CN101628730B - Method for preparing photographic-grade silver nitrate through one-time crystallization - Google Patents
Method for preparing photographic-grade silver nitrate through one-time crystallization Download PDFInfo
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- CN101628730B CN101628730B CN 200910065936 CN200910065936A CN101628730B CN 101628730 B CN101628730 B CN 101628730B CN 200910065936 CN200910065936 CN 200910065936 CN 200910065936 A CN200910065936 A CN 200910065936A CN 101628730 B CN101628730 B CN 101628730B
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Abstract
The invention discloses a method for preparing photographic-grade silver nitrate through one-time crystallization, comprising the following control conditions of temperature control, concentration control and purifying agent selection in the silver dissolving process, addition proportion and critical point identification, concentration temperature control, terminal point definition, crystallization time and drying temperature and the like. As the key production factors are well selected and controlled, the silver nitrate prepared by the invention features high purity and low impurity content,can be used for preparing film emulsion, has good light sensitivity and low fog density, can reach the standard of photographic-grade silver nitrate by crystallization for once, and has low production cost, short production cycle, high yield and small loss rate of products.
Description
Technical field
The invention belongs to the method for preparation method's technical field, particularly a kind of preparing photographic-grade silver nitrate through one-time crystallization of Silver Nitrate.
Background technology
The photographic-grade Silver Nitrate is the highest level in the present Silver Nitrate production field, and it is very high to the requirement of the Silver Nitrate that makes, comprises that mainly foreign matter content is low, and the time of guaranteeing the quality is long, prepared photograph halogen agent light sensitivity height, and fog density is low.Many deficiencies such as the Silver Nitrate that general method is produced is difficult to satisfy the demand of taking a picture, and ordinary method is produced the photographic-grade Silver Nitrate needs secondary crystal, even repeatedly crystallization, and impurity-eliminating effect is bad, and the Silver Nitrate productive rate is low, the production cycle long, the quality guaranteed period is short.
The method removal of impurities of the logical oxygen of the usefulness that has, as the patent No.: 01114721.0, publication number: CN1386707, denomination of invention: the disclosed preparation method of the preparation method of high-purity silver nitrate crystal, comprise the heating silver nitrate solution, in solution, add nitric acid, blast a large amount of gas in solution, subsequently with the following crystallization of silver nitrate solution cool to room temperature, finally by centrifugal, drying obtains silver nitrate crystal, wherein, the nitric acid that adds is more than 30%, the content of nitric acid is more than 5% in the silver nitrate solution behind the adding nitric acid, and the temperature that adds the preceding silver nitrate solution of nitric acid is that temperature remains on more than 40 ℃ after adding nitric acid more than 40 ℃.Reaction conditions is required height, and speed of response is difficult to control, and is easy to bring into new impurity, the requirement that does not reach the photographic-grade Silver Nitrate far away.
Summary of the invention
The invention provides the method for a kind of good impurity removing effect, Silver Nitrate productive rate height, with short production cycle, preparing photographic-grade silver nitrate through one-time crystallization that the maintenance phase is long.
A kind of method of preparing photographic-grade silver nitrate through one-time crystallization, it may further comprise the steps:
A. get GB 1
#12～18 kilograms on silver ingot is put into reactor, adds 11～16 liters of 60～70% concentrated nitric acids then in the reactor;
B. reactor heating, solution temperature is raise gradually, when reaching 60 ℃, react violent gradually, lasting heating reaches between 80～90 ℃ solution temperature, and it is fully reacted, after reaction finishes, continue heating 2-3 hour, till can't see oxynitride and overflowing, make the pH value of solution in 1～2 scope;
C. the above-mentioned solution that makes is changed over to and have the assorted of whipping appts and stir with 50 rev/mins rotating speeds except in the container, in the process that stirs, add silver suboxide, add-on is 50～70 grams, when the pH value of solution is 7.5～8.5, stop to stir 4～6 hours after-filtration of natural sedimentation;
D. the solution after will filtering is put into vaporizer, in solution, add 10～20 gram analytical pure nitric acid, 110～130 ℃ of thickening temperatures, concentrate about 2.5～3.5 hours, when solution surface forms tunica albuginea and be sticking slightly vaporizer inwall state, stop heating, solution is put into crystallizing tank, spontaneous nucleation is 10～15 hours under 5～15 ℃ of temperature, separates with whizzer;
E. separate the vacuum-drying 4～6 hours under 80～100 ℃ of temperature of back gained solid nitric acid silver, get silver nitrate crystal.
