CN103341639B - Method for dissolving rhodium powder difficult to dissolve - Google Patents
Method for dissolving rhodium powder difficult to dissolve Download PDFInfo
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- CN103341639B CN103341639B CN201310313714.3A CN201310313714A CN103341639B CN 103341639 B CN103341639 B CN 103341639B CN 201310313714 A CN201310313714 A CN 201310313714A CN 103341639 B CN103341639 B CN 103341639B
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Abstract
The invention relates to a method for dissolving rhodium powder difficult to dissolve. An HAuCl4 solution and the rhodium powder are subjected to a redox reaction under specified conditions, as a result, the rhodium powder is oxidized and dissolved to generate an H3RhCl6 solution while the HAuCl4 in the original solution is reduced to generate sponge gold powder. According to the specific technical scheme, the method comprises the following steps: (1) gold dissolution, wherein aqua regia is used for dissolving the sponge gold, and the purity of the gold is greater than 99.95%; (2) concentration and nitrate removal; (3) dissolution of the rhodium powder, wherein the HAuCl4 solution after the nitrate removal is placed in a three-mouth flask, the rhodium powder is added into the HAuCl4 solution while the HAuCl4 solution is stirred, and then the solution is heated to dissolve the rhodium powder; (4) filtering and washing, wherein the dissolved solution is cooled, filtered and washed to obtain the H3RhCl6 solution with the purity greater than 99.95%. By means of the method, the dissolution rate of the rhodium powder is greater than 95%; the process is simple, production cost is low, environmental pollution is little, and industrialization is easy to realize.
Description
Technical field
The present invention relates to technical field of noble metal metallurgy, particularly relate to a kind of dissolving method of indissoluble pure rhodium powder, be also applicable to the dissolving of the higher powdery rhodium waste material of rhodium content simultaneously.
Background technology
The rhodium raw material mainly pure rhodium powder supplied in the market, pure rhodium powder compact structure, has higher chemical inertness, is therefore difficult to be dissolved; And the rhodium of 80 ~ 90% is the form (as: RhCl with compound
3nH
2o, Rh
2(SO
4)
3, Rh (NO
3)
3, RhI
3, Rh (OAc)
x, RhH (CO) (PPh
3)
3deng) be widely used in the industry such as auto-exhaust catalyst, medical catalyst, Effect of Catalysis In Petrochemistry agent, therefore, the dissolving of rhodium is the prerequisite of application, and rhodium powder first must be converted into the basic compound of rhodium, then carries out being processed into coating material, rhodanizing liquid, organo-rhodium compounds etc.; Meanwhile, in powdery rhodium waste material, the recovery of rhodium also be unable to do without the dissolving of rhodium, and therefore the dissolving technology of rhodium is extremely important.
According to the content of rhodium, structure and existing forms, rhodium powder can adopt diverse ways to dissolve, and roughly can be divided into: 1. chemistry of aqueous solution dissolution method; 2. warm fusion method in; 3. high melt method; 4. electrochemical solution.
Patent CN200810236526.4, CN200610091177.2 adopt electrochemical process to dissolve rhodium powder, and prepare rhodium chloride, a solubilized 1200g pure rhodium powder, dissolution rate reaches 99.95%.The advantage of electrochemical solution is that course of dissolution does not introduce new impurity, and electrolyte can directly enter postorder refinery practice, and shortcoming is that dissolution velocity is slow.
Patent CN200910073730.3 barium peroxide fusion method process Pt-Rh bianry alloy net aqua regia insoluble slag (rhodium content is 30% ~ 80%).Detailed process is: fully mixed by the barium peroxide of aqua regia insoluble slag and 4 ~ 6 times amount, be warming up to 800 ~ 950 DEG C, constant temperature a period of time, makes rhodium be converted into acid-soluble compound.But the method can introduce a large amount of barium impurity, brings difficulty, SO to the separating-purifying of rhodium
4 2-precipitation is except in the process of barium, and precipitation is carried secretly, absorbed portion rhodium, reduces the rate of recovery of rhodium, and therefore domestic Jin You minority producer uses.
Patent CN200810058706.8 adopts hydrochloric acid+oxidant dissolved under pressure method to dissolve rhodium, and add pressure hydrochloric acid large to equipment corrosion, equipment cannot resist the corrosion of hydrochloric acid, does not also realize industrialization at present.
