CN114951688A - Preparation method of high-purity platinum powder - Google Patents
Preparation method of high-purity platinum powder Download PDFInfo
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- CN114951688A CN114951688A CN202210437638.6A CN202210437638A CN114951688A CN 114951688 A CN114951688 A CN 114951688A CN 202210437638 A CN202210437638 A CN 202210437638A CN 114951688 A CN114951688 A CN 114951688A
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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
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
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Abstract
The invention relates to a preparation method of high-purity platinum powder, which comprises the following steps: firstly, dissolving and making a platinum raw material: dissolving the crude platinum powder in aqua regia to obtain a platinum solution A; concentrating and expelling nitre: concentrating the platinum solution A, removing nitrate with concentrated hydrochloric acid, adding dilute hydrochloric acid for dissolving, and filtering to obtain a platinum solution B; performing cation exchange impurity removal: removing impurities from the platinum solution B by adopting a resin column to obtain a platinum solution C with the concentration of 500 g/L; ammonium chloride platinum precipitation: adding an ammonium chloride solution into the platinum solution C for precipitation, standing for 12-24 hours after complete precipitation, and performing suction filtration and washing to obtain platinum precipitate; carrying out thermolysis: carrying out staged heating and calcining on the platinum precipitate to obtain a platinum sample; sixthly, repeating the steps of the first step and the fifth step to obtain high-purity platinum powder with the purity of 99.999%. The method has the advantages of short flow, simple operation, stable production process and obvious removal effect on platinum group metal impurities such as palladium, rhodium, ruthenium, iridium and the like, and the prepared high-purity platinum powder can meet the high-purity platinum requirement of electronic components.
Description
Technical Field
The invention relates to the technical field of platinum group metal purification in precious metal smelting, in particular to a preparation method of high-purity platinum powder.
Background
Platinum is an important element in platinum group metals, has good chemical stability, high electrical conductivity and thermal conductivity, and unique electrical, magnetic and optical properties, and is one of the key basic raw materials in the electronic industry fields of semiconductor devices, magnetic recording materials, integrated circuits and the like. In the field of electronic industry, with the development of electronic materials, the related process technology is continuously improved and upgraded, and the purity requirement of platinum raw materials is higher and higher, for example, the purity of platinum raw materials for integrated circuits, evaporation film materials and the like is required to be more than or equal to 99.999% (representing '5N'), and the demand is larger and larger. In the case of platinum-based sputtering targets, strict control is required for alkali metal elements (Na, K, etc.), transition metal elements (Fe, Ni, Co, Cu, etc.), radioactive metal elements (U, Th, etc.), and nonmetal elements (C, O, N, H, etc.).
At present, researchers mostly adopt a method of raw material dissolution, oxidation hydrolysis impurity removal, ammonium chloride platinum precipitation and reducing by a reducing agent to prepare high-purity platinum powder. The method has the problems of more chemical additives, impurity pollution, low direct recovery rate of platinum, complex operation, poor stability, large waste gas amount and the like.
Disclosure of Invention
The invention aims to solve the technical problem of providing a simple preparation method of high-purity platinum powder with high yield.
In order to solve the problems, the preparation method of the high-purity platinum powder comprises the following steps:
firstly, dissolving and making a platinum raw material: dissolving the crude platinum powder in aqua regia to obtain a platinum solution A; the dosage ratio of the crude platinum powder to the aqua regia is 25-100 g: 120-700 mL;
concentrating and expelling nitre: concentrating the platinum solution A, removing nitrate with concentrated hydrochloric acid, adding dilute hydrochloric acid for dissolving, and filtering to obtain a platinum solution B;
performing cation exchange impurity removal: removing impurities from the platinum solution B by adopting a resin column to obtain a platinum solution C with the concentration of 500 g/L;
ammonium chloride platinum precipitation: adding an ammonium chloride solution with the mass concentration of 30-50% into the platinum solution C for precipitation, standing for 12-24 hours after complete precipitation, and performing suction filtration and washing to obtain a platinum precipitate; the molar ratio of the using amount of the ammonium chloride solution to the using amount of the crude platinum powder is 1: 2-3;
carrying out thermal decomposition: carrying out staged heating and calcining on the platinum precipitate to obtain a platinum sample;
sixthly, repeating the steps of the first step and the fifth step to obtain high-purity platinum powder with the purity of 99.999%.