As of the present invention a kind of preferred, a kind of method of preparing photographic-grade silver nitrate through one-time crystallization, it may further comprise the steps:
A. get GB 1
#15 kilograms on silver ingot is put into reactor, adds 13.5 liters of 65% concentrated nitric acids then in the reactor;
B. reactor heating, solution temperature is raise gradually, when reaching 60 ℃, react violent gradually, lasting heating reaches between 80～90 ℃ solution temperature, and it is fully reacted, after reaction finishes, continue heating 2-3 hour, till can't see oxynitride and overflowing, make the pH value of solution in 1～2 scope;
C. the above-mentioned solution that makes is changed over to and have the assorted of whipping appts and stir with 50 rev/mins rotating speeds except in the container, add silver suboxide in the process that stirs, add-on is 60 grams, when the pH value of solution is 8, stops to stir 5 hours after-filtration of natural sedimentation;
D. the solution after will filtering is put into vaporizer, in solution, add 15 gram analytical pure nitric acid, 120 ℃ of thickening temperatures, concentrate about 3 hours, when solution surface forms tunica albuginea and be sticking slightly vaporizer inwall state, stop heating, solution is put into crystallizing tank, spontaneous nucleation is 12 hours under 10 ℃ of temperature, separates with whizzer;
E. separate the vacuum-drying 5 hours under 90 ℃ of temperature of back gained solid nitric acid silver, get silver nitrate crystal.
The method of preparing photographic-grade silver nitrate through one-time crystallization of the present invention, comprise the selection of temperature control in the molten silver-colored process, concentration control, cleaner, additional proportion, stagnation point differentiate, the control of thickening temperature, terminal point define and control conditions such as time of crystallization and drying temperature.Owing to selected to have controlled the above-mentioned crucial factor of production well, make the preparation that Silver Nitrate purity height, the foreign matter content with the present invention's preparation is little, be used for film emulsion, light sensitivity is good, fog density is low.Disposable crystallization can reach photographic-grade Silver Nitrate standard.And production cost is low, life cycle of the product is short, productive rate is high, rate of loss is little.
Embodiment
Embodiment one:
A kind of method of preparing photographic-grade silver nitrate through one-time crystallization, it may further comprise the steps:
A. get GB 1
#13 kilograms on silver ingot is put into reactor, adds 11 liters of 61% concentrated nitric acids then in the reactor;
B. reactor heating, solution temperature is raise gradually, when reaching 60 ℃, react violent gradually, lasting heating reaches between 81 ℃ solution temperature, and it is fully reacted, after reaction finishes, continue heating 2 hours, till can't see oxynitride and overflowing, make the pH value of solution in 1～2 scope;
C. the above-mentioned solution that makes is changed over to and have the assorted of whipping appts and stir with 50 rev/mins rotating speeds except in the container, add silver suboxide in the process that stirs, add-on is 5 grams, when the pH value of solution is 7.6, stops to stir 4.2 hours after-filtration of natural sedimentation;
D. the solution after will filtering is put into vaporizer, in solution, add 11 gram analytical pure nitric acid, 110 ℃ of thickening temperatures, concentrate about 2.6 hours, when solution surface forms tunica albuginea and be sticking slightly vaporizer inwall state, stop heating, solution is put into crystallizing tank, spontaneous nucleation is 11 hours under 7 ℃ of temperature, separates with whizzer;
E. separate the vacuum-drying 4 hours under 82 ℃ of temperature of back gained solid nitric acid silver, get silver nitrate crystal.
