CN1037618C - Method for making pure iridium - Google Patents
Method for making pure iridium Download PDFInfo
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- CN1037618C CN1037618C CN95104410A CN95104410A CN1037618C CN 1037618 C CN1037618 C CN 1037618C CN 95104410 A CN95104410 A CN 95104410A CN 95104410 A CN95104410 A CN 95104410A CN 1037618 C CN1037618 C CN 1037618C
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Abstract
The present invention relates to a method for preparing pure iridium, which is characterized in that hydrochloric acid-hydrogen peroxide oxidizes an ammonium chloroiridite (III) solution, so ammonium hexachloroiridate is precipitated, the precipitate is filtered out and is dried, and then the ammonium hexachloroiridate is put in a crucible of a calcinator in a shaft furnace; the ammonium hexachloroiridate is heated to 350 DEG C in 5 to 6 hours, the temperature is gradually risen to 700 DEG C and is kept, and then the ammonium hexachloroiridate is decomposed at high temperature until white smoke in the furnace disappears and does not escape. The power is cut off, the substance is cooled with the furnace, nitrogen gas is immediately led into the calcinator until the temperature is lower than 100 DEG C to room temperature, and then 99.99% pure iridium products are obtained. The present invention is used for refining iridium and has the advantages of simple method, high safety, good labor condition and high production efficiency.
Description
The present invention relates to the refinement of precious metal, particularly the preparation method of pure iridium.
Because iridium more is difficult to generate sulfide precipitation than other metal, therefore in the iridium refining process, sulfuration method purifying iridium still is widely adopted so far.Refining when being purified to required purity when the inferior iridium acid ammonium of chlorine ((NH4) 3IrCl6) through vulcanizing, adopt nitric acid oxidation method to be settled out ammonium iridichloride usually, prepare pure iridium powder through calcining, hydrogen reduction again." precious metal ", 1981,2 (1), P.18-21 narrated with the refining iridium of ammonium sulfide method, obtain the inferior iridium acid ammonium solution of chlorine, be ammonium iridichloride ((NH4) 2IrCl6) precipitation with nitric acid oxidation then, again through calcining, hydrogen reduction prepares the pure iridium powder of purity 99.98%. " precious metal ", 1991,12 (3), P.32-35 adopt ammonium chloride refining, the method of sodium borohydride reduction is produced pure iridium, and promptly ammonium iridichloride solution is removed expensive with (NH4) 2S sulfuration, base metal impurity, solution adds HNO3 and solid ammonium chloride, obtain pure ammonium iridichloride, obtain the pure iridium of purity more than 99.9% with sodium borohydride reduction again.Aforesaid method process labor condition is abominable, and environmental pollution is serious, and dangerous.
The objective of the invention is to overcome the above-mentioned shortcoming that prior art exists, propose a kind of new method of producing pure iridium.Use the inventive method, can be safely, produce in large quantity, free from environmental pollution, the product purity height, with short production cycle, power consumption is low, the labour productivity height.
Technical scheme of the present invention is: replace the inferior iridium acid of nitric acid oxidation chlorine ammonium with hydrochloric acid-hydrogen peroxide, be settled out ammonium iridichloride.
Method of the present invention is to be raw material with the inferior iridium acid of the chlorine after purifying ammonium, it is characterized in that: in the inferior iridium acid ammonium solution of the chlorine of iridium concentration 30-50 grams per liter, add the chemical pure concentrated hydrochloric acid of 5-6 (volume) % and the analytical pure hydrogen peroxide of concentration 50 (volume) % (by every gram iridium 2ml H2O2) carries out oxidation, be settled out ammonium iridichloride, leach throw out, after the drying ammonium iridichloride is placed the crucible of calcinatory in the pit furnace, cover crucible cover, calcinatory cover and bell, carry out pyrolytic decomposition by following program then: room temperature-350 ℃/5-6 hour, 350-450 ℃/10 hours, 450-700 ℃/6 hours, disappear to stove words spoken by an actor from offstage cigarette, no longer overflow, the outage furnace cooling, and in calcinatory, feed nitrogen immediately, nitrogen flow is decided on the calcinatory volume, to be enough to guaranteeing that the nitrogen in the calcinatory is malleation to ambiance, make not oxidized being as the criterion of metal iridium after the decomposition,, promptly get pure iridium product to dying to room temperature below 100 ℃.
