CN110157921A - A method of rapidly extracting osmium in material containing osmium - Google Patents
A method of rapidly extracting osmium in material containing osmium Download PDFInfo
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- CN110157921A CN110157921A CN201910459510.8A CN201910459510A CN110157921A CN 110157921 A CN110157921 A CN 110157921A CN 201910459510 A CN201910459510 A CN 201910459510A CN 110157921 A CN110157921 A CN 110157921A
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- 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
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Abstract
The invention discloses a kind of methods of rapidly extracting osmium in material containing osmium, belong to technical field of noble metal metallurgy, it will use ozone to carry out selective distillation after containing osmium material dissolving with hydrochloric acid, the osmium tetroxide distilled carries out two-stage absorption using the mixed liquor of sodium hydroxide and alcohol, adjust solution ph, it is black to obtain osmium by hydrazine hydrate reduction, after calcining, hydrogen reduction Metal osmium powder.The present invention is guaranteeing that osmium tetroxide is not reduced simultaneously, improves distillation efficiency, and the time for distilling osmium shortened within 8 hours, and the present invention has many advantages, such as simple process, and process flow is short, easy to operate, stable product quality.
Description
Technical field
The invention belongs to field of metallurgy, and in particular to a method of the rapidly extracting osmium from osmium mineral or material containing osmium.
Background technique
Osmium is the very special metallic element of a property, and the osmium of metallic state has fusing point height, hardness big, is not easy machinery
Processing, but its inoxidizability is excessively poor, and sponge osmium can be oxidized to volatility very strong four by the oxygen in air at room temperature
Somuum oxide.Therefore, always with the volatilization of osmium tetroxide in the purification process of osmium, process is longer, loses bigger.Traditional osmium
Extracting method include reduction precipitation method, vulcanized sodium precipitating-oxygen blast calcination method, second distillation method, hydrogen direct-reduction OsO4Or
Na2OsO6Method etc..Process flow is long, and the recovery rate of osmium is low.Patent CN106222438 is disclosed in one kind material containing osmium and is extracted osmium
Method, osmium material will be contained and distilled under hydrochloric acid medium, distillation absorbing liquid it is 2-6 grades total, the 1st grade use 1%-5% NaClO
+ 20%-30% potassium hydroxide solution, 2-6 grades are absorbed using 20%-30% potassium hydroxide solution.Although the invention is because be added
NaClO ensure that osmium tetroxide is not reduced, but the time of 2-6 grades of distillations is still up to 12 hours or more in the time.
Summary of the invention
The present invention is directed to the deficiency of the above method, provides a kind of simple process, and distillation time is few, and the rate of recovery is high from containing
The method of osmium is extracted in osmium material.
The present invention is achieved by the following technical solutions: a method of rapidly extracting osmium, feature in material containing osmium
It is: will use ozone to carry out selective distillation after osmium material dissolving with hydrochloric acid will be contained, the osmium tetroxide distilled uses hydrogen-oxygen
The mixed liquor for changing sodium and alcohol carries out two-stage absorption, adjusts solution ph, and it is black to obtain osmium by hydrazine hydrate reduction, also through calcining, hydrogen
Metal osmium powder is obtained after original, specifically includes the following steps:
Step (1) dissolution: material containing osmium is added in the hydrochloric acid medium of 1-1.5mol/L and is dissolved；
Step (2) is selectively distilled: step (1) acquired solution being transferred to cucurbit, is passed through ozone 120-180mg/L, is distilled；
Step (3) mixed liquor absorbs osmium: mixed liquor using mass concentration 20%-30% NaOH+5%C2H5OH is to distilling
Osmium tetroxide carries out two-stage absorption；
The preparation of step (4) osmium powder: merging two-stage absorbing liquid and adjust pH value 4-5, and it is black to obtain osmium using hydrazine hydrate reduction, through dry
Dry, hydrogen reduction obtains Metal osmium powder.
The present invention adds hydrogen peroxide to carry out selective distillation using ozone, it may be assumed that is passed through ozone 120-180mg/L, distills 5 hours
After be added hydrogen peroxide, hydrogen peroxide and distillate are that 1:5-6 is added by volume, continue distillation 2-2.5 hours.
Material containing osmium of the invention is osmium sodium salt, and when dissolution, the liquid-solid ratio of material containing osmium and hydrochloric acid is 4-6:1.
