CN107838434B - Preparation method of high-purity platinum powder - Google Patents
Preparation method of high-purity platinum powder Download PDFInfo
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- CN107838434B CN107838434B CN201711037866.XA CN201711037866A CN107838434B CN 107838434 B CN107838434 B CN 107838434B CN 201711037866 A CN201711037866 A CN 201711037866A CN 107838434 B CN107838434 B CN 107838434B
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 41
- 239000012535 impurity Substances 0.000 claims abstract description 28
- 239000002253 acid Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 26
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000005406 washing Methods 0.000 claims abstract description 23
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 21
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 16
- 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 13
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 13
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 12
- 238000009835 boiling Methods 0.000 claims abstract description 11
- 239000000725 suspension Substances 0.000 claims abstract description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 150000001768 cations Chemical class 0.000 claims abstract description 6
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 6
- 238000005341 cation exchange Methods 0.000 claims abstract description 5
- 238000005342 ion exchange Methods 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims abstract description 4
- 230000001376 precipitating effect Effects 0.000 claims abstract 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 12
- 239000002244 precipitate Substances 0.000 claims description 11
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical group OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 7
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 4
- 239000003456 ion exchange resin Substances 0.000 claims description 4
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 4
- 150000002500 ions Chemical class 0.000 claims description 4
- 235000006408 oxalic acid Nutrition 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000003837 high-temperature calcination Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 abstract 5
- 238000009854 hydrometallurgy Methods 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 238000001556 precipitation Methods 0.000 description 4
- 238000001354 calcination Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910020437 K2PtCl6 Inorganic materials 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910002621 H2PtCl6 Inorganic materials 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000001036 glow-discharge mass spectrometry Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- -1 platinum group metals Chemical class 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
Abstract
The invention discloses a preparation method of ultra-pure platinum powder, which comprises the following steps: (1) precipitating platinum by ammonium chloride; (2) controlling potential reduction: precipitating ammonium chloroplatinate with deionized water to prepare a suspension, adding a reducing agent, and controlling the potential of the solution to reduce to obtain an ammonium platinochloride solution; (3) removing impurities by ion exchange: passing the ammonium platinochloride solution through a cation exchange column to further remove cation impurities to obtain a pure platinochloride solution; (4) deep reduction of chloroplatinic acid: adding hydrazine hydrate into the chloroplatinic acid solution for deep reduction, so that the platinum is reduced into a powder form; (5) acid boiling to remove impurities: and boiling and washing the obtained platinum powder with a mixed solution of nitric acid and hydrofluoric acid, fully washing with deionized water, and drying to obtain the high-purity platinum powder. The whole process of the invention adopts the conventional hydrometallurgy process technology, does not relate to the high-temperature calcination process, and has the advantages of low energy consumption, low cost, simple process, purity of more than 99.999 percent and the like.
Description
Technical Field
The invention relates to a preparation method of high-purity precious metal, in particular to a preparation method of high-purity platinum powder.
Background
The high-purity platinum has good chemical stability, high electrical conductivity and thermal conductivity, and unique electrical, magnetic, optical and other properties, is widely applied to industries such as national defense, military industry, satellites, electronics and the like, and the high-purity platinum powder becomes an indispensable and irreplaceable material for ensuring the properties of semiconductor devices and developing semiconductor technology. With the development of semiconductor technology and radio precision technology, the requirement for the purity of platinum metal is higher and higher. The presence of trace and even ultra trace impurities can affect the properties of the metal because the properties of the metal are often masked by the impurities in the event that the metal fails to reach a certain purity. At present, the domestic preparation method of high-purity platinum mainly adopts an ammonium chloroplatinate repeated precipitation method, and the platinum prepared by the method has low purity and cannot meet the requirements of modern scientific development. The foreign preparation of high-purity platinum is realized by a multi-purpose physical metallurgy method, such as pulling single crystal, and the like, and the method has large investment and complex operation.
