CN1288965A - Preparation of high-purity osmium powder - Google Patents
Preparation of high-purity osmium powder Download PDFInfo
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- CN1288965A CN1288965A CN 99115144 CN99115144A CN1288965A CN 1288965 A CN1288965 A CN 1288965A CN 99115144 CN99115144 CN 99115144 CN 99115144 A CN99115144 A CN 99115144A CN 1288965 A CN1288965 A CN 1288965A
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- osmium
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- osmium powder
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Abstract
The preparation method of high-purity osmium powder is characterized by using crude osmium powder or crude sodium osmate as raw material, distilling osmium to obtain OsO4, then directly introding OsO4 into reduction reactor, heating and introducing hydrogen gas to make reduction reaction so as to obtain the high-purity osmium powder whose purity is 99.99% and yield is greater than 99%.
Description
A kind of preparation of high-purity osmium powder.The present invention belongs to precious metals metallurgy.
Osmium is one of platinum family element, and osmium has stronger catalytic activity, or a kind of nutritive substance in the body reduction process.In recent years, high-purity osmium powder and compound thereof more and more are used to fields such as Aeronautics and Astronautics, microelectronics, biomedicine.Yet the easy oxidation of osmium generates stable oxide O
sO
4, 40.6～40.7 ℃ of this oxide fusing points, 134 ℃ of boiling points, as easy as rolling off a log volatilization, volatile matter has strong impulse and toxicity to human body, this just make purity be 99.99% and the preparation difficulty of above high-purity osmium powder bigger.(CSTAD, project year numbers: 92210294), adopt distillation osmium-alkali liquor absorption-hydrazine hydrate reduction to be settled out O " new technology of separating-purifying osmium from the osmium absorption liquid "
sO
4-calcining hydrogen reduction technology, prepare purity and be 99.9～99.95% osmium powder, still, do not reach purity and be 99.99% and the requirement of above high-purity osmium powder, mainly be the base metal content such as Cu, Fe, Ni between 0.002～0.005%, do not reach＜0.001% requirement.
The objective of the invention is to improve the preparation method of osmium powder, make it to produce purity and be 99.99% or above high-purity osmium powder.
A kind of preparation of high-purity osmium powder of inventing comprises with thick osmium powder or thick sodium osmic acid being that raw material distillation osmium is O
sO
4, the O that distills out
sO
4The direct hydrogen reduction of steam is 2 steps of osmium powder, its technical characterictic is: 1. be that 40%～99% thick osmium powder or thick sodium osmic acid are put into cucurbit with grade, adding concentration is the sulfuric acid solution of 3mol/L, about 100 ℃ of temperature, dripping concentration is the sodium chlorate solution of 10% weight ratio, makes osmium change O into
sO
4Distill out; 2.1 the O that step distills out
sO
4Steam imports directly that to lead to hydrogen reducing in the reduction reactor be the osmium powder, and reducing condition is: 150 ℃～800 ℃ of temperature, hydrogen dividing potential drop 0.2～0.5KPa, reducing gas flow 200～350ml/cm
2, reduction reactor is quartz tube reactor, the tube type resistance furnace external heating mode; Optimum reduction condition is: 500～550 ℃ of temperature, hydrogen dividing potential drop 0.4KPa, reducing gas flow 300ml/cm
2Through these two steps, can make the high-purity osmium powder of purity 99.99%, direct yield＞99%.
The advantage of invention: 1, the technical scheme flow process is short, and only needing can make purity from thick osmium powder or thick sodium osmic acid through 2 steps is 99.99% high-purity osmium powder.2, direct yield height can reach more than 99%.3, method is reliable, preparation high-purity osmium powder that can be stable.
Embodiment
Example 1, the 1st step: get the thick osmium powder 5g of purity 96%, contain osmium amount 4.8g, put into cucurbit, adding concentration is the sulfuric acid solution of 3mol/L, makes osmium change O into
sO
4Gas distills out; The 2nd step: the O that the 1st step distills out
sO
4Steam directly imports logical hydrogen reducing in the quartz tube reactor (tube type resistance furnace external heat), and reducing condition is: 450 ℃ of temperature, hydrogen dividing potential drop 0.3KPa, reducing gas flow 250ml/cm
2, the osmium powder 4.76g of acquisition purity 99.99% after the reduction, direct yield 99.1%.
Example 2, the 1st step: get the thick sodium osmic acid 100g of purity 98%, water content 40%, contain osmium amount 37.26g, the distillation osmium changes O into
sO
4The step condition is with 1: the 2 step O of example
sO
4It is that the condition of osmium powder is: 500 ℃ of temperature, hydrogen dividing potential drop 0.4KPa, reducing gas flow 300ml/cm that steam directly imports hydrogen reducing in the quartz tube reactor
2, the osmium powder 36.962g of acquisition purity 99.99%, direct yield 99.2%.
Example 3, get the thick osmium powder 200g of purity 92%, contain osmium 184g, the 1st step with example 2, obtains the osmium powder 182.528g of purity 99.99%, direct yield 99.2% with example 1, the 2 step.
