CN1626690A - New method for hydrogen reduction separating rhodium in iridium solution - Google Patents
New method for hydrogen reduction separating rhodium in iridium solution Download PDFInfo
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- CN1626690A CN1626690A CNA2003101219836A CN200310121983A CN1626690A CN 1626690 A CN1626690 A CN 1626690A CN A2003101219836 A CNA2003101219836 A CN A2003101219836A CN 200310121983 A CN200310121983 A CN 200310121983A CN 1626690 A CN1626690 A CN 1626690A
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- rhodium
- iridium
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- hydrogen reduction
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Abstract
A hydrogen reducing process for separating Rh from Ir solution includes loading the Rh contanied Ir solution into reactor, heating to a certain temp udner ordinary pressure, introducing H2 to it, and hydrogen reducing reaction to reduce Rh into solid metal. Its advantages are high purity (99% for Rh and 99.99% for Ir), short time, and no pollution.
Description
Technical field
The extraction that the present invention relates to the platinum metals with separate, particularly relate to the method for the separation and the extraction of rhodium in the platinum metals, iridium.
Background technology
In the precious metals metallurgy process, because the chemical property of rhodium, iridium is similar, its existence in hydrochloric acid medium is very complicated again, therefore, all is a difficult problem of generally acknowledging during being separated in of rhodium, iridium analyzed and refining is purified, and also is the problem of studying for many years.In general, rhodium, iridium separation all are after being placed on other metallic matrix separation, to carry out again.
For rhodium, the existing commentary of the isolating research overview of iridium.In years of researches, the chemist proposed various separation methods in order to measure rhodium iridium, and the some of them method is adopted by the metallargist.When illustrating the principle of separation method theoretically, can be divided into four classes to rhodium, iridium separation method substantially: the first kind, utilize the difference of rhodium, two kinds of metallochemistry character of iridium to separate; Second class, utilize IrCl
6 3-Thermodynamic stability and all high RhCl of kinetic inertness
6 3-Characteristics separate; The 3rd class, utilize IrCl
6 2-Compare RhCl
6 3-Characteristics with lower density of surface charge are separated; The 4th class, with RhCl
6 3-Being converted into complex cation separates.Wherein, the ultimate principle of the 4th class also is attributable to second class.Above the whole bag of tricks principle all can reach the separation between rhodium, the iridium, but owing to rhodium, the complicacy of iridium existence and the characteristic of appraising at the current rate fast of iridium in the solution, all brings limitation for various separation methods.Separate micro-iridium for thorough from a large amount of rhodiums, and being separated from each other in the feed liquid that concentration is bigger in that both ratios are close, more effective novel method waits in expectation in the production always.
Hydrogen reduction is a kind of reduction precipitation method of not introducing any detrimental impurity.For this method, the technology and the kinetics of pressurized hydrogen reduction iridium was once at length studied by Kunming Institute of Precious Metals, find that temperature of reaction is the key factor of hydrogen reduction iridium, temperature is greater than 80 ℃, the iridium coordination ion just might propose the method with pressurized hydrogen reduction method purifying iridium by hydrogen reduction to metallic state." precious metal " 1994 15 volumes 1 phase 1-9 page or leaf has also been reported the kinetics of the rhodium in the normal pressure hydrogen reduction hydrochloric acid medium, has studied temperature under the normal pressure, stirring intensity, and the rhodium starting point concentration, concentration of hydrochloric acid, chlorine ion concentrations etc. are to the quick-acting influence of hydrogen reduction rhodium reaction.Though the document has been reported temperature under the research normal pressure, stirring intensity, the rhodium starting point concentration, concentration of hydrochloric acid, chlorine ion concentrations etc. are to the quick-acting influence of hydrogen reduction rhodium reaction, under the contrast, the production research and the content of the present invention and inequality of document report, what the document was reported research only is rhodium, and does not also report detailed production craft step, just some theoretic discussions are not mentioned to iridium in the hydrochloric acid medium in the document.And the research of this project is rhodium in the iridium solution.In the prior art, the method for pressurized hydrogen reduction method purifying iridium is only arranged, and do not have the method for normal pressure hydrogen reduction purifying iridium.
Summary of the invention
The present invention proposes to use the method for hydrogen reduction separate rhodium, iridium under normal pressure, can overcome the method mesohigh still danger of pressurized hydrogen reduction method purifying iridium, and complicated operation, high pressure can't solve the problem of hydrogen-type corrosion down.The present invention comprises following concrete processing step: (1) puts into reactor with rhodium, the iridium solution of finite concentration ratio; (2) being raised to certain temperature feeding hydrogen under normal pressure reduces.The mass ratio of described rhodium and iridium＜1: 10, the concentration of hydrochloric acid [H of described iridium solution
+]=1～0.002mol/l.Described reactor has the insulation interlayer, feeds 50～80 ℃ hot water in the reaction process in the insulation interlayer.The flow of described hydrogen is 0.1～2 liter/minute, and the time of described logical hydrogen is 2～8 hours.In the reaction process of carrying out hydrogen reduction, control agitator speed with rotating electrode.Described stirring velocity is 20～1000 rev/mins.