The literature proposes that cation impurities in a platinum solution are removed by an ion exchange method, and high-purity platinum with the purity of 99.999 percent is obtained by chemical precipitation and calcination of a purified chloroplatinic acid solution. Patent EP1061145A1 discloses a process for preparing spongy platinum using K2PtCl6Obtaining H by ion exchange2PtCl6And reducing the solution by adopting hydrazine to obtain the spongy platinum, wherein the prepared spongy platinum has high potassium content. Is also disclosed in H2High temperature reduction K in gas stream2PtCl6The disadvantage of this process for the preparation of spongy platinum is the inclusion of potassium chloride in the platinum powder and the need for further washing treatments. Patent CN201410077800.3 discloses a process for preparing high purity platinum powders, by reacting K2PtCl6Dissolving in deionized water and passing through cation exchanger to obtain H2PtCl6Evaporating the solution on a rotary evaporator, adding hydrochloric acid into the obtained solution for acidification, slowly adding ammonium chloride solution, and stirring to obtain (NH)4)2PtCl6Settling, adding deionized water into the precipitate to prepare a suspension, adding hydrazine hydrate into the suspension for reduction to obtain spongy platinum, filtering and washing, and calcining the spongy platinum at 800 ℃ to obtain high-purity spongy platinum powder.
Disclosure of Invention
The invention aims to provide a preparation method of high-purity platinum powder aiming at the problems in the existing preparation of the high-purity platinum powder.
The preparation method of the high-purity platinum powder comprises the following steps:
(1) ammonium chloride precipitation of platinum: adding ammonium chloride into the chloroplatinic acid solution to generate ammonium chloroplatinate precipitate, and filtering and washing;
(2) controlling potential reduction: preparing ammonium chloroplatinate obtained in the step (1) into a suspension by using deionized water, slowly adding a reducing agent, controlling the potential of the solution to reduce, and filtering insoluble substances to obtain an ammonium chloroplatinate solution;
(3) cation exchange impurity removal: passing the ammonium platinochloride solution obtained in the step (2) through a cation exchange column to further remove cation impurities to obtain a pure platinochloride solution;
(4) deep reduction of chloroplatinic acid: adding hydrazine hydrate into the chloroplatinic acid solution obtained in the step (3) for deep reduction, so that platinum is reduced into a powder form;
(5) acid boiling to remove impurities: and (4) boiling and washing the platinum powder obtained in the step (4) by using nitric acid and hydrofluoric acid, fully washing the platinum powder by using deionized water, and drying the platinum powder in vacuum to obtain the high-purity platinum powder.
The invention has the advantages that the whole preparation process of the high-purity platinum powder adopts the conventional wet process technology, and the reagent used in the whole process does not contain metal impurity elements. The invention discloses a process for preparing high-purity platinum powder, which relates to four-stage impurity removal processes: ammonium chloride precipitation impurity removal, potential-controlled reduction impurity removal, ion exchange impurity removal, acid cooking washing impurity removal and good impurity element removal effect. In the whole process, adding ammonium chloride into a chloroplatinic acid solution to precipitate platinum to generate ammonium chloroplatinate, and filtering and washing to remove part of impurities in the solution; reducing ammonium chloroplatinate (IV) into soluble ammonium chloroplatinate (II) solution by controlling potential with sulfurous acid or oxalic acid, reducing gold, silver and the like into metals, not reducing other platinum group metals, filtering and separating to remove insoluble impurities; passing ammonium platinochloride through a cation exchange column to further remove cation impurities; and boiling and washing the platinum powder obtained by reduction by using nitric acid and hydrofluoric acid and washing by using deionized water, and effectively removing impurities such as hydrazine hydrate, silicon, alkali metal and the like, thereby obtaining the high-purity platinum powder. The preparation method is simple, compared with the traditional repeated precipitation and calcination process, the method has no high-temperature calcination process, and has the advantages of low energy consumption, low cost, high recovery rate, simple process and the like, and the purity of the obtained platinum powder is higher than 99.999%.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 is a schematic process flow diagram of the present invention.