The method comprises the steps of dissolving at the temperature of 150-200 ℃ for 4-6 h.
The method comprises the step of preparing the concentrated hydrochloric acid with the volume concentration of 40-80%.
The method comprises the step of enabling the volume concentration of the dilute hydrochloric acid to be 5-15%.
And c, removing impurities from the resin column in the step three, wherein the condition is that the pH value in the resin column is 2-4 and the flow rate is 2-6 mL/min.
The washing in step four is to wash with deionized water for 3-5 times.
And heating at the stage of the calcination temperature of 150-600 ℃ in the step fifthly, wherein the calcination time is 19 hours.
Compared with the prior art, the invention has the following advantages:
1. the preparation process of the invention does not add any additive, thereby reducing impurity pollution and generating no toxic and harmful gas in the reaction process.
2. The method has the advantages of short flow, simple operation and stable production process, and has obvious effect of removing platinum group metal impurities such as palladium, rhodium, ruthenium, iridium and the like.
3. After the method is adopted, the direct yield of the metal platinum reaches more than 97 percent, and the purity of the prepared high-purity platinum powder reaches 99.999 percent, so that the high-purity platinum powder can meet the requirement of high-purity platinum of electronic components.
Detailed Description
A preparation method of high-purity platinum powder comprises the following steps:
firstly, dissolving and making a platinum raw material: dissolving 25-100 g of crude platinum powder in 120-700 mL of aqua regia at 150-200 ℃ for 4-6 h to obtain a platinum solution A.
Concentrating and expelling nitre: heating the platinum solution A to 150-200 ℃ for concentration, then carrying out nitrate removal by using concentrated hydrochloric acid with the volume concentration of 40-80%, and then adding dilute hydrochloric acid with the volume concentration of 5-15% for dissolution and filtration after the nitrate removal is finished, so as to obtain a platinum solution B.
Performing cation exchange impurity removal: and (3) filling a resin column with the volume of 80mL with a glass tube with the volume of 100mL and resin, adjusting the pH value in the resin column to be 2-4, and enabling the platinum solution B to flow through the resin column at the speed of 2-6 mL/min for cation impurity removal to obtain a platinum solution C with the concentration of 500 g/L.
Ammonium chloride platinum precipitation: and adding 30-50% of ammonium chloride solution into the platinum solution C for precipitation, wherein the molar ratio of the ammonium chloride solution to the crude platinum powder is 1: 2-3. And after the platinum precipitate is completely precipitated, standing for 12-24 hours, and then performing suction filtration and deionized water washing for 3-5 times to obtain the platinum precipitate.
Carrying out thermal decomposition: and (3) calcining the platinum precipitate at the stage of 150-600 ℃ for 19 hours to obtain a platinum sample.
Sixthly, repeating the steps of the first step and the fifth step to obtain high-purity platinum powder with the purity of 99.999%.
Embodiment 1 a method for preparing high-purity platinum powder, comprising the steps of:
firstly, dissolving and making a platinum raw material: dissolving 25g of spongy platinum in 120mL of aqua regia at 150-200 ℃ for 4-6 h to obtain a platinum solution A.
Concentrating and expelling nitre: heating the platinum solution A to 150-200 ℃ for concentration, then using 50mL of concentrated hydrochloric acid with volume concentration of 40% to drive nitrate, adding 150mL of dilute hydrochloric acid with volume concentration of 10% after nitrate driving is finished, dissolving and filtering to obtain a platinum solution B.
Performing cation exchange and impurity removal: adjusting the pH value in the resin column to be 2-4, and enabling the platinum solution B to flow through the resin column at the speed of 2mL/min, further removing cationic impurities, and obtaining a platinum solution C with the concentration of 500 g/L.
Ammonium chloride platinum precipitation: to the platinum solution C, 100mL of a 40% ammonium chloride solution was added for precipitation. And standing for 12 hours after the precipitation is complete, and then performing suction filtration and deionized water washing for 3 times to obtain platinum precipitate.
Carrying out thermal decomposition: and (3) calcining the platinum precipitate at the stage of 150-600 ℃ for 19 hours to obtain a 24.25g platinum sample.
