CN114807622A - Method for reducing osmium secondary absorption liquid - Google Patents
Method for reducing osmium secondary absorption liquid Download PDFInfo
- Publication number
- CN114807622A CN114807622A CN202210232910.7A CN202210232910A CN114807622A CN 114807622 A CN114807622 A CN 114807622A CN 202210232910 A CN202210232910 A CN 202210232910A CN 114807622 A CN114807622 A CN 114807622A
- Authority
- CN
- China
- Prior art keywords
- osmium
- absorption liquid
- secondary absorption
- ethanol solution
- reducing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 229910052762 osmium Inorganic materials 0.000 title claims abstract description 62
- 239000007788 liquid Substances 0.000 title claims abstract description 40
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 52
- 229910052751 metal Inorganic materials 0.000 claims abstract description 9
- 239000002184 metal Substances 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 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 abstract description 11
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 abstract description 11
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 239000003638 chemical reducing agent Substances 0.000 abstract description 4
- 238000001556 precipitation Methods 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 description 5
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 230000007123 defense Effects 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- -1 platinum group metals Chemical class 0.000 description 2
- KXTKFKPHDLXHPU-UHFFFAOYSA-N [Os].[Na] Chemical compound [Os].[Na] KXTKFKPHDLXHPU-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
Abstract
The invention discloses a method for reducing osmium secondary absorption liquid, which is characterized in that the pH value of the osmium secondary absorption liquid is adjusted to 5-7, and the concentration of the osmium secondary absorption liquid is controlled to be 25-30 g/L; and heating the osmium secondary absorption liquid to 55-65 ℃, adding an ethanol solution, reacting for 1-2h at the constant temperature of 55-65 ℃, filtering, and washing to obtain the metal osmium. The invention uses the ethanol solution to replace hydrazine hydrate to reduce the secondary absorption liquid of osmium, thereby reducing the cost. The method adjusts the pH value of the osmium secondary absorption liquid before adding the ethanol solution, and can effectively control the osmium precipitation rate of the osmium absorption liquid; the ethanol solution is used for replacing hydrazine hydrate, and the hydrazine hydrate is a strong reducing agent and has certain danger, so that the safety risk is reduced; according to the invention, the osmium absorption liquid is heated to 55-65 ℃ before being reduced by adding an ethanol solution, the reduction efficiency is effectively improved, the reduction rate of osmium is more than or equal to 99%, and the content of osmium in the liquid after reaction is less than or equal to 0.01 g/L.
Description
Technical Field
A method for reducing osmium secondary absorption liquid, in particular to a method for reducing osmium-containing absorption liquid, belonging to the field of noble metal metallurgy.
Background
Noble metals, particularly platinum group metals, have unique physical and chemical properties, become important materials for modern industry and national defense construction, and are widely applied to various fields of national defense, fine chemical industry, petrochemical industry, medicines, energy sources, waste gas purification, bioengineering, metallurgical industry and the like. The application of the noble metals in the fields is realized by taking the compounds or the complexes thereof as carriers, and the products have various varieties and wide application. At present, osmium refining uses osmium primary absorption liquid produced by distillation as a raw material, and the osmium primary absorption liquid is reduced and secondarily distilled to produce an osmium powder product after refining, specifically, the osmium primary absorption liquid is reduced to osmium sodium salt by using the reducibility of sulfur dioxide, a cleaner osmium secondary absorption liquid is obtained by adopting the distillation refining principle, then hydrazine hydrate is used to reduce the osmium secondary absorption liquid to produce osmium black, and osmium is boiled, washed, calcined and reduced to produce an osmium powder product. However, hydrazine hydrate is a strong reducing agent, so that certain potential safety hazard exists; hydrazine hydrate is expensive, which causes over high cost; the hydrazine hydrate reacts violently in the reduction process, and the reaction process is difficult to control; the addition amount of hydrazine hydrate is difficult to control, and the endpoint of complete reduction is difficult to grasp.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for reducing osmium secondary absorption liquid, which uses a weak reducing agent ethanol solution to reduce osmium absorption liquid, achieves the purposes of convenience, rapidness, simple process, time saving and low cost by controlling temperature and reaction pH, and can master the reaction endpoint.