Detailed Description
The invention is tested for a plurality of times in sequence, and the effect of the invention is further described and verified in detail by taking a part of test results as reference examples.
Example 1, referring to fig. 1, ammonium chloride was added to a chloroplatinic acid solution to generate an ammonium chloroplatinate precipitate, which was filtered and washed; preparing the generated ammonium chloroplatinate precipitate into a suspension by using deionized water, slowly adding sulfurous acid, wherein the molar ratio of the sulfurous acid to the ammonium chloroplatinate is 1.2, controlling the solution potential to be 0.68 +/-0.2V in the whole process, reducing the ammonium chloroplatinate into soluble ammonium chloroplatinate, filtering to remove insoluble substances, and passing the ammonium chloroplatinate solution through a three-stage 001 multiplied by 7 ion exchange resin column to remove impurity ions; obtaining a pure chloroplatinic acid solution, adding superior pure hydrazine hydrate into the solution, wherein the molar ratio of hydrazine hydrate to chloroplatinic acid is 3, fully reducing to obtain platinum powder, boiling and washing the platinum powder with a mixed dilute solution of nitric acid and hydrofluoric acid for 60min, fully washing with deionized water, and drying in vacuum to obtain high-purity platinum powder, wherein the purity of the platinum powder is more than 99.999%.
Example 2, referring to fig. 1, ammonium chloride was added to a chloroplatinic acid solution to generate an ammonium chloroplatinate precipitate, which was filtered and washed; preparing ammonium chloroplatinate precipitate into a suspension by using deionized water, slowly adding sulfurous acid, wherein the molar ratio of sulfurous acid to ammonium chloroplatinate is 1.2, controlling the solution potential to be 0.65 +/-0.2V in the whole process, reducing the ammonium chloroplatinate into soluble ammonium chloroplatinate, filtering insoluble substances, and passing the ammonium chloroplatinate solution through a three-stage 001 multiplied by 7 ion exchange resin column to remove impurity ions; obtaining a pure chloroplatinic acid solution, adding superior pure hydrazine hydrate into the solution, wherein the molar ratio of hydrazine hydrate to chloroplatinic acid is 4, fully reducing to obtain platinum powder, boiling and washing the platinum powder with a mixed dilute solution of nitric acid and hydrofluoric acid for 40min, fully washing with deionized water, and drying in vacuum to obtain high-purity platinum powder, wherein the purity of the platinum powder is more than 99.999%.
Example 3 referring to figure 1, ammonium chloride was added to the chloroplatinic acid solution to produce an ammonium chloroplatinate precipitate, which was filtered and washed with saturated ammonium chloride solution; preparing ammonium chloroplatinate precipitate into a suspension by using deionized water, slowly adding oxalic acid, wherein the molar ratio of the oxalic acid to the ammonium chloroplatinate is 1.2, controlling the solution potential to be 0.70 +/-0.2V in the whole process, reducing the ammonium chloroplatinate into soluble ammonium chloroplatinate, filtering insoluble substances, and passing the ammonium chloroplatinate solution through a three-stage 001 multiplied by 7 ion exchange resin column to remove impurity ions; obtaining a pure chloroplatinic acid solution, adding superior pure hydrazine hydrate into the solution, wherein the molar ratio of hydrazine hydrate to chloroplatinic acid is 5, fully reducing to obtain platinum powder, boiling and washing the platinum powder with a mixed dilute solution of nitric acid and hydrofluoric acid for 40min, fully washing with deionized water, and drying in vacuum to obtain high-purity platinum powder, wherein the purity of the platinum powder is more than 99.999%.
The impurity element analysis of a typical platinum powder prepared according to the present invention using GDMS was performed, and the results are shown in table 1 below.