Sixthly, repeating the steps of the first step and the fifth step to obtain high-purity platinum powder with the purity of 99.999%.
Embodiment 2 a method for preparing high-purity platinum powder, comprising the steps of:
firstly, dissolving and making a platinum raw material: dissolving 25g of spongy platinum in 120mL of aqua regia at 150-200 ℃ for 4-6 h to obtain a platinum solution A.
Concentrating and expelling nitre: heating the platinum solution A to 150-200 ℃ for concentration, then carrying out nitrate removal by using 60mL of concentrated hydrochloric acid with the volume concentration of 40%, and after the nitrate removal is finished, adding 160mL of diluted hydrochloric acid with the volume concentration of 10% for dissolution and filtering to obtain a platinum solution B.
Performing cation exchange impurity removal: adjusting the pH value in the resin column to be 2-4, and enabling the platinum solution B to flow through the resin column at the speed of 2mL/min to further remove cationic impurities to obtain a platinum solution C with the concentration of 500 g/L.
Ammonium chloride platinum precipitation: to the platinum solution C, 100mL of a 50% ammonium chloride solution was added for precipitation. And standing for 12 hours after the precipitation is complete, and then performing suction filtration and deionized water washing for 3 times to obtain platinum precipitate.
Carrying out thermal decomposition: and (3) heating the platinum precipitate at the stage of 150-600 ℃ for calcining for 19 hours to obtain a 24.30g platinum sample.
Sixthly, repeating the steps of the first step and the fifth step to obtain high-purity platinum powder with the purity of 99.999%.
Embodiment 3 a method for preparing high-purity platinum powder, comprising the steps of:
firstly, dissolving and making a platinum raw material: dissolving 25g of spongy platinum in 120mL of aqua regia at 150-200 ℃ for 4-6 h to obtain a platinum solution A.
Concentrating and expelling nitre: heating the platinum solution A to 150-200 ℃ for concentration, then using 70mL of concentrated hydrochloric acid with the volume concentration of 50% to remove the nitrate, adding 170mL of dilute hydrochloric acid with the volume concentration of 10% after the nitrate removal is finished, dissolving and filtering to obtain a platinum solution B.
Performing cation exchange impurity removal: adjusting the pH value in the resin column to be 2-4, and enabling the platinum solution B to flow through the resin column at the speed of 2mL/min, further removing cationic impurities, and obtaining a platinum solution C with the concentration of 500 g/L.
Ammonium chloride platinum precipitation: 100mL of a 60% ammonium chloride solution was added to the platinum solution C for precipitation. And standing for 12 hours after the precipitation is complete, and then performing suction filtration and deionized water washing for 3 times to obtain platinum precipitate.
Carrying out thermal decomposition: and (3) calcining the platinum precipitate at the stage of 150-600 ℃ for 19 hours to obtain a 24.28g platinum sample.
Sixthly, repeating the steps of the first step and the fifth step to obtain high-purity platinum powder with the purity of 99.999%.
The results of the purity analysis (GDMS) of the platinum powders prepared in examples 1 to 3 are shown in Table 1.
TABLE 1 content of impurity elements (ppm)
As can be seen from table 1: the contents of platinum group metal elements, alkali metal elements and the like in the high-purity platinum powder prepared by the method are less than 0.5ppm, which shows that the method disclosed by the invention has good impurity removal effect on the coarse platinum powder.
Claims (7)
1. A preparation method of high-purity platinum powder comprises the following steps:
firstly, dissolving and making a platinum raw material: dissolving the crude platinum powder in aqua regia to obtain a platinum solution A; the dosage ratio of the crude platinum powder to the aqua regia is 25-100 g: 120-700 mL;
concentrating and expelling nitre: concentrating the platinum solution A, removing nitrate with concentrated hydrochloric acid, adding dilute hydrochloric acid for dissolving, and filtering to obtain a platinum solution B;
performing cation exchange impurity removal: removing impurities from the platinum solution B by adopting a resin column to obtain a platinum solution C with the concentration of 500 g/L;
ammonium chloride platinum precipitation: adding an ammonium chloride solution with the mass concentration of 30-50% into the platinum solution C for precipitation, standing for 12-24 hours after complete precipitation, and performing suction filtration and washing to obtain a platinum precipitate; the molar ratio of the using amount of the ammonium chloride solution to the using amount of the crude platinum powder is 1: 2-3;
carrying out thermal decomposition: carrying out staged heating and calcining on the platinum precipitate to obtain a platinum sample;
sixthly, repeating the steps of the first step and the fifth step to obtain high-purity platinum powder with the purity of 99.999%.
