CN1143900C - Refined platinum producing process - Google Patents
Refined platinum producing process Download PDFInfo
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- CN1143900C CN1143900C CNB011360992A CN01136099A CN1143900C CN 1143900 C CN1143900 C CN 1143900C CN B011360992 A CNB011360992 A CN B011360992A CN 01136099 A CN01136099 A CN 01136099A CN 1143900 C CN1143900 C CN 1143900C
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- platinum
- solution
- ammonium
- ammonium chloride
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 103
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 32
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 35
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 23
- 238000001556 precipitation Methods 0.000 claims abstract description 23
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 17
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 6
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001354 calcination Methods 0.000 claims abstract description 5
- CABDFQZZWFMZOD-UHFFFAOYSA-N hydrogen peroxide;hydrochloride Chemical compound Cl.OO CABDFQZZWFMZOD-UHFFFAOYSA-N 0.000 claims abstract description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 19
- 239000000047 product Substances 0.000 claims description 13
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000004090 dissolution Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 238000007865 diluting Methods 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000005272 metallurgy Methods 0.000 abstract 1
- 229910000510 noble metal Inorganic materials 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 8
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 5
- 238000001704 evaporation Methods 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000006188 syrup Substances 0.000 description 1
- 235000020357 syrup Nutrition 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The present invention provides a refined platinum producing process which relates to a noble metal wet metallurgy process. The present invention comprises the processes that coarse ammonium chloroplatinate is dissolved in a sodium hydroxide solution, hydrazine hydrate is added for reduction, platinum black is filtered and is dissolved by hydrochloric acid hydrogen peroxide, ammonium chloride is added for the fractional precipitation of the platinum in an ammonium chloroplatinate state according to the theoretic amount of 20 to 80%, and spongy platinum is obtained via conventional calcination. The method of the present invention has the advantages of short technological cycle, lower production cost than traditional production methods, low energy consumption and good operating condition and can simultaneously produce products with different quality according to market demand.
Description
(I) technical field
A process for producing refined platinum relates to a precious metal hydrometallurgy process, in particular to an improvement of a purification process of ammonium chloroplatinate in platinum production.
(II) background of the invention
Conventional platinum refining processes, usually byOne part volume of nitric acid HNO3Mixing with three parts of HCl (aqua regia) under boiling to remove impure crude ammonium chloroplatinate [ (NH)4)2PtCl6]The dissolution was carried out, the following reaction took place:
in order to completely dissolve ammonium chloroplatinate, more than 5-6 times of aqua regia must be added, and the aqua regia must be prepared at present, and the whole dissolving time is at least more than 6 hours. For removing nitrate NO from dissolved platinum solution3 -The operation of completely evaporating the solution to near dryness and adding diluted hydrochloric acid after thickening like syrup must be repeated for more than three times. Will finally be nitrate-free NO3 -Adding dilute hydrochloric acid into the solution, heating and boiling to obtain a platinum dissolved solution, cooling, filtering, adding ammonium chloride to precipitate pure (NH)4)2PtCl6The reaction is as follows:
the above-mentioned aqua regia dissolving-evaporating to remove nitre-dilute hydrochloric acid dissolving-ammonium chloride precipitating process is repeated three times to obtain pure (NH)4)2PtCl6After calcination, pure 99.99% spongy platinum is produced.
Because the traditional platinum refining process adopts aqua regia as a solvent, the time of the dissolving process is long, at least 72 hours are needed from crude ammonium platinate chloride to high-purity platinum, and each process needs to be heated, so the energy consumption is high, the reagent dosage is large, and the labor condition is poor.
Disclosure of the invention
The invention aims to overcome the defects of the prior art and provide a novel process for producing and refining platinum, which can effectively reduce the dissolving time, reduce the energy consumption and save the reagent dosage.
The purpose of the invention is realized by the following technical scheme.
A process for producing refined platinum is characterized by comprising the following steps:
a. dissolving crude ammonium chloroplatinate with 1M-5M NaOH solution, and filtering off a small amount of insoluble substances;
b. adding hydrazine hydrate into the platinum solution for reduction, and immediately filtering out platinum black and washing with pure water when judging that Pt in the solution is completely precipitated;
c. dissolving the obtained platinum black by using hydrogen peroxide hydrochloride to obtain platinum black, slurrying the platinum black by using pure water, adding hydrochloric acid under the condition of stirring, adding hydrogen peroxide, wherein the ratio of the added hydrochloric acid to the hydrogen peroxide is 1: 1 until the platinum black is completely dissolved, continuously heating and boiling after the dissolution is finished to evaporate residual HCl, then diluting the solution byusing the pure water to control the concentration of platinum in the solution to be 80-160g/l, cooling, filtering, and filtering out insoluble substances;
d. using ammonium chloride to perform fractional precipitation;
under the condition that the solution is heated and boiled, ammonium chloride is added according to 20% -80% of theoretical amount to enable platinum to be subjected to first-step precipitation by ammonium chloroplatinate, and an ammonium chloroplatinate product with high purity is obtained; adding ammonium chloride into the platinum-containing solution after the first-step precipitation to completely precipitate the platinum-containing solution to obtain ammonium chloroplatinate with lower purity;
e. obtaining sponge platinum by a conventional calcination method.
