CN103341639A - Method for dissolving rhodium powder difficult to dissolve - Google Patents
Method for dissolving rhodium powder difficult to dissolve Download PDFInfo
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- CN103341639A CN103341639A CN2013103137143A CN201310313714A CN103341639A CN 103341639 A CN103341639 A CN 103341639A CN 2013103137143 A CN2013103137143 A CN 2013103137143A CN 201310313714 A CN201310313714 A CN 201310313714A CN 103341639 A CN103341639 A CN 103341639A
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- rhodium powder
- dissolving
- rhodium
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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 the precious metals metallurgy technical field, relate in particular to a kind of dissolving method of indissoluble pure rhodium powder, also be applicable to the dissolving of the powdery rhodium waste material that rhodium content is higher simultaneously.
Background technology
Gong Ying rhodium raw material mainly is pure rhodium powder in the market, and the pure rhodium powder compact structure has higher chemical inertness, therefore is difficult to dissolved; And 80 ~ 90% rhodium 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, petrochemical industry catalyst, therefore, the dissolving of rhodium is the prerequisite of using, and the rhodium powder must be converted into the basic compound of rhodium earlier, is processed into coating material, rhodanizing liquid, organic rhodium compound etc. again; Simultaneously, the recovery of rhodium also be unable to do without the dissolving of rhodium in the powdery rhodium waste material, so the dissolving technology of rhodium is extremely important.
According to content, the structure of rhodium and there is form, the rhodium powder can adopt the diverse ways dissolving, 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 dissolving rhodium powder, the preparation rhodium chloride, and a solubilized 1200g pure rhodium powder, dissolution rate reaches 99.95%.The advantage of electrochemical solution is that course of dissolution is not introduced new impurity, and electrolyte can directly enter the postorder refinery practice, and shortcoming is that dissolution velocity is slow.
Patent CN200910073730.3 handles Pt-Rh bianry alloy net aqua regia insoluble slag (rhodium content is 30%～80%) with the barium peroxide fusion method.Detailed process is: the abundant mixing of barium peroxide with aqua regia insoluble slag and 4 ~ 6 times of amounts, be warming up to 800 ~ 950 ℃, and constant temperature a period of time, make rhodium be converted into acid-soluble compound.But the method can be introduced a large amount of barium impurity, brings difficulty, SO for the separation purification of rhodium
4 2-Precipitation is except in the process of barium, and precipitation is carried secretly, the absorbed portion rhodium, has reduced the rate of recovery of rhodium, and therefore domestic only have minority producer to use.
Patent CN200810058706.8 adopts hydrochloric acid+oxidant dissolved under pressure method dissolving rhodium, adds that to depress hydrochloric acid big to equipment corrosion, and equipment can't be resisted the corrosion of hydrochloric acid, does not also realize industrialization at present.
Summary of the invention
Main purpose of the present invention provides a kind of dissolving method of indissoluble rhodium powder.The present invention HAuCl
4The redox reaction that solution and rhodium powder take place under given conditions, rhodium pruinescence oxidation dissolution generates H
3RhCl
6Solution, and the HAuCl in the solution
4Be reduced and generate the sponge bronze.In hydrochloric acid medium, HAuCl
4The redox reaction of solution dissolving rhodium powder is suc as formula (1):
2HAuCl
4 + 2Rh + 4HCl → 2Au + 2H
3RhCl
6 （1）
The rhodium powder is excessive in the course of reaction, final H
3RhCl
6[AuCl in the solution
4 -] ion is reduced substantially, is conducive to improve the quality of follow-up rhodium based compound product.