Two-stage absorption of the present invention is respectively as follows: first order mass concentration 20%NaOH+5%C2H5OH absorbs, the second level
With mass concentration 25-30%NaOH+5%C2H5OH absorbs.
The present invention uses hydrochloride adjusted solution pH=4-5.
Compared with the prior art, the advantages of the present invention are as follows:
The method that the present invention uses ozone selectively to distill is not reduced simultaneously in guarantee osmium tetroxide, improves distillation efficiency,
The time for compared with prior art distilling osmium shortened within 8 hours.Simple process of the invention, it is high-efficient.Metal returns
High income, product quality is steady, reduces the influence volatilized due to osmium tetroxide to environment.Add in particular by more ozone few
Hydrogen peroxide carries out selectivity distillation mode, shortens the time of osmium distillation, shortens entire process flow, and improve mentioning for osmium
Take rate.
Specific embodiment
The present invention is described in further detail combined with specific embodiments below；
Embodiment 1
1.5mol/L hydrochloric acid is added in osmium sodium salt, liquid-solid ratio 4.5:1 is dissolved, and solution, which is transferred in cucurbit, to be distilled, first
First, ozone 140mg/L is passed through in distillate, is distilled 5 hours, be then added hydrogen peroxide (distillate: dioxygen water volume ratio is 5:
1), continue distillation 2.5 hours；The osmium tetroxide distilled is absorbed using two-stage, first order mass concentration 20%NaOH+
Mass concentration 5%C2H5OH absorbs, second level mass concentration 25%NaOH+ mass concentration 5%C2H5OH absorbs, and closes after absorption
And multistage absorption liquid is handled, pH value 4-5 is adjusted with hydrochloric acid, it is black to obtain osmium using hydrazine hydrate reduction, obtains gold through drying, hydrogen reduction
Belong to osmium powder.Each link testing result is as follows:
The testing result of 1 embodiment of table, 1 product
Embodiment 2
1mol/L hydrochloric acid is added in osmium sodium salt, liquid-solid ratio 6:1 is dissolved, and solution, which is transferred in cucurbit, to be distilled, firstly,
It is passed through ozone 160mg/L in distillate, distills 5 hours, hydrogen peroxide (distillate: dioxygen water volume ratio is 6:1) is then added, after
Continuous distillation 2 hours；The osmium tetroxide distilled is absorbed using two-stage, first order mass concentration 20%NaOH+ mass concentration
5%C2H5OH absorbs, second level mass concentration 25%NaOH+ mass concentration 5%C2H5OH absorbs.Merging treatment is more after absorption
Grade absorbing liquid, adjusts pH value 4-5 with hydrochloric acid, and it is black to obtain osmium using hydrazine hydrate reduction, obtains Metal osmium powder through drying, hydrogen reduction.
Each link testing result is as follows:
The testing result of 2 embodiment of table, 2 product
。
Claims (4)
1. a kind of method of rapidly extracting osmium in material containing osmium, it is characterised in that: will contain after osmium material dissolving with hydrochloric acid using smelly
Oxygen carries out selective distillation, and the osmium tetroxide distilled carries out two-stage absorption using the mixed liquor of sodium hydroxide and alcohol, adjusts
It is black to obtain osmium by hydrazine hydrate reduction for whole solution ph, after calcining, hydrogen reduction Metal osmium powder.
2. the method for rapidly extracting osmium in a kind of material containing osmium according to claim 1, it is characterised in that: specifically include with
Lower step,
Step (1) dissolution: material containing osmium is added in the hydrochloric acid medium of 1-1.5mol/L and is dissolved；
Step (2) is selectively distilled: step (1) acquired solution being transferred to cucurbit, is passed through ozone 120-180mg/L, is distilled；
Step (3) mixed liquor absorbs osmium: using mass concentration 20%-30% NaOH+5%C2H5The mixed liquor of OH is to distilling
Osmium tetroxide carries out two-stage absorption；
The preparation of step (4) osmium powder: merging two-stage absorbing liquid and adjust pH value 4-5, and it is black to obtain osmium using hydrazine hydrate reduction, through dry
Dry, hydrogen reduction obtains Metal osmium powder.
3. the method for rapidly extracting osmium in a kind of material containing osmium according to claim 2, it is characterised in that: added using ozone
Hydrogen peroxide carries out selective distillation.