The spectroscopic analysis result that 3 examples obtain the osmium powder is listed as showing:
| Numbering | ????1 | ????2 | ????3 |
| ????Fe | ?＜0.0006 | ?＜0.0006 | ?＜0.0006 |
| ????Ni | ?＜0.0003 | ?＜0.0003 | ?0.00045 |
| ????Cu | ?0.00004 | ?0.00005 | ?0.00001 |
| ????Mg | ?0.00006 | ?0.00006 | ?0.00006 |
| ????Al | ＜0.0003 | ?＜0.0003 | ＜0.0003 |
| ????Si | ?0.001 | ?0.001 | ?0.001 |
| ????Ag | ?0.000015 | ?0.000045 | ?0.000028 |
| ????Au | ＜0.0003 | ?＜0.0003 | ＜0.0003 |
| ????Pd | ＜0.0002 | ?＜0.0002 | ＜0.0002 |
| ????Ru | ?0.002 | ?0.0018 | ＜0.001 |
| ????Pt | ?＜0.001 | ?＜0.001 | ＜0.001 |
| ????Co | ?＜0.0012 | ?＜0.0012 | ＜0.0012 |
| ????Ir | ＜0.002 | ?＜0.002 | ＜0.002 |
| ????Rh | ＜0.0003 | ?＜0.0003 | ＜0.0003 |
| Purity % | ?＞99.9907 | ?＞99.9909 | ＞99.992 |
The effect of invention: can find out from the result of 3 embodiment, take thick osmium powder (or thick sodium osmic acid) as raw material, be O through the distillation osmium only
sO
4And O
sO
42 steps of the direct hydrogen reducing of steam, just obtained the high-purity osmium powder of purity 99.99%, direct yield＞99%, than " new technology of separating-purifying osmium from the osmium absorption liquid " (CSTAD, project year numbers 92210294), technology has reduced by 2 steps, and purity improves, and direct yield improves.This is to have reduced by 2 steps by what, has also just avoided simultaneously the influence of the trace impurity that brings in these two step agents useful for same and the operation, so the method steps of being invented is few, and the osmium powder purity height (reaching 99.99%) that obtains, direct yield height (＞99%).
Claims (2)
1, plants preparation of high-purity osmium powder, comprise with thick osmium powder or thick sodium osmic acid being that raw material distillation osmium is O
sO
4, the O of distillation
sO
4The direct hydrogen reduction of steam is 2 steps of osmium powder, it is characterized in that:
11 is that 90%～99% thick osmium powder or thick sodium osmic acid are put into cucurbit with grade, and adding concentration is the sulfuric acid solution of 3mol/L, about 100 ℃ of temperature, and dripping concentration is the sodium chlorate solution of 10% weight ratio, makes osmium change O into
sO
4Distill out;
The O that 121 steps distill out
sO
4Steam imports directly that to lead to hydrogen reducing in the reduction reactor be the osmium powder, and reducing condition is: 150 ℃～800 ℃ of temperature, hydrogen dividing potential drop 0.2～0.5KPa, reducing gas flow 200～350ml/cm
2, reduction reactor is quartz tube reactor, the tube type resistance furnace heating.
2, a kind of preparation of high-purity osmium powder as claimed in claim 1 is characterized in that the condition of step 2 hydrogen reducing is: 500～550 ℃ of temperature, hydrogen dividing potential drop 0.4KPa, reducing gas flow 300ml/cm
2
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99115144A CN1102176C (en) | 1999-09-17 | 1999-09-17 | Preparation of high-purity osmium powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99115144A CN1102176C (en) | 1999-09-17 | 1999-09-17 | Preparation of high-purity osmium powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1288965A true CN1288965A (en) | 2001-03-28 |
| CN1102176C CN1102176C (en) | 2003-02-26 |
Family
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN99115144A Expired - Fee Related CN1102176C (en) | 1999-09-17 | 1999-09-17 | Preparation of high-purity osmium powder |
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| CN (1) | CN1102176C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100433407C (en) * | 2006-04-06 | 2008-11-12 | 上海申建冶金机电技术有限公司 | Cell box explosion preventing method, cell box employing the same and high fusion heat absorption material therefor |
| CN101985699A (en) * | 2010-12-01 | 2011-03-16 | 金川集团有限公司 | Method for extracting osmium from osmium-containing material |
| CN105420511A (en) * | 2015-11-18 | 2016-03-23 | 金川集团股份有限公司 | Method for reducing osmium absorption liquid |
| 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 |
| 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 |
-
1999
- 1999-09-17 CN CN99115144A patent/CN1102176C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100433407C (en) * | 2006-04-06 | 2008-11-12 | 上海申建冶金机电技术有限公司 | Cell box explosion preventing method, cell box employing the same and high fusion heat absorption material therefor |
| CN101985699A (en) * | 2010-12-01 | 2011-03-16 | 金川集团有限公司 | Method for extracting osmium from osmium-containing material |
| CN105420511A (en) * | 2015-11-18 | 2016-03-23 | 金川集团股份有限公司 | Method for reducing osmium absorption liquid |
| CN105420511B (en) * | 2015-11-18 | 2018-05-15 | 金川集团股份有限公司 | A kind of method for reducing osmium absorbing liquid |
| 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 |
| CN106222438B (en) * | 2016-08-29 | 2018-01-12 | 金川集团股份有限公司 | A kind of method that osmium is extracted from material containing 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1102176C (en) | 2003-02-26 |
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Owner name: GUIYAN PLATIUM CO., LTD. Free format text: FORMER OWNER: KUNMING INSTITUTE OF PRECIOUS METALS Effective date: 20010620 |
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Effective date of registration: 20010620 Applicant after: Guiyan Platinum Industry Co., Ltd. Applicant before: Kunming Institute of Precious Metals |
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