Summary of the invention
Main purpose of the present invention is to provide a kind of dissolving method of indissoluble rhodium powder.The present invention HAuCl
4the redox reaction that solution and rhodium powder occur under given conditions, rhodium pruinescence oxidation dissolution generates H
3rhCl
6solution, and the HAuCl in solution
4be reduced and generate sponge bronze.In hydrochloric acid medium, HAuCl
4the redox reaction of solubilize rhodium powder is such as formula (1):
2HAuCl
4+ 2Rh + 4HCl → 2Au + 2H
3RhCl
6（1）
In course of reaction, rhodium powder is excessive, final H
3rhCl
6[AuCl in solution
4 -] ion is reduced substantially, is conducive to the quality improving follow-up rhodium based compound product.
The present invention carries out successively mainly through following steps:
(1) dissolving of gold: dissolve cake of gold with wang aqueous solution in there-necked flask, the purity > 99.95% of cake of gold;
(2) concentrate, catch up with nitre: by the HAuCl of step (1) gained
4concentrate after solution cooling, catch up with nitre;
(3) dissolving of rhodium powder: the solution of step (2) gained is put into there-necked flask, adds rhodium powder while stirring, then heating for dissolving;
(4) filtration washing: by the solution cooled and filtered of step (3) gained, washing, filtrate is the H of higher degree
3rhCl
6solution;
The quality of cake of gold described in step (1): the quality=1 ~ 2:1 of rhodium powder, the reaction condition of cake of gold aqua regia dissolution is: solid-to-liquid ratio=1:1 ~ 5, temperature 90 ~ 120 DEG C, 30 ~ 180 minutes time, stir speed (S.S.) 20 ~ 100 r/min;
The HAuCl after nitre is caught up with described in step (2)
4the ion concentration of GOLD FROM PLATING SOLUTION is 50 ~ 400 g/L, and concentration of hydrochloric acid is 6 ~ 12mol/L;
The reaction condition that rhodium powder described in step (3) dissolves is: the solid-to-liquid ratio (quality of rhodium powder: HAuCl
4the volume of solution)=1:3 ~ 10, temperature 80 ~ 150 DEG C, 1 ~ 20 hour time, stir speed (S.S.) 10 ~ 50 r/min; Use HAuCl
4in solubilize rhodium powder process, there-necked flask adds condensation reflux unit, the non-volatile loss of hydrochloric acid;
The present invention adopts HAuCl
4solution dissolves rhodium powder, compared with prior art has the following advantages: the dissolution rate > 95% of (1) rhodium powder, is not returned next group by the rhodium powder dissolved on a small quantity, and final rhodium powder can be dissolved almost completely; (2) loss of rhodium is low, rhodium rate of recovery > 99.8%; (3) in rhodium powder course of dissolution, auri does not originally lose, and can realize the closed circulation that cake of gold dissolves rhodium powder; (4) H obtained
3rhCl
6the content < 30ppm of GOLD FROM PLATING SOLUTION, does not introduce other impurity element, the rhodium based compound constant product quality of production; (5) present invention process is simple, and production cost is low, and environmental pollution is little, is easy to realize industrialization.
Accompanying drawing explanation
Fig. 1 is process chart of the present invention.
Detailed description of the invention
Below in conjunction with accompanying drawing 1 and instantiation, the present invention is described in further detail, and verifies its effect.
Embodiment one
Take the cake of gold 400 grams that purity is greater than 99.95%, dissolve with 1.6 L wang aqueous solutions, concentrate after cake of gold dissolving completely, catch up with nitre, after being diluted to 1 L, put into there-necked flask, open mechanical agitation, then take the pure rhodium powder 205 grams that Umicore Company produces, purity is 99.98%, slowly adds in there-necked flask, heating for dissolving, temperature 110 DEG C, 5 hours time, stir speed (S.S.) 30 r/min; After dissolving completes, cold filtration, washing, filtrate is the H of 99.98% purity
3rhCl
6solution, rhodium-containing 197.32g, dissolution rate is 98.66%.
Embodiment two
Take the cake of gold 400 grams that purity is greater than 99.95%, dissolve with 1.6 L wang aqueous solutions, concentrate after cake of gold dissolving completely, catch up with nitre, after being diluted to 1 L, put into there-necked flask, open mechanical agitation, then take the pure rhodium powder 205 grams that Heraeus Inc. produces, purity is 99.97%, slowly adds in there-necked flask, heating for dissolving, temperature 110 DEG C, 5 hours time, stir speed (S.S.) 30 r/min; After dissolving completes, cold filtration, washing, filtrate is the H of 99.97% purity
3rhCl
6solution, rhodium-containing 197.88g, dissolution rate is 98.94%.