Embodiment two:
A kind of method of preparing photographic-grade silver nitrate through one-time crystallization, it may further comprise the steps:
A. get GB 1
#178 kilograms on silver ingot is put into reactor, adds 16 liters of 69% concentrated nitric acids then in the reactor;
B. reactor heating, solution temperature is raise gradually, when reaching 60 ℃, react violent gradually, lasting heating reaches between 90 ℃ solution temperature, and it is fully reacted, after reaction finishes, continue heating 3 hours, till can't see oxynitride and overflowing, make the pH value of solution in 1～2 scope;
C. the above-mentioned solution that makes is changed over to and have the assorted of whipping appts and stir with 50 rev/mins rotating speeds except in the container, add silver suboxide in the process that stirs, add-on is 70 grams, when the pH value of solution is 8.4, stops to stir 6 hours after-filtration of natural sedimentation;
D. the solution after will filtering is put into vaporizer, in solution, add 19 gram analytical pure nitric acid, 130 ℃ of thickening temperatures, concentrate about 3.5 hours, when solution surface forms tunica albuginea and be sticking slightly vaporizer inwall state, stop heating, solution is put into crystallizing tank, spontaneous nucleation is 14 hours under 14 ℃ of temperature, separates with whizzer;
E. separate the vacuum-drying 6 hours under 98 ℃ of temperature of back gained solid nitric acid silver, get silver nitrate crystal.
Embodiment three:
A kind of method of preparing photographic-grade silver nitrate through one-time crystallization, it may further comprise the steps:
A. get GB 1
#15 kilograms on silver ingot is put into reactor, adds 13.5 liters of 65% concentrated nitric acids then in the reactor;
B. reactor heating, solution temperature is raise gradually, when reaching 60 ℃, react violent gradually, lasting heating reaches between 80～90 ℃ solution temperature, and it is fully reacted, after reaction finishes, continue heating 2-3 hour, till can't see oxynitride and overflowing, make the pH value of solution in 1～2 scope;
C. the above-mentioned solution that makes is changed over to and have the assorted of whipping appts and stir with 50 rev/mins rotating speeds except in the container, add silver suboxide in the process that stirs, add-on is 60 grams, when the pH value of solution is 8, stops to stir 5 hours after-filtration of natural sedimentation;
D. the solution after will filtering is put into vaporizer, in solution, add 15 gram analytical pure nitric acid, 120 ℃ of thickening temperatures, concentrate about 3 hours, when solution surface forms tunica albuginea and be sticking slightly vaporizer inwall state, stop heating, solution is put into crystallizing tank, spontaneous nucleation is 12 hours under 10 ℃ of temperature, separates with whizzer;
E. separate the vacuum-drying 5 hours under 90 ℃ of temperature of back gained solid nitric acid silver, get silver nitrate crystal.
The reaction principle of above-described embodiment is:
4Ag+6HNO3＝4AgNO3+NO+NO2+3H2O
Owing in the silver nitrate solution that generates, contain metal ions such as copper, iron, lead, bismuth, become the major impurity of the Silver Nitrate quality factor that influences.Select the high silver suboxide of purity as cleaner, by reconciling pH value, make impurity hydrolytic precipitations such as copper, iron, lead, bismuth, thereby reach the purpose of purification.Disposable removal of impurities thoroughly and not forms secondary pollution, has realized using a kind of chemical reagent to remove the purpose of Determination of Multi-Impurities.Its removal of impurities principle mainly is that to utilize silver suboxide be the characteristic of basic oxide, and the H+ ion in the neutralization solution is achieved.
Ag2O+2HNO3＝2AgNO3+H2O
By the Silver Nitrate after the removal of impurities operation, because pH value is higher, oxidized easily, storage period is long slightly, the surface oxidation flavescence, and namely Silver Nitrate is rotten.For addressing this problem, when concentrated, add a certain amount of nitric acid, forming the Silver Nitrate surface protection film of acidifying, can prolonged preservation and never degenerate for a long time.