The present invention also can carry out like this, promptly comprises following processing step: (1) puts into reactor with rhodium, the iridium solution of finite concentration ratio; (2) under normal pressure, be raised to certain temperature feeding hydrogen and reduce, and can select different processing condition and differing temps for use, it is carried out rhodium and the iridium that multipole reduction obtains different purity according to the different concns ratio of rhodium, iridium.
In the inventive method, rhodium is reduced into metal, and iridium is not reduced.Hydrogen purity＞99.95% is controlled agitator speed with rotating electrode.
The present invention is a raw material with rhodium, iridium solution, with hydrogen reducing separate rhodium, iridium, can more efficiently realize the thorough separation of rhodium, iridium under normal pressure, is a kind of separation method preferably, has that reaction process is short, the rate of recovery of rhodium and iridium advantages of higher very all.After the separation, the purity of iridium＞99.99%; The purity of rhodium＞99%.That the advantage of present method is is pollution-free, flow process short, it is more thorough to separate, and can select different processing condition and differing temps for use according to the different concns ratio of rhodium, iridium, and it is carried out rhodium and the iridium that multipole reduction obtains different purity.Problems such as this project is the novel method of a kind of separate rhodium, iridium, and the process that can overcome traditional method is tediously long, separate thoroughly, direct yield is not high can increase substantially the rate of recovery of iridium, improve the purity of rhodium.In sum as can be seen: the present invention has significant technical progress and outstanding substantive distinguishing features, can produce good economic and social benefit.
Embodiment:
Embodiment 1:
Chloro-iridic acid (38g/l) storing solution of getting the chlorine rhodium acid (45.5g/l) of 0.44ml and 2.6ml is made into rhodium-containing 0.1g/l, contains the solution 200ml of iridium 1.5g/l in volumetric flask.Its acidity is pH=1, change the rhodium iridium solution for preparing over to homemade glass reactor after, begin stir to heat up, stirring velocity is 600 rev/mins, after treating that temperature reaches 70 ℃, feed hydrogen and fast its flow is transferred to 200 ml/min, pick up counting, after reaction reaches 2 hours, close hydrogen and feed nitrogen simultaneously, remove hydrogen unnecessary in the reactor, get 10 ml solns and filter in the exsiccant volumetric flask, analyze the concentration of metal rhodium in the filtrate, its result is 0.0005g/l for rhodium-containing in the solution.Reduction ratio is 99.5%.
Embodiment 2
Chloro-iridic acid (38g/l) storing solution of getting the chlorine rhodium acid (45.5g/l) of 0.44ml and 7.9ml is made into rhodium-containing 0.1g/l, contains the solution 200ml of iridium 1.5g/l in volumetric flask.Its acidity is pH=1, change the rhodium iridium solution for preparing over to homemade glass reactor after, begin stir to heat up, stirring velocity is 600 rev/mins, after treating that temperature reaches 70 ℃, feed hydrogen and fast its flow is transferred to 400 ml/min, pick up counting, after reaction reaches 2 hours, close hydrogen and feed nitrogen simultaneously, remove hydrogen unnecessary in the reactor, get 10 ml solns and filter in the exsiccant volumetric flask, analyze the concentration of metal rhodium in the filtrate, its result is 0.00036g/l for rhodium-containing in the solution.Reduction ratio is 99.64%.
Embodiment 3
Chloro-iridic acid (38g/l) storing solution of getting the chlorine rhodium acid (45.5g/l) of 0.33ml and 7.9ml is made into rhodium-containing 0.075g/l, contains the solution 200ml of iridium 1.5g/l in volumetric flask.Its acidity is pH=1, change the rhodium iridium solution for preparing over to homemade glass reactor after, begin stir to heat up, stirring velocity is 600 rev/mins, after treating that temperature reaches 70 ℃, feed hydrogen and fast its flow is transferred to 200 ml/min, pick up counting, after reaction reaches 2 hours, close hydrogen and feed nitrogen simultaneously, remove hydrogen unnecessary in the reactor, get 10 ml solns and filter in the exsiccant volumetric flask, analyze the concentration of metal rhodium in the filtrate, its result is 0.00046g/l for rhodium-containing in the solution.Reduction ratio is 99.4%.
Embodiment 4
Chloro-iridic acid (38g/l) storing solution of getting the chlorine rhodium acid (45.5g/l) of 0.44ml and 7.9ml is made into rhodium-containing 0.1g/l, contains the solution 200ml of iridium 1.5g/l in volumetric flask.Its acidity is pH=1, change the rhodium iridium solution for preparing over to homemade glass reactor after, begin stir to heat up, stirring velocity is 800 rev/mins, after treating that temperature reaches 70 ℃, feed hydrogen and fast its flow is transferred to 200 ml/min, pick up counting, after reaction reaches 2 hours, close hydrogen and feed nitrogen simultaneously, remove hydrogen unnecessary in the reactor, get 10 ml solns and filter in the exsiccant volumetric flask, analyze the concentration of metal rhodium in the filtrate, its result is 0.0004g/l for rhodium-containing in the solution.Reduction ratio is 99.6%.