2. The method for preparing high-purity platinum powder according to claim 1, wherein the method comprises the following steps: the method comprises the steps of dissolving at the temperature of 150-200 ℃ for 4-6 h.
3. The method for preparing high-purity platinum powder according to claim 1, wherein the method comprises the following steps: the method comprises the step of preparing the concentrated hydrochloric acid with the volume concentration of 40-80%.
4. The method for preparing high-purity platinum powder according to claim 1, wherein the method comprises the following steps: the method comprises the step of enabling the volume concentration of the dilute hydrochloric acid to be 5-15%.
5. The method for preparing high-purity platinum powder according to claim 1, wherein the method comprises the following steps: and c, removing impurities from the resin column in the step three, wherein the condition that the pH value in the resin column is 2-4 and the flow speed is 2-6 mL/min.
6. The method for preparing high-purity platinum powder according to claim 1, wherein the method comprises the following steps: the fourth washing is 3-5 times by using deionized water.
7. The method for preparing high-purity platinum powder according to claim 1, wherein the method comprises the following steps: and heating at the stage of the calcination temperature of 150-600 ℃ in the step fifthly, wherein the calcination time is 19 hours.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102296183A (en) * | 2011-08-19 | 2011-12-28 | 天津市化学试剂研究所 | Method for preparing high-purity platinum |
| CN103555937A (en) * | 2013-11-07 | 2014-02-05 | 铜陵有色金属集团股份有限公司 | Platinum refining process based on two-stage sedimentation method |
| KR101392179B1 (en) * | 2013-02-08 | 2014-05-08 | 강희남 | Recovery method of platinum group metal and apparatus for recovering platinum group metal |
| CN104028773A (en) * | 2013-03-05 | 2014-09-10 | 贺利氏贵金属有限责任两合公司 | Method for producing highly pure platinum powder, as well as platinum powder that can be obtained according to said method, and use thereof |
| 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 |
| CN105177305A (en) * | 2014-11-01 | 2015-12-23 | 陕西华特新材料股份有限公司 | Platinum wet purification method |
| CN107838434A (en) * | 2017-10-30 | 2018-03-27 | 贵研铂业股份有限公司 | A kind of preparation method of high-purity platinum powder |
| 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 |
| CN111926195A (en) * | 2020-06-24 | 2020-11-13 | 重庆材料研究院有限公司 | Method for preparing high-purity platinum from platinum alloy waste |
-
2022
- 2022-04-25 CN CN202210437638.6A patent/CN114951688A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102296183A (en) * | 2011-08-19 | 2011-12-28 | 天津市化学试剂研究所 | Method for preparing high-purity platinum |
| KR101392179B1 (en) * | 2013-02-08 | 2014-05-08 | 강희남 | Recovery method of platinum group metal and apparatus for recovering platinum group metal |
| CN104028773A (en) * | 2013-03-05 | 2014-09-10 | 贺利氏贵金属有限责任两合公司 | Method for producing highly pure platinum powder, as well as platinum powder that can be obtained according to said method, and use thereof |
| CN103555937A (en) * | 2013-11-07 | 2014-02-05 | 铜陵有色金属集团股份有限公司 | Platinum refining process based on two-stage sedimentation method |
| CN105177305A (en) * | 2014-11-01 | 2015-12-23 | 陕西华特新材料股份有限公司 | Platinum wet purification method |
| 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 |
| CN107838434A (en) * | 2017-10-30 | 2018-03-27 | 贵研铂业股份有限公司 | A kind of preparation method of high-purity platinum powder |
| 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 |
| CN111926195A (en) * | 2020-06-24 | 2020-11-13 | 重庆材料研究院有限公司 | Method for preparing high-purity platinum from platinum alloy waste |
Non-Patent Citations (1)
| Title |
|---|
| 郭学益等: "高纯金属材料", 冶金工业出版社, pages: 193 - 194 * |
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