The present invention mainly carries out as follows successively:
(1) Jin dissolving: in there-necked flask, dissolve cake of gold with wang aqueous solution, the purity of cake of gold＞99.95%;
(2) concentrate, catch up with nitre: with the HAuCl of step (1) gained
4Concentrate, catch up with nitre after the solution cooling;
(3) dissolving of rhodium powder: the solution of step (2) gained is put into there-necked flask, add the rhodium powder while stirring, then heating for dissolving;
(4) filtration washing: with solution cooled and filtered, the washing of step (3) gained, filtrate is the H of higher degree
3RhCl
6Solution;
The quality of cake of gold described in the step (1): the quality of rhodium powder=1 ~ 2:1, cake of gold with the reaction condition of aqua regia dissolution is: solid-to-liquid ratio=1:1 ~ 5,90 ~ 120 ℃ of temperature, 30 ~ 180 minutes time, stir speed (S.S.) 20 ~ 100 r/min;
Catch up with the HAuCl behind the nitre described in the 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 of the dissolving of rhodium powder described in the step (3) is: the solid-to-liquid ratio (quality of rhodium powder: HAuCl
4The volume of solution)=and 1:3 ~ 10,80 ~ 150 ℃ of temperature, 1 ~ 20 hour time, stir speed (S.S.) 10 ~ 50 r/min; Use HAuCl
4In the solution dissolving rhodium powder process, add condensation reflux unit at there-necked flask, the non-volatile loss of hydrochloric acid;
The present invention adopts HAuCl
4Solution dissolves the rhodium powder, and following advantage is compared with prior art arranged: dissolution rate＞95% of (1) rhodium powder, and a small amount of not dissolved rhodium powder returns next group, and final rhodium powder can all be dissolved; (2) loss of rhodium is low, the rhodium rate of recovery＞99.8%; (3) auri does not originally lose in the rhodium powder course of dissolution, can realize the closed circulation of cake of gold dissolving rhodium powder; (4) H that obtains
3RhCl
6Content＜the 30ppm of GOLD FROM PLATING SOLUTION does not introduce other impurity element, the rhodium based compound constant product quality of production; (5) technology of the present invention is simple, and production cost is low, and environmental pollution is little, is easy to realize industrialization.
Description of drawings
Fig. 1 is process chart of the present invention.
The specific embodiment
Below in conjunction with accompanying drawing 1 and instantiation the present invention is done to describe in further detail, and verify its effect.
Embodiment one
Take by weighing purity greater than 99.95% cake of gold, 400 grams, with 1.6 L wang aqueous solutions dissolvings, concentrate, catch up with nitre after the cake of gold dissolving fully, put into there-necked flask after being diluted to 1 L, open mechanical agitation, take by weighing pure rhodium powder 205 grams that Umicore Company produces then, purity is 99.98%, slowly adds in the there-necked flask, heating for dissolving, 110 ℃ of temperature, 5 hours time, stir speed (S.S.) 30 r/min; After dissolving is finished, cold filtration, washing, filtrate is the H of 99.98% purity
3RhCl
6Solution, rhodium-containing 197.32g, dissolution rate are 98.66%.
Embodiment two
Take by weighing purity greater than 99.95% cake of gold, 400 grams, with 1.6 L wang aqueous solutions dissolvings, concentrate, catch up with nitre after the cake of gold dissolving fully, put into there-necked flask after being diluted to 1 L, open mechanical agitation, take by weighing pure rhodium powder 205 grams that Heraeus Inc. produces then, purity is 99.97%, slowly adds in the there-necked flask, heating for dissolving, 110 ℃ of temperature, 5 hours time, stir speed (S.S.) 30 r/min; After dissolving is finished, cold filtration, washing, filtrate is the H of 99.97% purity
3RhCl
6Solution, rhodium-containing 197.88g, dissolution rate are 98.94%.
Embodiment three
Take by weighing purity greater than 99.95% cake of gold, 400 grams, with 1.6 L wang aqueous solutions dissolvings, concentrate, catch up with nitre after the cake of gold dissolving fully, put into there-necked flask after being diluted to 1 L, open mechanical agitation, take by weighing pure rhodium powder 205 grams that village letter Wan Feng company produces then, purity is 99.95%, slowly adds in the there-necked flask, heating for dissolving, 110 ℃ of temperature, 5 hours time, stir speed (S.S.) 30 r/min; After dissolving is finished, cold filtration, washing, filtrate is the H of 99.95% purity
3RhCl
6Solution, rhodium-containing 198.26g, dissolution rate are 99.13%.