TABLE 1 analysis of purity of high-purity platinum powder
Claims (2)
1. A preparation method of high-purity platinum powder for electronic components is characterized by comprising the following process steps:
(1) precipitating platinum by ammonium chloride;
(2) reducing and dissolving ammonium chloroplatinate;
(3) removing impurities by ion exchange;
(4) deep reduction of chloroplatinic acid;
(5) acid boiling to remove impurities;
the method comprises the following specific steps: adding ammonium chloride into the chloroplatinic acid solution to produce ammonium chloroplatinate precipitate, filtering and washing; precipitating ammonium chloroplatinate with deionized water to prepare a suspension, slowly adding a reducing agent, controlling the potential of the solution to reduce, and filtering insoluble substances to obtain an ammonium chloroplatinate solution; passing the ammonium platinochloride solution through a cation exchange column to further remove cation impurities to obtain a pure platinochloride solution; adding hydrazine hydrate into the chloroplatinic acid solution for deep reduction, so that the platinum is reduced into a powder form; boiling and washing the obtained platinum powder with nitric acid and hydrofluoric acid, fully washing with deionized water, and drying in vacuum to obtain high-purity platinum powder;
the reducing agent is sulfurous acid or oxalic acid, the molar ratio of the reducing agent/platinum is 1.1-1.3, the solution potential is controlled to be 0.65-0.70V by the adding amount of the reducing agent,
all the reagents are guaranteed reagent.
2. A preparation method of high-purity platinum powder for electronic components is characterized by comprising the following process steps:
adding ammonium chloride into the chloroplatinic acid solution to generate ammonium chloroplatinate precipitate, and filtering and washing; preparing the generated ammonium chloroplatinate precipitate into a suspension by using deionized water, slowly adding sulfurous acid, wherein the molar ratio of the sulfurous acid to the ammonium chloroplatinate is 1.2, controlling the solution potential to be 0.68 +/-0.2V in the whole process, reducing the ammonium chloroplatinate into soluble ammonium chloroplatinate, filtering to remove insoluble substances, and passing the ammonium chloroplatinate solution through a three-stage 001 multiplied by 7 ion exchange resin column to remove impurity ions; obtaining a pure chloroplatinic acid solution, adding superior pure hydrazine hydrate into the solution, wherein the molar ratio of hydrazine hydrate to chloroplatinic acid is 3, fully reducing to obtain platinum powder, boiling and washing the platinum powder with a mixed dilute solution of nitric acid and hydrofluoric acid for 60min, fully washing with deionized water, and drying in vacuum to obtain high-purity platinum powder, wherein the purity of the platinum powder is more than 99.999%.
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| CN108555313B (en) * | 2018-05-21 | 2020-01-10 | 金川集团股份有限公司 | Preparation method of medical high-purity platinum powder |
| 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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| CN110340377B (en) * | 2018-11-05 | 2022-11-29 | 贵研铂业股份有限公司 | Method for preparing high-purity platinum powder by full-wet method |
| CN111321308A (en) * | 2020-03-09 | 2020-06-23 | 贵研铂业股份有限公司 | Method for preparing high-purity platinum based on microbial adsorption |
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| CN113477938A (en) * | 2021-07-12 | 2021-10-08 | 安徽拓思贵金属有限公司 | Preparation method of high-purity platinum powder |
| CN114226749B (en) * | 2021-12-28 | 2022-10-25 | 中国石油大学(北京) | Method for preparing platinum powder |
| CN114951688A (en) * | 2022-04-25 | 2022-08-30 | 金川集团股份有限公司 | Preparation method of high-purity platinum powder |
| CN115198101A (en) * | 2022-06-23 | 2022-10-18 | 浙江微通催化新材料有限公司 | Platinum refining method |
| CN115090895B (en) * | 2022-06-30 | 2024-03-26 | 国药集团化学试剂有限公司 | Preparation method of high-purity platinum powder |
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Address after: No. 988, Keji Road, high tech Development Zone, Kunming, Yunnan 650000 (Kunming Precious Metals Research Institute) Patentee after: Yunnan Precious Metal New Materials Holding Group Co.,Ltd. Country or region after: China Address before: No. 988, Keji Road, high tech Development Zone, Kunming, Yunnan 650000 (Kunming Precious Metals Research Institute) Patentee before: Sino-Platinum Metals Co.,Ltd. Country or region before: China |