Comparative example one:
A. get GB 1
#15 kilograms on silver ingot is put into reactor, adds 13.5 liters of 65% concentrated nitric acids then in the reactor;
B. reactor heating, solution temperature is raise gradually, when reaching 60 ℃, react violent gradually, lasting heating reaches between 80～90 ℃ solution temperature, and it is fully reacted, after reaction finishes, continue heating 2-3 hour, till can't see oxynitride and overflowing, make the pH value of solution in 1～2 scope;
C. the solution after will filtering is put into vaporizer, in solution, add 15 gram analytical pure nitric acid, 120 ℃ of thickening temperatures, concentrate about 3 hours, when solution surface forms tunica albuginea and be sticking slightly vaporizer inwall state, stop heating, solution is put into crystallizing tank, spontaneous nucleation is 12 hours under 10 ℃ of temperature, separates with whizzer;
D. separate the vacuum-drying 5 hours under 90 ℃ of temperature of back gained solid nitric acid silver, get silver nitrate crystal.
Three embodiment of the invention described above and a comparative example gained Silver Nitrate index and former the Ministry of Chemical Industry photograph one-level
Standard is compared as follows table:
From last table as seen, the Silver Nitrate that the Silver Nitrate foreign matter content for preparing with the present invention prepares well below ordinary method, and all meet and exceed the Ministry of Chemical Industry's photograph first quality standard.
The method of preparing photographic-grade silver nitrate through one-time crystallization of the present invention, comprise the selection of temperature control in the molten silver-colored process, concentration control, cleaner, additional proportion, stagnation point differentiate, the control of thickening temperature, terminal point define and control conditions such as time of crystallization and drying temperature.Owing to selected to have controlled the above-mentioned crucial factor of production well, make the preparation that Silver Nitrate purity height, the foreign matter content with the present invention's preparation is little, be used for film emulsion, light sensitivity is good, fog density is low.Disposable crystallization can reach photographic-grade Silver Nitrate standard.And production cost is low, life cycle of the product is short, productive rate is high, rate of loss is little.
Claims (2)
1. the method for a preparing photographic-grade silver nitrate through one-time crystallization is characterized in that, it may further comprise the steps:
A. get GB 1
#12～18 kilograms on silver ingot is put into reactor, adds 11～16 liters of 60～70% concentrated nitric acids then in the reactor;
B. reactor heating, solution temperature is raise gradually, when reaching 60 ℃, react violent gradually, lasting heating reaches between 80～90 ℃ solution temperature, and it is fully reacted, after reaction finishes, continue heating 2-3 hour, till can't see oxynitride and overflowing, make the pH value of solution in 1～2 scope;
C. the above-mentioned solution that makes is changed over to and have the assorted of whipping appts and stir with 50 rev/mins rotating speeds except in the container, in the process that stirs, add silver suboxide, add-on is 50～70 grams, when the pH of solution value is 7.5～8.5, stop to stir 4～6 hours after-filtration of natural sedimentation;
D. the solution after will filtering is put into vaporizer, in solution, add 10～20 gram analytical pure nitric acid, 110～130 ℃ of thickening temperatures, concentrate about 2.5～3.5 hours, when solution surface forms tunica albuginea and be sticking slightly vaporizer inwall state, stop heating, solution is put into crystallizing tank, spontaneous nucleation is 10～15 hours under 5～15 ℃ of temperature, separates with whizzer;
E. separate the vacuum-drying 4～6 hours under 80～100 ℃ of temperature of back gained solid nitric acid silver, get silver nitrate crystal.
2. the method for preparing photographic-grade silver nitrate through one-time crystallization as claimed in claim 1 is characterized in that, it may further comprise the steps:
A. get GB 1
#15 kilograms on silver ingot is put into reactor, adds 13.5 liters of 65% concentrated nitric acids then in the reactor;
B. reactor heating, solution temperature is raise gradually, when reaching 60 ℃, react violent gradually, lasting heating reaches between 80～90 ℃ solution temperature, and it is fully reacted, after reaction finishes, continue heating 2-3 hour, till can't see oxynitride and overflowing, make the pH value of solution in 1～2 scope;
C. the above-mentioned solution that makes is changed over to and have the assorted of whipping appts and stir with 50 rev/mins rotating speeds except in the container, add silver suboxide in the process that stirs, add-on is 60 grams, when the pH of solution value is 8, stops stirring, 5 hours after-filtration of natural sedimentation;
D. the solution after will filtering is put into vaporizer, in solution, add 15 gram analytical pure nitric acid, 120 ℃ of thickening temperatures, concentrate about 3 hours, when solution surface forms tunica albuginea and be sticking slightly vaporizer inwall state, stop heating, solution is put into crystallizing tank, spontaneous nucleation is 12 hours under 10 ℃ of temperature, separates with whizzer;
E. separate the vacuum-drying 5 hours under 90 ℃ of temperature of back gained solid nitric acid silver, get silver nitrate crystal.
