentration, cooling crystallization, solid-liquid separation and drying through an evaporation kettle to obtain a finished product of silver nitrate, wherein the primary yield of the silver nitrate is 80%, and the lead content in the finished product of silver nitrate is less than 1 ppm.
Example two:
(1) the lead content in the raw material silver is 43ppm, the raw material silver is fed by 800kg once, and the density of the silver nitrate and silver nitrate aqueous solution in the hydrolysis process is 1.7g/cm3Using silver oxide with pH value of 4, adopting three times of hydrolysis, first hydrolysis, adding silver carbonate with 5kg respectively, reacting for 4 hr, standing for 1 hr, and using second and third times of waterThe adding amount of the silver carbonate is 2kg and 2kg respectively, the reaction lasts for 2 hours, the standing lasts for 1 hour, the silver nitrate is subjected to bag type filtration through a filter tank and filtration through an organic polymer film with 1 ten thousand molecular weight, and then concentration, cooling crystallization, solid-liquid separation and drying are sequentially carried out through an evaporation kettle to obtain the finished product of silver nitrate, the primary yield of the silver nitrate is 80%, and the lead content in the finished product is less than 2 ppm.
Claims (5)
1. The silver nitrate lead-removing purification process is characterized by comprising the following steps:
(1) a concentration adjusting and liquid preparing process: adding a silver nitrate solution generated by the reaction of nitric acid and silver into a hydrolyzer, and adjusting the density of the silver nitrate solution to 1.5-2.0 g/cm by using water3Adjusting the pH value in the hydrolyzer to 3-5 by using silver oxide;
(2) impurity removal and filtration processes: adding an impurity removing agent silver carbonate into the hydrolyzer subjected to concentration adjustment and solution preparation in the step (1), starting a stirring device of the hydrolyzer, stirring for 2-4 h, stopping the stirring device, standing the solution in the hydrolyzer for 1-4 h, introducing the solution into a filter tank, filtering, introducing the obtained filtrate into a filtrate storage tank, washing the obtained filter cake with deionized water, and then removing the filter cake into a collecting bin;
(3) and (3) an inspection process: analyzing and testing the indexes of the filtrate in the filtrate storage tank obtained in the step (2), and if the lead content in the filtrate is more than or equal to 10ppm, sequentially repeating the steps (1) - (2) for a plurality of times until the lead content in the filtrate storage tank is less than 10 ppm;
(4) a precise filtering process: introducing the qualified filtrate obtained by the previous step into a membrane filtration component by a pump for filtration;
(5) an evaporation concentration process: pumping the filtrate obtained in the precise filtering process in the step (4) to an evaporation kettle for concentration;
(6) and (5) a crystal drying procedure, namely cooling and crystallizing the silver nitrate solution obtained in the evaporation and concentration procedure in the step (5), and carrying out solid-liquid separation and drying to obtain the finished product of silver nitrate.
2. The silver nitrate lead-removing purification process as claimed in claim 1, which is characterized in that: the addition amount of the impurity removing agent is 0.1-1% of the mass of silver in the silver nitrate solution.
3. The silver nitrate lead-removing purification process as claimed in claim 1, which is characterized in that: the molecular weight of the polymer membrane selected by the membrane filtration component is 1-10 ten thousand.
4. The silver nitrate lead-removing purification process as claimed in claim 1 or 3, characterized in that: the membrane filtering component is a hollow tubular membrane component.
5. The silver nitrate lead-removing purification process as claimed in claim 4, characterized in that: the membrane of the membrane filtration component is an organic maple membrane.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010824970.9A CN111924869A (en) | 2020-08-17 | 2020-08-17 | Silver nitrate lead-removing purification process |
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| CN202010824970.9A CN111924869A (en) | 2020-08-17 | 2020-08-17 | Silver nitrate lead-removing purification process |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4136157A (en) * | 1976-07-09 | 1979-01-23 | Fuji Photo Film Co., Ltd. | Method of preparing purified silver nitrate |
| CN1124174A (en) * | 1994-01-07 | 1996-06-12 | 株式会社久保田 | Filtration membrane module |
| CN102040240A (en) * | 2009-10-16 | 2011-05-04 | 中科铜都粉体新材料股份有限公司 | Method for producing high-purity silver nitrate |
| CN103214022A (en) * | 2013-04-12 | 2013-07-24 | 西陇化工股份有限公司 | Method for preparing high-purity silver nitrate |
| CN108190938A (en) * | 2017-12-22 | 2018-06-22 | 昆明理工大学 | It is a kind of to give up the method that silver paste prepares high purity silver nitrate from photovoltaic |
| CN108585025A (en) * | 2018-07-11 | 2018-09-28 | 郴州市金贵银业股份有限公司 | A kind of recovery method of silver oxide slag |
| 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 |
-
2020
- 2020-08-17 CN CN202010824970.9A patent/CN111924869A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4136157A (en) * | 1976-07-09 | 1979-01-23 | Fuji Photo Film Co., Ltd. | Method of preparing purified silver nitrate |
| CN1124174A (en) * | 1994-01-07 | 1996-06-12 | 株式会社久保田 | Filtration membrane module |
| CN102040240A (en) * | 2009-10-16 | 2011-05-04 | 中科铜都粉体新材料股份有限公司 | Method for producing high-purity silver nitrate |
| CN103214022A (en) * | 2013-04-12 | 2013-07-24 | 西陇化工股份有限公司 | Method for preparing high-purity silver nitrate |
| CN108190938A (en) * | 2017-12-22 | 2018-06-22 | 昆明理工大学 | It is a kind of to give up the method that silver paste prepares high purity silver nitrate from photovoltaic |
| CN108585025A (en) * | 2018-07-11 | 2018-09-28 | 郴州市金贵银业股份有限公司 | A kind of recovery method of silver oxide slag |
| 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 |
Non-Patent Citations (2)
| Title |
|---|
| 夏焕锦等: "纳滤膜去除硝酸银中痕量多价金属的研究", 《膜科学与技术》 * |
| 韩长日，宋小平主编: "《电子及信息用化学品生产工艺与技术》", 31 July 2019, 科学技术文献出版社 * |
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Application publication date: 20201113 |