Claims (7)
1, a kind of hydrogen reduction separates the novel method of rhodium in the iridium solution, and it is characterized in that comprising following processing step: (1) puts into reactor with rhodium, the iridium solution of finite concentration ratio; (2) being raised to certain temperature feeding hydrogen under normal pressure reduces.
2, hydrogen reduction according to claim 1 separates the method for rhodium in the iridium solution, it is characterized in that: the mass ratio of described rhodium and iridium＜1: 10, the concentration of hydrochloric acid [H of described iridium solution
+]=1～0.002mol/1.
3, hydrogen reduction according to claim 1 separates the method for rhodium in the iridium solution, and it is characterized in that: described reactor has the insulation interlayer, feeds 50～80 ℃ hot water in the reaction process in the insulation interlayer.
4, hydrogen reduction according to claim 1 separates the method for rhodium in the iridium solution, and it is characterized in that: the flow of described hydrogen is 0.1～2 liter/minute, and the time of described logical hydrogen is 2～8 hours.
5, hydrogen reduction according to claim 1 separates the method for rhodium in the iridium solution, it is characterized in that: in the reaction process of carrying out hydrogen reduction, control agitator speed with rotating electrode.
6, hydrogen reduction according to claim 5 separates the method for rhodium in the iridium solution, and it is characterized in that: described stirring velocity is 20～1000 rev/mins.
7, a kind of hydrogen reduction separates the novel method of rhodium in the iridium solution, and it is characterized in that: it is characterized in that comprising following processing step: (1) puts into reactor with rhodium, the iridium solution of finite concentration ratio; (2) under normal pressure, be raised to certain temperature feeding hydrogen and reduce, and can select different processing condition and differing temps for use, it is carried out rhodium and the iridium that multipole reduction obtains different purity according to the different concns ratio of rhodium, iridium.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2003101219836A CN1260378C (en) | 2003-12-10 | 2003-12-10 | New method for hydrogen reduction separating rhodium in iridium solution |
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|---|---|---|---|
| CNB2003101219836A CN1260378C (en) | 2003-12-10 | 2003-12-10 | New method for hydrogen reduction separating rhodium in iridium solution |
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| CN1626690A true CN1626690A (en) | 2005-06-15 |
| CN1260378C CN1260378C (en) | 2006-06-21 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103302298A (en) * | 2013-06-03 | 2013-09-18 | 贵研资源（易门）有限公司 | Method for separating and purifying iridium |
| CN103343239A (en) * | 2013-07-25 | 2013-10-09 | 贵研资源（易门）有限公司 | Method for separating and purifying rhodium |
| CN113008723A (en) * | 2021-02-03 | 2021-06-22 | 广东金正龙科技有限公司 | Method for detecting content of high-purity rhodium compound solution |
| CN113020615A (en) * | 2021-03-03 | 2021-06-25 | 中海油(山西)贵金属有限公司 | Method for preparing high-purity rhodium powder by using rhodium trichloride |
| CN113816846A (en) * | 2021-09-15 | 2021-12-21 | 浙江微通催化新材料有限公司 | Method for synthesizing rhodium carboxylate dimer based on hydrogen reduction |
-
2003
- 2003-12-10 CN CNB2003101219836A patent/CN1260378C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103302298A (en) * | 2013-06-03 | 2013-09-18 | 贵研资源（易门）有限公司 | Method for separating and purifying iridium |
| CN103302298B (en) * | 2013-06-03 | 2015-11-18 | 贵研资源（易门）有限公司 | A kind of method of separating-purifying iridium |
| CN103343239A (en) * | 2013-07-25 | 2013-10-09 | 贵研资源（易门）有限公司 | Method for separating and purifying rhodium |
| CN103343239B (en) * | 2013-07-25 | 2014-08-20 | 贵研资源（易门）有限公司 | Method for separating and purifying rhodium |
| CN113008723A (en) * | 2021-02-03 | 2021-06-22 | 广东金正龙科技有限公司 | Method for detecting content of high-purity rhodium compound solution |
| CN113020615A (en) * | 2021-03-03 | 2021-06-25 | 中海油(山西)贵金属有限公司 | Method for preparing high-purity rhodium powder by using rhodium trichloride |
| CN113816846A (en) * | 2021-09-15 | 2021-12-21 | 浙江微通催化新材料有限公司 | Method for synthesizing rhodium carboxylate dimer based on hydrogen reduction |
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|---|---|
| CN1260378C (en) | 2006-06-21 |
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Granted publication date: 20060621 Termination date: 20121210 |