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| CN 200910065936 CN101628730B (en) | 2009-08-26 | 2009-08-26 | Method for preparing photographic-grade silver nitrate through one-time crystallization |
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| CN 200910065936 CN101628730B (en) | 2009-08-26 | 2009-08-26 | Method for preparing photographic-grade silver nitrate through one-time crystallization |
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| CN101628730B true CN101628730B (en) | 2013-09-11 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103214022B (en) * | 2013-04-12 | 2015-01-07 | 西陇化工股份有限公司 | Method for preparing high-purity silver nitrate |
| CN106044839A (en) * | 2016-08-23 | 2016-10-26 | 太仓沪试试剂有限公司 | Silver nitrate purification method |
| CN115108577B (en) * | 2022-06-28 | 2024-04-19 | 桐柏泓鑫新材料有限公司 | Low-energy-consumption preparation method and system for high-purity silver nitrate |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3554883A (en) * | 1968-06-06 | 1971-01-12 | Eastman Kodak Co | Method of purifying aqueous silver nitrate solutions |
| CN1073412A (en) * | 1992-11-04 | 1993-06-23 | 四川省环境保护科研监测所 | The pollution-free method for preparing silver nitrate solution |
| JP2587313B2 (en) * | 1990-07-19 | 1997-03-05 | 富士写真フイルム株式会社 | Activated alumina for removing heavy metals and method for producing silver nitrate using the same |
| CN1386707A (en) * | 2001-05-18 | 2002-12-25 | 广东省三水市鑫荣华实业发展有限公司 | Process for preparing high-purity silver nitrate crystal |
| CN101367542A (en) * | 2008-07-31 | 2009-02-18 | 常州市武进庙桥第二化工有限公司 | Preparation method for high purity silver nitrate |
-
2009
- 2009-08-26 CN CN 200910065936 patent/CN101628730B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3554883A (en) * | 1968-06-06 | 1971-01-12 | Eastman Kodak Co | Method of purifying aqueous silver nitrate solutions |
| JP2587313B2 (en) * | 1990-07-19 | 1997-03-05 | 富士写真フイルム株式会社 | Activated alumina for removing heavy metals and method for producing silver nitrate using the same |
| CN1073412A (en) * | 1992-11-04 | 1993-06-23 | 四川省环境保护科研监测所 | The pollution-free method for preparing silver nitrate solution |
| CN1386707A (en) * | 2001-05-18 | 2002-12-25 | 广东省三水市鑫荣华实业发展有限公司 | Process for preparing high-purity silver nitrate crystal |
| CN101367542A (en) * | 2008-07-31 | 2009-02-18 | 常州市武进庙桥第二化工有限公司 | Preparation method for high purity silver nitrate |
Non-Patent Citations (2)
| Title |
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| 张圣南等.高纯硝酸银的工业制备及生产过程控制.《湖南有色金属》.2006,第22卷(第4期),25-27. |
| 高纯硝酸银的工业制备及生产过程控制;张圣南等;《湖南有色金属》;20060831;第22卷(第4期);25-27 * |
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Effective date of registration: 20141128 Address after: 474750 Chengdong Development Zone, Tongbai County, Henan Province Patentee after: Tongbai Xinhong Silver Products Co., Ltd. Patentee after: State Grid Corporation of China Patentee after: Zhoukou Power Supply Company of State Grid Henan Electric Power Company Address before: 474750 Chengdong Development Zone, Tongbai County, Henan, Nanyang Patentee before: Tongbai Xinhong Silver Products Co., Ltd. |
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