4. the method for rapidly extracting osmium in a kind of material containing osmium according to claim 3, it is characterised in that: be passed through ozone
Hydrogen peroxide is added in 120-180mg/L, distillation after 5 hours, hydrogen peroxide and distillate are that 1:5-6 is added by volume, continues to distill
2-2.5 hour.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910459510.8A CN110157921A (en) | 2019-05-29 | 2019-05-29 | A method of rapidly extracting osmium in material containing osmium |
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| CN201910459510.8A CN110157921A (en) | 2019-05-29 | 2019-05-29 | A method of rapidly extracting osmium in material containing osmium |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111663055A (en) * | 2020-08-03 | 2020-09-15 | 国家地质实验测试中心 | Extraction of rhenium and radioactive origin187Methods for Os |
| CN111876617A (en) * | 2020-08-03 | 2020-11-03 | 国家地质实验测试中心 | Extraction of molybdenum, rhenium and radioactive origin187Methods for Os |
| CN111983005A (en) * | 2020-07-29 | 2020-11-24 | 中国科学院地质与地球物理研究所 | Secondary oxidation distillation separation device and separation method for Os element and application of secondary oxidation distillation separation device |
| CN114433863A (en) * | 2022-02-11 | 2022-05-06 | 广东先导稀材股份有限公司 | Method for preparing osmium powder from osmium oxide material |
| CN114807622A (en) * | 2022-03-10 | 2022-07-29 | 金川集团股份有限公司 | Method for reducing osmium secondary absorption liquid |
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| CN1288964A (en) * | 1999-09-17 | 2001-03-28 | 贵研铂业股份有限公司 | Preparation of high-purity chloro-osmate solution |
| CN101985699A (en) * | 2010-12-01 | 2011-03-16 | 金川集团有限公司 | Method for extracting osmium from osmium-containing material |
| EP2762452A1 (en) * | 2011-05-31 | 2014-08-06 | National University Corporation Hamamatsu University School of Medicine | Recovery of reusable osmium tetroxide |
| CN104232919A (en) * | 2013-06-13 | 2014-12-24 | 无锡市森信精密机械厂 | Technology for extracting noble metals from rutheniridosmine |
| 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 |
| CN108660323A (en) * | 2018-06-20 | 2018-10-16 | 南京东锐铂业有限公司 | The new method of osmium powder purification |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1288964A (en) * | 1999-09-17 | 2001-03-28 | 贵研铂业股份有限公司 | Preparation of high-purity chloro-osmate solution |
| CN101985699A (en) * | 2010-12-01 | 2011-03-16 | 金川集团有限公司 | Method for extracting osmium from osmium-containing material |
| EP2762452A1 (en) * | 2011-05-31 | 2014-08-06 | National University Corporation Hamamatsu University School of Medicine | Recovery of reusable osmium tetroxide |
| CN104232919A (en) * | 2013-06-13 | 2014-12-24 | 无锡市森信精密机械厂 | Technology for extracting noble metals from rutheniridosmine |
| 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 |
| CN108660323A (en) * | 2018-06-20 | 2018-10-16 | 南京东锐铂业有限公司 | The new method of osmium powder purification |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111983005A (en) * | 2020-07-29 | 2020-11-24 | 中国科学院地质与地球物理研究所 | Secondary oxidation distillation separation device and separation method for Os element and application of secondary oxidation distillation separation device |
| CN111983005B (en) * | 2020-07-29 | 2022-01-28 | 中国科学院地质与地球物理研究所 | Secondary oxidation distillation separation device and separation method for Os element and application of secondary oxidation distillation separation device |
| CN111663055A (en) * | 2020-08-03 | 2020-09-15 | 国家地质实验测试中心 | Extraction of rhenium and radioactive origin187Methods for Os |
| CN111876617A (en) * | 2020-08-03 | 2020-11-03 | 国家地质实验测试中心 | Extraction of molybdenum, rhenium and radioactive origin187Methods for Os |
| CN111663055B (en) * | 2020-08-03 | 2022-02-22 | 国家地质实验测试中心 | Extraction of rhenium and radioactive origin187Methods for Os |
| CN111876617B (en) * | 2020-08-03 | 2022-02-22 | 国家地质实验测试中心 | Extraction of molybdenum, rhenium and radioactive origin187Methods for Os |
| CN114433863A (en) * | 2022-02-11 | 2022-05-06 | 广东先导稀材股份有限公司 | Method for preparing osmium powder from osmium oxide material |
| CN114807622A (en) * | 2022-03-10 | 2022-07-29 | 金川集团股份有限公司 | Method for reducing osmium secondary absorption liquid |
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Application publication date: 20190823 |