CN114604911B - Method for removing potassium and sodium from ammonium chloroplatinate product - Google Patents
Method for removing potassium and sodium from ammonium chloroplatinate product Download PDFInfo
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- CN114604911B CN114604911B CN202210217986.2A CN202210217986A CN114604911B CN 114604911 B CN114604911 B CN 114604911B CN 202210217986 A CN202210217986 A CN 202210217986A CN 114604911 B CN114604911 B CN 114604911B
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- potassium
- sodium
- ammonium
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- remover
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- 239000011734 sodium Substances 0.000 title claims abstract description 43
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 title claims abstract description 41
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 title claims abstract description 36
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910052700 potassium Inorganic materials 0.000 title claims abstract description 36
- 239000011591 potassium Substances 0.000 title claims abstract description 36
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 17
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 14
- 235000012501 ammonium carbonate Nutrition 0.000 claims abstract description 14
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 claims description 23
- 238000005406 washing Methods 0.000 claims description 23
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 20
- 235000019270 ammonium chloride Nutrition 0.000 claims description 10
- 238000009835 boiling Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000007921 spray Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 210000003298 dental enamel Anatomy 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 abstract description 4
- 229910000027 potassium carbonate Inorganic materials 0.000 abstract description 2
- 239000002244 precipitate Substances 0.000 abstract description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 31
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 12
- 229910052697 platinum Inorganic materials 0.000 description 6
- 229910000510 noble metal Inorganic materials 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
- C01G55/002—Compounds containing, besides ruthenium, rhodium, palladium, osmium, iridium, or platinum, two or more other elements, with the exception of oxygen or hydrogen
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention provides a method for removing potassium and sodium from ammonium chloroplatinate, which adopts ammonium carbonate as the main component of a remover to lead CO in the ammonium carbonate 3 2‑ With K in ammonium chloroplatinate + And Na (Na) + The impurities combine to form soluble potassium carbonate and sodium carbonate, which contain NH 4 + With PtCl 6 2‑ The ammonium chloroplatinate precipitate is formed by combination, and potassium and sodium impurities are washed and removed. The invention has the characteristics of not increasing the process flow and not introducing new impurities, and is convenient and effective.
Description
Technical Field
The invention belongs to the technical field of noble metal purification, and relates to a method for removing potassium and sodium from an ammonium chloroplatinate product.
Background
Noble metal elements are widely applied to the fields of strategic materials such as electronics, medical treatment, aerospace and the like, and have important significance in the aspect of resource guarantee, and economic value cannot be ignored. The noble metal salt products such as ammonium chloroplatinate and the like are very important as intermediate products in the noble metal element purification process.
When refining and purifying platinum at home and abroad, a qualified platinum product is mostly obtained by adopting a process of chloridizing dissolution, extraction separation, refining and purifying. In the preparation of ammonium chloroplatinate, the front-end process needs to use a chemical reagent containing potassium and sodium for refining and purification, so that potassium and sodium enter a platinum solution and are accumulated continuously, a large amount of potassium and sodium are accumulated in the ammonium chloroplatinate finally, and the potassium and sodium can be enriched again in high power when the ammonium chloroplatinate is calcined to prepare the corresponding sponge platinum. Although the related requirements on the content of potassium and sodium in the ammonium chloroplatinate product are not made in the 2015 national standard, the existence of potassium and sodium impurities in the ammonium chloroplatinate can lead to the product reaching the purity requirement of less than 99.99%, so that the quality of the product is reduced and the influence is extremely bad.
Disclosure of Invention
The invention aims to solve the problems in the prior art, and provides a method for removing potassium and sodium from ammonium chloroplatinate products, which solves the problem of product quality degradation caused by higher potassium and sodium impurities in ammonium chloroplatinate.