The nitrogen flow of promotion be the 3.5-4 liter/minute.
Compared with prior art, the present invention has following advantage:
1. owing to replace the inferior iridium acid of nitric acid oxidation chlorine ammonium, improved labor condition with hydrochloric acid-hydrogen peroxide.
2. owing to the ammonium iridichloride pyrolytic decomposition finishes after, feed nitrogen immediately, and until below 100 ℃, thereby avoid the reoxidation of high-temperature decomposition product metal iridium, and suction hydrogen when having avoided being cooled to low temperature, significantly reduced the hydrogen content of iridium product.
3. use the inventive method, (more than the 4kg) produces pure iridium in enormous quantities, raises labour productivity more than 10 times, shortens the production cycle more than one times, and economize on electricity is more than 50%.
4. calcination process is guaranteed production safety and quality product without hydrogen, and iridium purity can reach more than 99.99%.
Embodiment 1
Containing the iridium amount is that (the iridium concentration in the solution is 30 grams per liters) adds the chemical pure concentrated hydrochloric acid of 5 (volume) % and the analytical pure H2O2 of 8022.5ml concentration 50 (volume) % in the inferior iridium acid ammonium solution of the 4011.25 gram chlorine of having purified, carry out oxidation, be settled out ammonium iridichloride, leach throw out, after the drying ammonium iridichloride is placed the crucible of calcinatory in the pit furnace, cover crucible cover, calcinatory cover and bell, heated to 350 ℃ with 5 hours then, afterwards according to 350-450 ℃/10 hours, pyrolytic decomposition is carried out in the also insulation that heats up of 450-700 ℃/6 hours programmed heating, disappears to stove words spoken by an actor from offstage cigarette, no longer overflow, outage furnace cooling, and the flow that divides with 3.5ml/ immediately feeds nitrogen in calcinatory is died to room temperature to 100 ℃, obtain 99.99% pure iridium product 3293.3 grams, yield 82%.
Embodiment 2
Containing the iridium amount is that (iridium concentration is 50 grams per liters) adds the chemical pure concentrated hydrochloric acid of 6 (volume) % and the analytical pure H2O2 of 17000ml concentration 50 (volume) % in the inferior iridium acid ammonium solution of the 8500 gram chlorine of having purified, carry out oxidation, be settled out ammonium iridichloride, leach throw out, after the drying ammonium iridichloride is placed the crucible of calcinatory in the pit furnace, cover crucible cover, calcinatory cover and bell, heated to 350 ℃ with 6 hours then, afterwards according to 350-450 ℃/10 hours, pyrolytic decomposition is carried out in the also insulation that heats up of 450-700 ℃/6 hours programmed heating, disappears to stove words spoken by an actor from offstage cigarette, no longer overflow, outage furnace cooling, and the flow that divides with 4ml/ immediately feeds nitrogen in calcinatory is died to room temperature to 100 ℃, obtain 99.99% pure iridium product 7241.9 grams, yield 85%.
Embodiment 3-4
Handle two batches respectively according to the method for embodiment 1 and contain the inferior iridium acid of the chlorine ammonium that the iridium amount is 0.485 gram, handle two batches with prior art in addition and contain the inferior iridium acid of the chlorine ammonium that the iridium amount is 0.485 gram, promptly with using the inferior iridium acid of nitric acid oxidation chlorine ammonium, handle resulting ammonium iridichloride with method of the present invention then, the result compares with gained, and its result is as shown in table 1.