The method for reducing the osmium secondary absorption liquid comprises the following steps:
(1) adjusting the pH value of the osmium secondary absorption liquid to 5-7, and controlling the concentration of the osmium secondary absorption liquid to 25-30 g/L;
(2) and heating the osmium secondary absorption liquid to 55-65 ℃, adding an ethanol solution with the volume fraction of 75%, reacting at the constant temperature of 55-65 ℃ for 1-2h, filtering, and washing to obtain the metal osmium. Wherein the molar ratio of the ethanol to the osmium in the osmium secondary absorption liquid is 30-50: 1.
The invention has the beneficial effects that:
1. the invention uses the ethanol solution to replace hydrazine hydrate to reduce the secondary absorption liquid of osmium, thereby reducing the cost.
2. The method adjusts the pH value of the osmium secondary absorption liquid before adding the ethanol solution, and can effectively control the osmium precipitation rate of the osmium absorption liquid.
3. The invention replaces hydrazine hydrate with ethanol solution, and reduces safety risk because hydrazine hydrate is a strong reducing agent and has certain danger.
4. According to the invention, the osmium absorption liquid is heated to 55-65 ℃ before being reduced by adding an ethanol solution, the reduction efficiency is effectively improved, the reduction rate of osmium is more than or equal to 99%, and the content of osmium in the liquid after reaction is less than or equal to 0.01 g/L.
Detailed Description
Example 1
Taking 3L of secondary osmium absorption liquid containing 25g/L of osmium, and adding 75% ethanol solution by volume fraction, wherein the ethanol is 12.5 mol. And then heating the solution to 55 ℃, keeping the temperature for 1h, standing for 30min, cooling, filtering and washing to obtain the metal osmium.
Example 2
Taking 2L of secondary osmium absorption liquid containing about 30g/L of osmium, and adding 75% ethanol solution by volume fraction, wherein 15mol of ethanol is added. And then heating the solution to 55 ℃, keeping the temperature for 1h, standing for 30min, cooling, filtering and washing to obtain the metal osmium.
Example 3
Taking 2L of osmium secondary absorption liquid containing 30g/L of osmium, and adding 75% ethanol solution by volume fraction, wherein 30mol of ethanol is added. And then heating the solution to 55 ℃, keeping the temperature for 1h, standing for 30min, cooling, filtering and washing to obtain the metal osmium.
Example 4
Taking 2L of osmium secondary absorption liquid containing 25g/L of osmium, and adding 75% ethanol solution by volume fraction, wherein the ethanol is 12.5 mol. And then heating the solution to 65 ℃, keeping the temperature for 1h, standing for 30min, cooling, filtering and washing to obtain the metal osmium.
Example 5
Taking 2L of osmium secondary absorption liquid containing 30g/L of osmium, and adding 75% ethanol solution by volume fraction, wherein 15mol of ethanol is added. And then heating the solution to 65 ℃, keeping the temperature for 1h, standing for 30min, cooling, filtering and washing to obtain the metal osmium.
Claims (3)
1. A method for reducing osmium secondary absorption liquid comprises the following steps:
(1) adjusting the pH value of the osmium secondary absorption liquid to 5-7, and controlling the concentration of the osmium secondary absorption liquid to 25-30 g/L;
(2) and heating the osmium secondary absorption liquid to 55-65 ℃, adding an ethanol solution to react for 1-2h at the constant temperature of 55-65 ℃, filtering and washing to obtain the metal osmium.