The invention adopts ammonium carbonate as the main component of the remover to lead CO in the ammonium carbonate 3 2- With K in ammonium chloroplatinate + And Na (Na) + The impurities combine to form soluble potassium carbonate and sodium carbonate which enter the wash liquor, while they contain NH 4 + With PtCl 6 2- The ammonium chloroplatinate precipitate is formed by combination, and potassium and sodium impurities are washed and removed. The invention does not increase the process flow and introduce new impurities, and is convenient and effective.
The reaction equation involved in the invention is:
K 2 PtCl 6 +（NH 4 ） 2 CO 3 =（NH 4 ） 2 PtCl 6 ↓+K 2 CO 3
and Na (Na) 2 PtCl 6 +（NH 4 ） 2 CO 3 =（NH 4 ） 2 PtCl 6 ↓+Na 2 CO 3 。
For this purpose, the invention adopts the following technical scheme:
a method for removing potassium and sodium from an ammonium chloroplatinate product, comprising the steps of:
a. preparing a potassium sodium remover: adding a certain amount of pure water into ammonium carbonate and ammonium chloride, controlling the mass fraction of the ammonium carbonate in the solution to be 5-10% and the mass fraction of the ammonium chloride to be 8-12%, heating, boiling and dissolving in an enamel reaction kettle or a glass beaker until the solution is clear, cooling to 45-55 ℃ and filtering to obtain a potassium-sodium remover;
b. washing products: according to m Ammonium chloroplatinate product ：V Potassium sodium remover The solid-to-liquid ratio of 1:3.5-4.5, measuring potassium-sodium remover, keeping the temperature of the potassium-sodium remover at 30-40 ℃, and then uniformly mixing 70-80% of the potassium-sodium removerSpraying the solution on the surface of an ammonium chloroplatinate product for spray washing, and finally, rapidly washing the ammonium chloroplatinate product with the rest of 20-30% of potassium and sodium remover for one time to remove more than 90% of potassium and sodium in the ammonium chloroplatinate product at one time.
The invention has the beneficial effects that:
1. the method can remove potassium and sodium in the ammonium chloroplatinate product at one time without introducing new impurities, and is simple to operate, convenient and effective;
2. the removal rate of potassium and sodium can reach more than 90%, the loss rate of platinum is lower than 0.1%, the removal rate of potassium and sodium is high, and the loss of platinum is less;
3. the invention is easy to realize industrialized production, has no influence on normal process connection and has strong operability.
Drawings
FIG. 1 is a flow chart of the steps of the present invention.
Detailed Description
The technical scheme of the invention is described in the following with reference to the accompanying drawings and the implementation method.
Example 1:
as shown in fig. 1, a method for removing potassium and sodium from an ammonium chloroplatinate product comprises the following steps:
a. taking an ammonium chloroplatinate product 103 g containing potassium and sodium, preparing a potassium and sodium remover of 412 mL according to the requirement, adding 24.72g of ammonium carbonate and 41.20 g of ammonium chloride into a beaker, adding pure water to a total volume of 412 mL, controlling the mass fraction of the system ammonium carbonate to be 6% and the mass fraction of the ammonium chloride to be 10%, heating and boiling, dissolving until the solution is clear, cooling to 49 ℃ and filtering to prepare the potassium and sodium remover;
b. and (3) keeping the temperature of the potassium-sodium remover at 35 ℃, uniformly spraying 310 mL potassium-sodium remover on the surface of the ammonium chloroplatinate product for spray washing, and then rapidly washing once by using 102 ml potassium-sodium remover to finish washing, thereby obtaining the ammonium chloroplatinate refined product 102.781 g.
The implementation effect is as follows:
the content of the detected and analyzed elements of the decomposition products calcined at 800℃before and after the ammonium chloroplatinate washing is shown in Table 1, and it is found that the removal rate of potassium was 90.33% and the removal rate of sodium was 91.99%.