The method adopts the process of dissolving the platinum chloride by the sodium hydroxide to prepare the refined platinum, has short process period, has important significance for extremely high-value platinum metal and acceleration of capital, only needs 16 hours when the platinum chloride is put into production of the sponge platinum product, has lower production cost than the traditional production method, has low energy consumption and good operation condition, and can simultaneously produce products with different qualities according to market demands.
(IV) detailed description of the preferred embodiments
The process of the present invention is further illustrated below with reference to examples.
a. Firstly, dissolving crude ammonium chloroplatinate by using a sodium hydroxide (NaOH) solution with the concentration of 1M-5M, and filtering a small amount of insoluble substances; the reaction formula is as follows:
the operating process conditions are as follows: crude ammonium chloroplatinate is placed in a container, and the requirement on the container is low due to no need of heating, and the container is only a common plastic container; then adding NaOH solution, generally having a concentration of 1m-2m, if the treatment capacity is large, increasing the concentration, dissolving at room temperature under stirring, adding NaOH while dissolving, and stopping adding NaOH after dissolving. The dissolution process is very rapid and can be completed in a few minutes. If the throughput is small, it can be completed in a few seconds. After dissolution, the mixture was filtered to remove a small amount of insoluble matter, and the filtrate was sent to the reduction step.
b. The platinum solution is then reduced with hydrazine hydrate, the reaction formula is:
the reduction is carried out at room temperature with stirring, and due to the rapid and violent reaction, the hydrazine hydrate is slowly added in an amount which can be calculated theoretically, but the actual amount is more than the theoretical amount. When the pt in the solution was judged to have completely precipitated by the rapid test method, no hydrazine hydrate was added. Immediately after the reduction, the platinum black was filtered off and washed with pure water, and then transferred to an acid-resistant and heatable vessel for the next dissolution operation. The reduction operation can be completed within 30-40 minutes.
c. Dissolving platinum black by hydrogen peroxide hydrochloride, wherein the reaction formula is as follows:
during operation, the platinum black is slurried by pure water, then hydrochloric acid is added under the condition of stirring, and then hydrogen peroxide is added, wherein the ratio of hydrogen peroxide to hydrochloric acid is 1: 1. Since the platinum black is in a fresh state, is easily dissolved, the reaction is rapid and violent, when the reaction is slow, heating is carried out and HCl and H are added2O2And (3) continuously heating and boiling until the platinum black is completely dissolved, evaporating residual HCl after the dissolution is finished, diluting the solution by pure water to control the concentration of platinum in the solution to be 80-160g/l, cooling, filtering insoluble substances, and allowing the filtrate to enter the next process. This process takes about 3-4 hours.
d. Using ammonium chloride to perform fractional precipitation; under the condition that the solution is heated and boiled, adding ammonium chloride to precipitate platinum as ammonium chloroplatinate according to 20% -80% of theoretical amount, wherein the obtained first batch of ammonium chloroplatinate is a product with higher purity; and adding ammonium chloride into the platinum-containing solution after the first-step precipitation to ensure that the ammonium chloroplatinate obtained by complete precipitation has lower purity. Obtaining sponge platinum by a conventional calcination method.
The process of the present invention is further illustrated below with reference to examples.
Example one
The platinum solution processed by the processes of a, b and c of the crude ammonium chloroplatinate comprises the following components: pd0.179g/l, Au less than 0.005g/l, Rh0.625g/l, Ir0.220g/l and Pt146g/l, adding ammonium chloride according to 20% of theoretical amount to make precipitation, the precipitation rate of platinum is 18%, the quality purity of obtained product is 99.99% and the purity of product obtained by two-step complete precipitation is 99.9%.
Example two
The platinum solution obtained after the crude ammonium chloroplatinate is processed by the processes of a, b and c comprises the following components: pd0.0028g/l, Au<0.0005g/l, Rh0.059g/l, Ir0.00712g/l and Pt160g/l, wherein ammonium chloride is added according to 80% of theoretical amount, the precipitation rate of platinum is-80%, the purity of the obtained product is 99.99%, and the purity of the product obtained by two-step complete precipitation is more than 99.9%.
