CN108128796A - A kind of environment-friendly preparation method thereof of high purity silver nitrate - Google Patents
A kind of environment-friendly preparation method thereof of high purity silver nitrate Download PDFInfo
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- CN108128796A CN108128796A CN201810210405.6A CN201810210405A CN108128796A CN 108128796 A CN108128796 A CN 108128796A CN 201810210405 A CN201810210405 A CN 201810210405A CN 108128796 A CN108128796 A CN 108128796A
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- silver nitrate
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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
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Abstract
The invention discloses a kind of environment-friendly preparation method thereofs of high purity silver nitrate, after metallic silver is cleaned surface with dust technology, are dissolved with 60 68% nitric acid of weight concentration, and the stoichiometric ratio of nitric acid and silver is 1.1 1.3, and reaction temperature is controllably 80 90 DEG C；After the reaction was complete, crystalline mother solution and cleaner are added in, silver oxide is added in and adjusts pH=6.5 ± 0.5 of solution or so, stand 0.5 1 hours, filtering and impurity removing；Filtrate temperature is reduced to 30 40 DEG C, and the high price foreign ion in silver nitrate solution, trapped fluid reuse are further removed using NF membrane；Purified silver nitrate solution temperature is down to 0 DEG C of crystallization below, filtering drying obtains finished product；Crystalline mother solution reuse.Method using the present invention can realize the stability contorting of trace impurity, prepare high-purity silver nitrate, and preparation process is generated without waste liquid.
Description
Technical field
The present invention relates to the environment-friendly preparation method thereof of high purity silver nitrate, particularly for high-purity in electronics industry, photosensitive material
Spend the preparation method of silver nitrate.
Background technology
Silver nitrate is water white transparency crystallization or white crystals.PH value of water solution is about 6.Silver nitrate is one in photosensitive industry
Kind important materials, purity, especially metal, the content of nonmetallic inclusion directly influence photosensitive effect.
Chinese patent application CN1386707A discloses a kind of preparation method of high-purity silver nitrate crystal, to the nitric acid of heating
Nitric acid is added in silver-colored solution, blasts gas, crystallisation by cooling.This method each metal impurities ion, nonmetallic inclusion content all
Reach more than 400-1000ppb.
The preparation method of high-purity silver nitrate disclosed in Chinese patent application CN101367542A, it is anti-with silver and dust technology
Ying Hou adds silver oxide, is cooled to -10 ± 2 DEG C, and impurities H oxide precipitation is precipitated, then condensing crystallizing, and it is pure that product reaches analysis
Or top pure grade.But the requirement that the purity of silver nitrate is made to reach photosensitive material is only difficult to by silver oxide removal of impurities.
Chinese patent application CN102040240A discloses a kind of method for producing high purity silver nitrate, with silver and dust technology
Reaction adds in cleaner magnesia, re-evaporation crystallization, 10-100ppb of silver nitrate impurity ion content of production after dilution.
Chinese patent application CN102040241A discloses a kind of production method for producing photographic-grade silver nitrate, by silver ingot with it is pure
Nitric acid reaction, reaction solution dilution add in impurity elimination agent magnesium carbonate, then condensing crystallizing, foreign metal ion reached 100ppb with
On.
Chinese patent application CN102285680A discloses a kind of preparation method of high purity silver nitrate, using silver nitrate as raw material,
In deionized water, activated carbon decolorizing is added in, using the earth silicon material mesoporous adsorbent through EDTA surface modifications, Ran Houjin
Row post processing, is prepared target product, heavy metal and precious metal impurity ion concentration are below the index value of 1ppm.
Chinese patent application CN 103214022 discloses a kind of preparation method of high purity silver nitrate, by the dense nitre of metallic silver
Acid is most of in the silver nitrate being prepared by evaporative crystallization by hydrolyzing coprecipitated removal foreign ion in 80-90 DEG C of dissolving
Foreign metal ion content drops to 10ppb hereinafter, the content for still still having partial impurities ion is higher than 10ppb.