Table 1 specimen coding raw material contains iridium amount (g) oxygenant iridium product (g) yield % embodiment 3 0.485 HCl-H2O2 0.4749 97.91 embodiment 4 0.485 HCl-H2O2 0.4735 97.63 Comparative Examples 1 0.485 HNO3 0.4145 85.46 Comparative Examples 2 0.485 HNO3 0.4195 86.49
As seen from Table 1, the method with the inferior iridium acid of HCl-H2O2 chlorine monoxide of the present invention ammonium is higher more than 10% than using its yield of prior art nitric acid oxidation method.
Claims (2)
1. method for preparing pure iridium, use the inferior iridium acid of the chlorine of having purified ammonium to be raw material, it is characterized in that: in the inferior iridium acid ammonium solution of the chlorine of iridium concentration 30-50 grams per liter, add the chemical pure concentrated hydrochloric acid of 5-6 (volume) % and the analytical pure hydrogen peroxide of concentration 50 (volume) %, carry out oxidation by every gram iridium 2ml H2O2, be settled out ammonium iridichloride, leach throw out, after the drying ammonium iridichloride is placed the crucible of calcinatory in the pit furnace, cover crucible cover, calcinatory cover and bell, carry out pyrolytic decomposition by following program then: room temperature-350 ℃/5-6 hour, 350-450 ℃/10 hours, 450-700 ℃/6 hours, disappear to stove words spoken by an actor from offstage cigarette, no longer overflow, the outage furnace cooling, and in calcinatory, feed nitrogen immediately, nitrogen flow is decided on the calcinatory volume, to be enough to guaranteeing that the nitrogen in the calcinatory is malleation to ambiance, make not oxidized being as the criterion of metal iridium after the decomposition,, promptly get pure iridium product to dying to room temperature below 100 ℃.
2. according to the method for claim 1, it is characterized in that, nitrogen flow be the 3.5-4 liter/minute.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95104410A CN1037618C (en) | 1995-04-17 | 1995-04-17 | Method for making pure iridium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95104410A CN1037618C (en) | 1995-04-17 | 1995-04-17 | Method for making pure iridium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1116243A CN1116243A (en) | 1996-02-07 |
| CN1037618C true CN1037618C (en) | 1998-03-04 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN95104410A Expired - Fee Related CN1037618C (en) | 1995-04-17 | 1995-04-17 | Method for making pure iridium |
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| CN (1) | CN1037618C (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101985696A (en) * | 2010-12-01 | 2011-03-16 | 金川集团有限公司 | Method for extracting iridium from iridium containing materials |
| CN102797018B (en) * | 2012-08-30 | 2015-09-23 | 贵研资源（易门）有限公司 | A kind of method adopting controlling potential separating-purifying platinum |
| CN108217754B (en) * | 2017-12-25 | 2020-02-14 | 贵研铂业股份有限公司 | IrO with large specific surface2Preparation method of (1) |
| CN108913913B (en) * | 2018-06-28 | 2020-06-26 | 清远先导材料有限公司 | Method for recovering iridium from iridium-containing zirconium dioxide |
| CN108821354B (en) * | 2018-09-22 | 2020-10-16 | 泸西县扩铂贵金属有限公司 | Method for preparing iridium nitrate solution |
| CN110000370A (en) * | 2019-04-19 | 2019-07-12 | 贵研铂业股份有限公司 | A kind of Large ratio surface iridium is black and preparation method thereof |
| CN114105229B (en) * | 2021-11-29 | 2024-02-13 | 英特派铂业股份有限公司 | Preparation method of high-purity iridium trichloride |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3867137A (en) * | 1973-06-22 | 1975-02-18 | Atomic Energy Commission | Purification of iridium |
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1995
- 1995-04-17 CN CN95104410A patent/CN1037618C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3867137A (en) * | 1973-06-22 | 1975-02-18 | Atomic Energy Commission | Purification of iridium |
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| CN1116243A (en) | 1996-02-07 |
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