2. The method of claim 1, wherein: in the ethanol solution, the volume fraction of ethanol is 75%.
3. The method of claim 1, wherein: the molar ratio of the ethanol to the osmium in the osmium secondary absorption liquid is 30-50: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210232910.7A CN114807622A (en) | 2022-03-10 | 2022-03-10 | Method for reducing osmium secondary absorption liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210232910.7A CN114807622A (en) | 2022-03-10 | 2022-03-10 | Method for reducing osmium secondary absorption liquid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114807622A true CN114807622A (en) | 2022-07-29 |
Family
ID=82528619
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210232910.7A Pending CN114807622A (en) | 2022-03-10 | 2022-03-10 | Method for reducing osmium secondary absorption liquid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114807622A (en) |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20010006612A1 (en) * | 2000-01-05 | 2001-07-05 | Matthias Grehl | Method for extracting osmium and ruthenium from noble metal |
| CN101985699A (en) * | 2010-12-01 | 2011-03-16 | 金川集团有限公司 | Method for extracting osmium from osmium-containing material |
| CN102676836A (en) * | 2011-03-18 | 2012-09-19 | 贺利氏贵金属有限及两合公司 | Method for recovery of precious metal from functionalised absorption materials containing precious metals |
| CN105420511A (en) * | 2015-11-18 | 2016-03-23 | 金川集团股份有限公司 | Method for reducing osmium absorption liquid |
| CN106148725A (en) * | 2016-08-29 | 2016-11-23 | 金川集团股份有限公司 | A kind of method separating refine osmium |
| CN106222438A (en) * | 2016-08-29 | 2016-12-14 | 金川集团股份有限公司 | A kind of from containing the method extracting osmium osmium material |
| CN110157921A (en) * | 2019-05-29 | 2019-08-23 | 金川集团股份有限公司 | A method of rapidly extracting osmium in material containing osmium |
| CN111411240A (en) * | 2020-04-23 | 2020-07-14 | 贺利氏贵金属技术(中国)有限公司 | Method for recovering noble metal from waste catalyst containing noble metal |
| CN111876597A (en) * | 2020-08-03 | 2020-11-03 | 国家地质实验测试中心 | Extraction of radioactive cause from molybdenite187Methods for Os |
| CN112226621A (en) * | 2020-10-15 | 2021-01-15 | 江苏欣诺科催化剂有限公司 | Method for recovering noble metal from deactivated noble metal catalyst |
-
2022
- 2022-03-10 CN CN202210232910.7A patent/CN114807622A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20010006612A1 (en) * | 2000-01-05 | 2001-07-05 | Matthias Grehl | Method for extracting osmium and ruthenium from noble metal |
| CN101985699A (en) * | 2010-12-01 | 2011-03-16 | 金川集团有限公司 | Method for extracting osmium from osmium-containing material |
| CN102676836A (en) * | 2011-03-18 | 2012-09-19 | 贺利氏贵金属有限及两合公司 | Method for recovery of precious metal from functionalised absorption materials containing precious metals |
| CN105420511A (en) * | 2015-11-18 | 2016-03-23 | 金川集团股份有限公司 | Method for reducing osmium absorption liquid |
| CN106148725A (en) * | 2016-08-29 | 2016-11-23 | 金川集团股份有限公司 | A kind of method separating refine osmium |
| CN106222438A (en) * | 2016-08-29 | 2016-12-14 | 金川集团股份有限公司 | A kind of from containing the method extracting osmium osmium material |
| CN110157921A (en) * | 2019-05-29 | 2019-08-23 | 金川集团股份有限公司 | A method of rapidly extracting osmium in material containing osmium |
| CN111411240A (en) * | 2020-04-23 | 2020-07-14 | 贺利氏贵金属技术(中国)有限公司 | Method for recovering noble metal from waste catalyst containing noble metal |
| CN111876597A (en) * | 2020-08-03 | 2020-11-03 | 国家地质实验测试中心 | Extraction of radioactive cause from molybdenite187Methods for Os |
| CN112226621A (en) * | 2020-10-15 | 2021-01-15 | 江苏欣诺科催化剂有限公司 | Method for recovering noble metal from deactivated noble metal catalyst |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right |
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) Applicant 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 Applicant before: JINCHUAN GROUP Co.,Ltd. Country or region before: China |