Embodiment four
Take by weighing purity greater than 99.95% cake of gold, 400 grams, with 1.6 L wang aqueous solutions dissolvings, concentrate, catch up with nitre after the cake of gold dissolving fully, put into there-necked flask after being diluted to 1 L, open mechanical agitation, take by weighing expensive pure rhodium powder 205 grams that resource (Yimen) Co., Ltd produces that grind then, purity is 99.95%, slowly adds in the there-necked flask, heating for dissolving, 110 ℃ of temperature, 5 hours time, stir speed (S.S.) 30 r/min; After dissolving is finished, cold filtration, washing, filtrate is the H of 99.95% purity
3RhCl
6Solution, rhodium-containing 198.08g, dissolution rate are 99.04%.
Claims (7)
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 the solution
4Be reduced and generate the sponge bronze; The rhodium powder is excessive a little, the H that obtains at last
3RhCl
6Solution, H
3RhCl
6The content of GOLD FROM PLATING SOLUTION is less than 30ppm; Auri does not originally lose in the rhodium powder course of dissolution, realizes HAuCl
4The closed circulation of solution dissolving rhodium powder.
2. a kind of dissolving method of indissoluble rhodium powder is characterized in that carrying out successively as follows:
(1) Jin dissolving: in there-necked flask, dissolve cake of gold with wang aqueous solution, the purity of cake of gold＞99.95%;
(2) concentrate, catch up with nitre: with the HAuCl of step (1) gained
4Concentrate, catch up with nitre after the solution cooling;
(3) dissolving of rhodium powder: the solution of step (2) gained is put into there-necked flask, add the rhodium powder while stirring, then heating for dissolving;
(4) filtration washing: with solution cooled and filtered, the washing of step (3) gained, filtrate is the H of higher degree
3RhCl
6Solution.
3. a kind of dissolving method of indissoluble rhodium powder according to claim 2 is characterized in that the quality of cake of gold described in the step (1): the quality of rhodium powder=1 ~ 2:1.
4. a kind of dissolving method of indissoluble rhodium powder according to claim 2, it is characterized in that cake of gold described in the step (1) with the reaction condition of aqua regia dissolution is: solid-to-liquid ratio=1:1 ~ 5,80 ~ 120 ℃ of temperature, 30 ~ 180 minutes time, stir speed (S.S.) 20 ~ 100r/min.
5. a kind of dissolving method of indissoluble rhodium powder according to claim 2 is characterized in that catching up with described in the step (2) HAuCl behind the nitre
4The concentration of GOLD FROM PLATING SOLUTION is 50 ~ 400 g/L, and concentration of hydrochloric acid is 6 ~ 12 mol/L.
6. a kind of dissolving method of indissoluble rhodium powder according to claim 2 is characterized in that using HAuCl described in the step (3)
4In the solution dissolving rhodium powder process, add condensation reflux unit at there-necked flask, the non-volatile loss of hydrochloric acid.
7. a kind of dissolving method of indissoluble rhodium powder according to claim 2, it is characterized in that the reaction condition of the dissolving of rhodium powder described in the step (3) is: solid-to-liquid ratio is the quality of rhodium powder: HAuCl
4Volume=the 1:3 of solution ~ 10,80 ~ 150 ℃ of temperature, 1 ~ 20 hour time, stir speed (S.S.) 10 ~ 50 r/min.
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|---|---|---|---|
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|---|---|---|---|
| CN201310313714.3A CN103341639B (en) | 2013-07-24 | 2013-07-24 | Method for dissolving rhodium powder difficult to dissolve |
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| CN103341639A true CN103341639A (en) | 2013-10-09 |
| CN103341639B CN103341639B (en) | 2015-03-25 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100280220A1 (en) * | 2009-05-04 | 2010-11-04 | 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 |
| CN103074492A (en) * | 2013-01-24 | 2013-05-01 | 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 |
-
2013
- 2013-07-24 CN CN201310313714.3A patent/CN103341639B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100280220A1 (en) * | 2009-05-04 | 2010-11-04 | 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 |
| CN103074492A (en) * | 2013-01-24 | 2013-05-01 | 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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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|---|---|
| CN103341639B (en) | 2015-03-25 |
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