TABLE 1
| Element(s) | K | Na |
| Before washing (%) | 0.0890 | 0.1461 |
| Post-washing (%) | 0.0086 | 0.0117 |
| Removal rate (%) | 90.33 | 91.99 |
Example 2:
a method for removing potassium and sodium from an ammonium chloroplatinate product, comprising the steps of:
a. taking an ammonium chloroplatinate product 157 g containing potassium and sodium, preparing a potassium and sodium remover of 660 mL according to the requirement, adding 50.24 g ammonium carbonate and 62.80 g ammonium chloride into a beaker, adding pure water to the total volume of 660 mL, controlling the mass fraction of the ammonium carbonate of the system to be 7.61% and the mass fraction of the ammonium chloride to be 9.51%, heating, boiling, dissolving until the solution is clear, cooling to 51 ℃, and filtering to prepare the potassium and sodium remover;
b. and (3) maintaining the temperature of the potassium-sodium remover at 36 ℃, uniformly spraying the 500 mL potassium-sodium remover on the surface of the ammonium chloroplatinate product for spray washing, and then rapidly washing once by using the 160 ml potassium-sodium remover to finish washing to obtain the ammonium chloroplatinate refined product 156.6546 g.
The implementation effect is as follows:
the content of the detected and analyzed elements of the decomposition products calcined at 800℃before and after washing of ammonium chloroplatinate is shown in Table 2, and it is found that the removal rate of potassium was 90.77% and the removal rate of sodium was 92.53%.
TABLE 2
| Element(s) | K | Na |
| Before washing (%) | 0.0921 | 0.1365 |
| Post-washing (%) | 0.0085 | 0.0102 |
| Removal rate (%) | 90.77 | 92.53 |
Example 3:
a method for removing potassium and sodium from an ammonium chloroplatinate product, comprising the steps of:
a. providing 2400 g ammonium chloroplatinate product containing potassium and sodium, preparing 10000 mL potassium and sodium remover according to the requirement, adding 800 g ammonium carbonate and 1000 g ammonium chloride into a beaker, adding pure water to the total volume of 10000 mL, controlling the mass fraction of system ammonium carbonate to be 8% and the mass fraction of ammonium chloride to be 10%, heating and boiling, dissolving until the solution is clear, cooling to 46 ℃ and filtering to prepare the potassium and sodium remover;
b. and (3) keeping the temperature of the potassium-sodium remover at 33 ℃, uniformly spraying 7500 and mL potassium-sodium remover on the surface of the ammonium chloroplatinate product for spray washing, and then rapidly washing once by using 2500 and ml potassium-sodium remover to finish washing, thereby obtaining the ammonium chloroplatinate refined product 2394.2976 g.
The implementation effect is as follows:
the content of the detected and analyzed elements of the decomposition products calcined at 800℃before and after washing of ammonium chloroplatinate is shown in Table 3, and it is found that the removal rate of potassium was 92.96% and the removal rate of sodium was 94.32%.