Invention content
The purpose of the present invention is to provide a kind of environment-friendly preparation method thereof of the high purity silver nitrate of stabilization, by produced by the present invention
Silver nitrate foreign metal ion content reaches 10ppb hereinafter, and not generating waste liquid in preparation process.
Technical scheme is as follows, and flow diagram is shown in attached drawing 1：
A kind of environment-friendly preparation method thereof of high purity silver nitrate, which is characterized in that include the following steps：
(1) synthesis of silver nitrate：Metallic silver weight concentration 60-68% nitric acid is dissolved, the stoichiometry of nitric acid and silver
Than for 1.1-1.3, reaction temperature is controllably 80-90 DEG C；
(2) it cleans：After the reaction was complete, add in crystalline mother solution and cleaner, add in silver oxide adjust the pH=6.5 of solution ±
0.5 or so, 0.5-1 hours are stood, filtering and impurity removing；
(3) solution purification：Above-mentioned filtrate temperature is reduced to 30-40 DEG C, and it is molten that silver nitrate is then further removed using NF membrane
High price foreign ion in liquid, trapped fluid can be back to step (2)；
(4) it crystallizes, filter, drying：Purified silver nitrate solution temperature is down to 0 DEG C of crystallization below, filtering drying obtains
Finished product；Crystalline mother solution can be back to step (2).
Further, in step (2), after the reaction was complete, 80-90 DEG C is maintained, adds in crystalline mother solution and cleaner.
Further, in step (2), complex salt of the cleaner for aluminum nitrate and bismuth nitrate.
Further, the aluminum nitrate and bismuth nitrate mass ratio are 1:1.
According to the environment-friendly preparation method thereof of high purity silver nitrate of the present invention, in step (2), add in silver oxide powder adjust it is molten
The pH of liquid.
According to the environment-friendly preparation method thereof of high purity silver nitrate of the present invention, in step (2), it is most of to pass through silver oxide removal
Foreign ion in step (3), passes through nanofiltration technique and removes trace impurity ion.
According to the environment-friendly preparation method thereof of high purity silver nitrate of the present invention, further, in step (1), pure water can be added in.
According to the environment-friendly preparation method thereof of high purity silver nitrate of the present invention, in step (4), kept away by the reuse of crystalline mother solution
The generation of waste liquid is exempted from.
Specifically, the present invention provides a kind of environment-friendly preparation method thereof of high purity silver nitrate, include the following steps：
A. the synthesis of silver nitrate：Metallic silver weight concentration 60-68% nitric acid is dissolved, the stoichiometric ratio of nitric acid and silver
For 1.1-1.3, reaction temperature is controllably 80-90 DEG C；
B. it cleans：After the reaction was complete, 80-90 DEG C is maintained, crystalline mother solution and cleaner is added under stirring condition, adds in oxygen
Change silver powder and adjust pH=6.5 ± 0.5 of solution or so, after standing 0.5-2 hours, filtering and impurity removing；
C. solution purification：Above-mentioned filtrate temperature is reduced to 30-40 DEG C, then further removes silver nitrate solution using NF membrane
In high price foreign ion, to ensure in silver nitrate that impurity ion content is less than desired value；
D. it crystallizes：Purified silver nitrate solution temperature is down to 0 DEG C of crystallization below, crystalline mother solution is used for step B.
E. it filters, dry：The crystallization generated in crystallization process, it is filtered, dry to obtain finished product.
Advantageous effects of the present invention：
The impurity that the present invention carries out solution purification and ensure final products by introducing nanofiltration after removal step
Metal ion content is less than 10ppb, and realizes the reuse of crystalline mother solution, forms high purity silver nitrate green technology of preparing.
Description of the drawings
Fig. 1 is a kind of flow chart of the environment-friendly preparation method thereof of high purity silver nitrate of the present invention.
Specific embodiment
With reference to specific embodiment, the present invention is described in detail.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill to this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection domain.
Embodiment 1：A kind of environment-friendly preparation method thereof of high purity silver nitrate
A. it synthesizes：After silver ingot 200g is cleaned surface with dust technology, put into reaction kettle, add 100mL pure water, be slowly added to
The nitric acid 300g of 65wt%, 80-90 DEG C of controlling reaction temperature.After the reaction was complete, stop heating.