Embodiment three
Take the cake of gold 400 grams that purity is greater than 99.95%, dissolve with 1.6 L wang aqueous solutions, concentrate after cake of gold dissolving completely, catch up with nitre, after being diluted to 1 L, put into there-necked flask, open mechanical agitation, then take the pure rhodium powder 205 grams that village letter Wan Feng company produces, purity is 99.95%, slowly adds in there-necked flask, heating for dissolving, temperature 110 DEG C, 5 hours time, stir speed (S.S.) 30r/min; After dissolving completes, cold filtration, washing, filtrate is the H of 99.95% purity
3rhCl
6solution, rhodium-containing 198.26g, dissolution rate is 99.13%.
Embodiment four
Take the cake of gold 400 grams that purity is greater than 99.95%, dissolve with 1.6 L wang aqueous solutions, concentrate after cake of gold dissolving completely, catch up with nitre, after being diluted to 1 L, put into there-necked flask, open mechanical agitation, then take the expensive pure rhodium powder 205 grams grinding resource (Yimen) Co., Ltd and produce, purity is 99.95%, slowly adds in there-necked flask, heating for dissolving, temperature 110 DEG C, 5 hours time, stir speed (S.S.) 30 r/min; After dissolving completes, cold filtration, washing, filtrate is the H of 99.95% purity
3rhCl
6solution, rhodium-containing 198.08g, dissolution rate is 99.04%.
Claims (1)
1. a kind of dissolving method of indissoluble rhodium powder, is characterized in that:
Adopt HAuCl
4solution and rhodium powder generation redox reaction, rhodium pruinescence oxidation dissolution generates H
3rhCl
6solution, and the HAuCl in solution
4be reduced and generate sponge bronze; Rhodium powder is excessive a little, the H finally obtained
3rhCl
6solution, H
3rhCl
6the content of GOLD FROM PLATING SOLUTION is less than 30ppm; In rhodium powder course of dissolution, auri does not originally lose, and realizes HAuCl
4the closed circulation of solubilize rhodium powder,
Specifically carry out successively as follows:
(1) dissolving of gold: dissolve cake of gold with wang aqueous solution in there-necked flask, the purity > 99.95% of cake of gold;
(2) concentrate, catch up with nitre: by the HAuCl of step (1) gained
4concentrate after solution cooling, catch up with nitre;
(3) dissolving of rhodium powder: the solution of step (2) gained is put into there-necked flask, adds rhodium powder while stirring, then heating for dissolving;
(4) filtration washing: by the solution cooled and filtered of step (3) gained, washing, filtrate is the H of higher degree
3rhCl
6solution,
The quality of cake of gold described in described step (1): the quality=1 ~ 2:1 of rhodium powder,
Described in described step (1), the reaction condition of cake of gold aqua regia dissolution is: solid-to-liquid ratio=1:1 ~ 5, temperature 80 ~ 120 DEG C, 30 ~ 180 minutes time, stir speed (S.S.) 20 ~ 100r/min,
The HAuCl after nitre is caught up with described in described step (2)
4the concentration of GOLD FROM PLATING SOLUTION is 50 ~ 400g/L, and concentration of hydrochloric acid is 6 ~ 12mol/L,
Described step uses HAuCl described in (3)
4in solubilize rhodium powder process, there-necked flask adds condensation reflux unit, the non-volatile loss of hydrochloric acid,
The reaction condition that rhodium powder described in described step (3) dissolves is: the quality of solid-to-liquid ratio and rhodium powder: HAuCl
4volume=1:3 ~ 10 of solution, temperature 80 ~ 150 DEG C, 1 ~ 20 hour time, stir speed (S.S.) 10 ~ 50r/min.
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| CN103341639B true CN103341639B (en) | 2015-03-25 |
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| CN111304457A (en) * | 2020-03-20 | 2020-06-19 | 康纳新型材料(杭州)有限公司 | Efficient activation dissolving method for rhodium powder |
| CN114427036A (en) * | 2020-09-25 | 2022-05-03 | 中国石油化工股份有限公司 | Method for dissolving rhodium powder and rhodium dissolving solution obtained by same |
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| US8088740B2 (en) * | 2009-05-04 | 2012-01-03 | Gwangju Institute Of Science And Technology | Gold binding peptides and shape-and size-tunable synthesis of gold nanostructures |
| CN102703691A (en) * | 2012-06-20 | 2012-10-03 | 四川省天泽贵金属有限责任公司 | New technology for extracting high-purity gold by adopting wet process |
| CN103074492B (en) * | 2013-01-24 | 2014-08-20 | 贵研资源（易门）有限公司 | Method for separating and purifying gold from noble metal solution |
| CN103088221A (en) * | 2013-02-22 | 2013-05-08 | 昆山鸿福泰环保科技有限公司 | Gold filter element recovery technique |
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