TABLE 3 Table 3
| Element(s) | K | Na |
| Before washing (%) | 0.1123 | 0.1578 |
| Post-washing (%) | 0.0079 | 0.0091 |
| Removal rate (%) | 92.96 | 94.23 |
Claims (1)
1. A method for removing potassium and sodium from an ammonium chloroplatinate product, comprising the steps of:
a. preparing a potassium sodium remover: adding a certain amount of pure water into ammonium carbonate and ammonium chloride, controlling the mass fraction of the ammonium carbonate in the solution to be 5-10% and the mass fraction of the ammonium chloride to be 8-12%, heating, boiling and dissolving in an enamel reaction kettle or a glass beaker until the solution is clear, cooling to 45-55 ℃ and filtering to obtain a potassium-sodium remover;
b. washing products: according to m Ammonium chloroplatinate product ：V Potassium sodium remover The solid-to-liquid ratio of 1:3.5-4.5 is measured, a potassium-sodium remover is measured, the temperature of the potassium-sodium remover is kept at 30-40 ℃, then 70-80% of the potassium-sodium remover is uniformly sprayed on the surface of an ammonium chloroplatinate product for spray washing, and finally, the potassium-sodium remover with the residual content of 20-30% is rapidly washed once, so that more than 90% of potassium-sodium in the ammonium chloroplatinate product can be removed at one time.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210217986.2A CN114604911B (en) | 2022-03-08 | 2022-03-08 | Method for removing potassium and sodium from ammonium chloroplatinate product |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210217986.2A CN114604911B (en) | 2022-03-08 | 2022-03-08 | Method for removing potassium and sodium from ammonium chloroplatinate product |
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| Publication Number | Publication Date |
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| CN114604911A CN114604911A (en) | 2022-06-10 |
| CN114604911B true CN114604911B (en) | 2023-09-22 |
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Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02294416A (en) * | 1989-05-09 | 1990-12-05 | Ishifuku Kinzoku Kogyo Kk | Production of platinum powder |
| JP2003129145A (en) * | 2001-10-22 | 2003-05-08 | Nikko Materials Co Ltd | Method for recovering platinum |
| JP2008106349A (en) * | 2006-09-28 | 2008-05-08 | Kojima Kagaku Yakuhin Kk | Method for producing platinum powder |
| CN103484687A (en) * | 2013-10-11 | 2014-01-01 | 金川集团股份有限公司 | Platinum refining technology |
| CN104889413A (en) * | 2015-05-13 | 2015-09-09 | 贵研铂业股份有限公司 | Method for preparing high purity platinum powder for electronic component |
| CN108929953A (en) * | 2018-08-15 | 2018-12-04 | 大冶有色金属有限责任公司 | A kind of platinum fining process |
| CN109234528A (en) * | 2018-11-09 | 2019-01-18 | 荆楚理工学院 | A kind of platinum refinery practice |
| RU2711762C1 (en) * | 2019-09-04 | 2020-01-22 | Игорь Владимирович Федосеев | Method of extracting platinum from an industrial salt of ammonium hexachloroplatinate |
| 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 |
| 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 |
| CN110964905A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Method for purifying 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 |
-
2022
- 2022-03-08 CN CN202210217986.2A patent/CN114604911B/en active Active
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02294416A (en) * | 1989-05-09 | 1990-12-05 | Ishifuku Kinzoku Kogyo Kk | Production of platinum powder |
| JP2003129145A (en) * | 2001-10-22 | 2003-05-08 | Nikko Materials Co Ltd | Method for recovering platinum |
| JP2008106349A (en) * | 2006-09-28 | 2008-05-08 | Kojima Kagaku Yakuhin Kk | Method for producing platinum powder |
| CN103484687A (en) * | 2013-10-11 | 2014-01-01 | 金川集团股份有限公司 | Platinum refining technology |
| CN104889413A (en) * | 2015-05-13 | 2015-09-09 | 贵研铂业股份有限公司 | Method for preparing high purity platinum powder for electronic component |
| CN108929953A (en) * | 2018-08-15 | 2018-12-04 | 大冶有色金属有限责任公司 | A kind of platinum fining process |
| 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 |
| 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 |
| CN110964905A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Method for purifying 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 |
| CN109234528A (en) * | 2018-11-09 | 2019-01-18 | 荆楚理工学院 | A kind of platinum refinery practice |
| RU2711762C1 (en) * | 2019-09-04 | 2020-01-22 | Игорь Владимирович Федосеев | Method of extracting platinum from an industrial salt of ammonium hexachloroplatinate |
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Effective date of registration: 20240508 Address after: 737199 No. 2 Jianshe Road, Jinchuan District, Jinchang City, Gansu Province (east of Beijing Road, west of Heya Road, south of Guiyang Road) Patentee after: Jinchuan Group Copper Gui Co.,Ltd. Country or region after: China Address before: No.98, Jinchuan Road, Jinchuan District, Jinchang City, Gansu Province 737100 Patentee before: JINCHUAN GROUP Co.,Ltd. Country or region before: China |