B. it cleans：Complex salt (aluminum nitrate and the bismuth nitrate mass ratio of cleaner aluminum nitrate and bismuth nitrate are added under stiring
It is 1:1) 1.2g adds the dilution of 100mL pure water, adds in silver oxide adjusting pH value of solution=6.5, crosses solution after standing 1 hour and filter out
It is miscellaneous.
C. solution purification：Above-mentioned filtrate cools to after 40 DEG C and further removes trace impurity by nanofiltration device.
D. freezing and crystallizing：Silver nitrate solution frozen cooling after will be refined crystallizes silver nitrate to -5 DEG C.
E. it filters, is dry：Centrifuge dripping will be crystallized, silver nitrate crystal is dried to obtain in 80 DEG C.
Foreign metal ion content detection result is as follows in product：
Instrument：ICP-MS (icp ms) unit：ppb
| Serial number | Detection project | Testing result |
| 1 | Bismuth (Bi) | 1.0 |
| 2 | Cadmium (Cd) | 1.5 |
| 3 | Chromium (Cr) | 5.0 |
| 4 | Copper (Cu) | 0.7 |
| 5 | Iron (Fe) | 3.6 |
| 6 | Mercury (Hg) | 0.1 |
| 7 | Manganese (Mn) | 1.4 |
| 8 | Nickel (Ni) | 4.1 |
| 9 | Lead (Pb) | 3.6 |
| 10 | Antimony (Sb) | 4.5 |
| 11 | Selenium (Se) | 6.3 |
| 12 | Tin (Sn) | 4.6 |
| 13 | Tellurium (Te) | 4.3 |
| 14 | Zinc (Zn) | 0.4 |
| 15 | Aluminium (Al) | 0.2 |
Embodiment 2：A kind of environment-friendly preparation method thereof of high purity silver nitrate
A. it synthesizes：After silver ingot 200g is cleaned surface with dust technology, put into reaction kettle, add 100mL pure water, be slowly added to
The nitric acid 300g of 65wt%, 80-90 DEG C of controlling reaction temperature.After the reaction was complete, stop heating.
B. it cleans：Complex salt (aluminum nitrate and the bismuth nitrate mass ratio of cleaner aluminum nitrate and bismuth nitrate are added under stiring
It is 1:1) 1.2g adds the nanofiltration retentate fluid in 1 step C of embodiment and the crystalline mother solution in step D, adds in silver oxide adjusting solution
PH=6.5, by solution filtering and impurity removing after standing 1 hour.
C. solution purification：Above-mentioned filtrate cools to after 40 DEG C and further removes trace impurity by nanofiltration device.
D. freezing and crystallizing：Silver nitrate solution frozen cooling after will be refined crystallizes silver nitrate to -5 DEG C.
E. it filters, is dry：Centrifuge dripping will be crystallized, silver nitrate crystal is dried to obtain in 80 DEG C.
Foreign metal ion content detection result is as follows in product：
Instrument：ICP-MS (icp ms) unit：ppb
| Serial number | Detection project | Testing result |
| 1 | Bismuth (Bi) | 1.1 |
| 2 | Cadmium (Cd) | 1.4 |
| 3 | Chromium (Cr) | 5.1 |
| 4 | Copper (Cu) | 0.8 |
| 5 | Iron (Fe) | 3.5 |
| 6 | Mercury (Hg) | 0.1 |
| 7 | Manganese (Mn) | 1.3 |
| 8 | Nickel (Ni) | 4.2 |
| 9 | Lead (Pb) | 3.2 |
| 10 | Antimony (Sb) | 4.7 |
| 11 | Selenium (Se) | 6.1 |
| 12 | Tin (Sn) | 4.7 |
| 13 | Tellurium (Te) | 4.5 |
| 14 | Zinc (Zn) | 0.5 |
| 15 | Aluminium (Al) | 0.3 |
In conclusion only presently preferred embodiments of the present invention, be not used for limiting the range that the present invention is implemented, it is all according to
The equivalent changes and modifications carried out by shape, construction, feature and spirit described in scope of the invention as claimed should all be included in this
In the right of invention.