Example three
The platinum solution obtained after the crude ammonium chloroplatinate is processed by the processes of a, b and c has the same components as the example I, but pure water is added before ammonium chloride is added for precipitation to increase the volume by one time, namely the platinum concentration is controlled to be 73g/l, the ammonium chloride is added according to 60 percent of theoretical amount in the first-step precipitation, the precipitation rate is 57 percent, the purity of the obtained product is 99.99 percent, and the purity of the product obtained by the second-step complete precipitation is more than 99.9 percent.
Example four
The solution obtained after the crude ammonium chloroplatinate is processed by the processes of a, b and c has the same components as the second example, but pure water is added before ammonium chloride is added for precipitation to increase the volume by one time, the platinum concentration is controlled to be 80g/l, the ammonium chloride is added into the first step of precipitation according to 90 percent of theoretical amount, the precipitation rate is 88.5 percent, the purity of the obtained product is 99.992 percent, and the purity of the product obtained by the second step of complete precipitation is 99.985 percent.
Claims (1)
1. A process for producing refined platinum is characterized by comprising the following steps:
a. dissolving crude ammonium chloroplatinate with 1M-5M NaOH solution, and filtering off a small amount of insoluble substances;
b. adding hydrazine hydrate into the platinum solution for reduction, and immediately filtering out platinum black and washing with pure water when judging that Pt in the solution is completely precipitated;
c. dissolving the obtained platinum black by using hydrogen peroxide hydrochloride to obtain platinum black, slurrying the platinum black by using pure water, adding hydrochloric acid under the condition of stirring, adding hydrogen peroxide, wherein the ratio of the added hydrochloric acid to the hydrogen peroxide is 1: 1 until the platinum black is completely dissolved, continuously heating and boiling after the dissolution is finished to evaporate residual HCl, then diluting the solution by using the pure water to control the concentration of platinum in the solution to be 80-160g/l, cooling, filtering, and filtering out insoluble substances;
D. using ammonium chloride to perform fractional precipitation;
under the condition that the solution is heated and boiled, ammonium chloride is added according to 20% -80% of theoretical amount to enable platinum to be subjected to first-step precipitation by ammonium chloroplatinate, and an ammonium chloroplatinate product with high purity is obtained; adding ammonium chloride into the platinum-containing solution after the first-step precipitation to completely precipitate the platinum-containing solution to obtain ammonium chloroplatinate with lower purity;
e. obtaining sponge platinum by a conventional calcination method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011360992A CN1143900C (en) | 2001-10-09 | 2001-10-09 | Refined platinum producing process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011360992A CN1143900C (en) | 2001-10-09 | 2001-10-09 | Refined platinum producing process |
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| CN1370845A CN1370845A (en) | 2002-09-25 |
| CN1143900C true CN1143900C (en) | 2004-03-31 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB011360992A Expired - Fee Related CN1143900C (en) | 2001-10-09 | 2001-10-09 | Refined platinum producing process |
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| CN108655415A (en) * | 2018-06-20 | 2018-10-16 | 南京东锐铂业有限公司 | A kind of new process preparing high-purity platinum |
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| CN110964919A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Preparation method of spongy platinum |
| CN110964920A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Method for recovering refined platinum from crude ammonium chloroplatinate |
| CN110964922A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Method for recovering refined platinum from crude ammonium chloroplatinate |
| CN110482618A (en) * | 2019-08-13 | 2019-11-22 | 中船重工黄冈贵金属有限公司 | A kind of synthetic method of no nitre chloroplatinic acid |
| CN111690819A (en) * | 2020-06-24 | 2020-09-22 | 广东金正龙科技有限公司 | Platinum purification method and reaction kettle |
| CN111534700A (en) * | 2020-06-24 | 2020-08-14 | 广东金正龙科技有限公司 | Method for recovering residual precious metals in platinum purification wastewater |
| CN114717418B (en) * | 2022-02-24 | 2024-02-23 | 阳谷祥光铜业有限公司 | Method for extracting high-purity sponge platinum from platinum waste liquid |
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- 2001-10-09 CN CNB011360992A patent/CN1143900C/en not_active Expired - Fee Related
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Assignee: Taiyuan Huagui Metal Co., Ltd. Assignor: Jinchuan Group Corp., Ltd. Contract fulfillment period: 2007.3.25 to 2012.3.26 Contract record no.: 2010990000044 Denomination of invention: Refined platinum producing process Granted publication date: 20040331 License type: Exclusive license Record date: 2010.1.27 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2007.3.25 TO 2012.3.26; CHANGE OF CONTRACT Name of requester: TAIYUAN HUAGUI PRECIOUS METAL CO.,LTD. Effective date: 20100127 |
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Address after: 737103 Jinchang City, Gansu province Jinchuan Non-ferrous Metals Company Patentee after: Jinchuan Group Co., Ltd. Address before: 737103 Jinchang City, Gansu province Jinchuan Non-ferrous Metals Company Patentee before: Jinchuan Group Corp., Ltd. |
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