Claims (8)
1. a kind of environment-friendly preparation method thereof of high purity silver nitrate, which is characterized in that include the following steps：
(1) synthesis of silver nitrate：Metallic silver weight concentration 60-68% nitric acid is dissolved, the stoichiometric ratio of nitric acid and silver is
1.1-1.3, reaction temperature are controllably 80-90 DEG C；
(2) it cleans：After the reaction was complete, crystalline mother solution and cleaner are added in, adds in pH=6.5 ± 0.5 that silver oxide adjusts solution
Left and right stands 0.5-1 hours, filtering and impurity removing；
(3) solution purification：Above-mentioned filtrate temperature is reduced to 30-40 DEG C, is then further removed in silver nitrate solution using NF membrane
High price foreign ion, trapped fluid can be back to step (2)；
(4) it crystallizes, filter, drying：Purified silver nitrate solution temperature is down to 0 DEG C of crystallization below, filtering drying obtains finished product；
Crystalline mother solution can be back to step (2).
2. the environment-friendly preparation method thereof of high purity silver nitrate according to claim 1, which is characterized in that in step (2), the reaction was complete
Afterwards, 80-90 DEG C is maintained, adds in crystalline mother solution and cleaner.
3. the environment-friendly preparation method thereof of high purity silver nitrate according to claim 1, which is characterized in that in step (2), the removal of impurities
Complex salt of the agent for aluminum nitrate and bismuth nitrate.
4. the environment-friendly preparation method thereof of high purity silver nitrate according to claim 3, which is characterized in that the aluminum nitrate and bismuth nitrate
Mass ratio is 1:1.
5. the environment-friendly preparation method thereof of high purity silver nitrate according to claim 1, which is characterized in that in step (2), add in oxidation
Silver powder adjusts the pH of solution.
6. the environment-friendly preparation method thereof of high purity silver nitrate according to claim 1, which is characterized in that in step (2), pass through oxidation
Silver removal most of foreign ion in step (3), passes through nanofiltration technique and removes trace impurity ion.
7. the environment-friendly preparation method thereof of high purity silver nitrate according to claim 1, which is characterized in that in step (1), can add in pure
Water.
8. the environment-friendly preparation method thereof of high purity silver nitrate according to claim 1, which is characterized in that in step (4), pass through crystallization
The reuse of mother liquor avoids the generation of waste liquid.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810210405.6A CN108128796A (en) | 2018-03-14 | 2018-03-14 | A kind of environment-friendly preparation method thereof of high purity silver nitrate |
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| CN201810210405.6A CN108128796A (en) | 2018-03-14 | 2018-03-14 | A kind of environment-friendly preparation method thereof of high purity silver nitrate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN111732120A (en) * | 2020-06-17 | 2020-10-02 | 中船重工黄冈贵金属有限公司 | Environment-friendly efficient production method of high-purity silver nitrate |
| CN112121751A (en) * | 2020-07-30 | 2020-12-25 | 广东先导稀材股份有限公司 | Nitrate removing device, nitrate removing system and nitrate removing method |
| CN113929130A (en) * | 2021-10-14 | 2022-01-14 | 太仓沪试试剂有限公司 | Method for removing impurities from silver nitrate |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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2018
- 2018-03-14 CN CN201810210405.6A patent/CN108128796A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 夏焕锦等: "纳滤膜去除硝酸银中痕量多价金属的研究", 《膜科技与技术》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN111732120A (en) * | 2020-06-17 | 2020-10-02 | 中船重工黄冈贵金属有限公司 | Environment-friendly efficient production method of high-purity silver nitrate |
| CN112121751A (en) * | 2020-07-30 | 2020-12-25 | 广东先导稀材股份有限公司 | Nitrate removing device, nitrate removing system and nitrate removing method |
| CN113929130A (en) * | 2021-10-14 | 2022-01-14 | 太仓沪试试剂有限公司 | Method for removing impurities from silver nitrate |
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Application publication date: 20180608 |
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