CN110964921A - Production method of refined palladium - Google Patents
Production method of refined palladium Download PDFInfo
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- CN110964921A CN110964921A CN201811140294.2A CN201811140294A CN110964921A CN 110964921 A CN110964921 A CN 110964921A CN 201811140294 A CN201811140294 A CN 201811140294A CN 110964921 A CN110964921 A CN 110964921A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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Abstract
The invention discloses a production method of refined palladium, which is implemented according to the following steps: step 1, slurrying ammonium chloropalladate, and adding analytically pure ammonia water until the pH value of the solution is 8-9 to obtain slurry; step 2, heating and stirring the slurrying solution, then cooling and filtering to obtain a filtrate, adding analytically pure hydrochloric acid into the filtrate until the pH value of the filtrate is 0.5-1, and filtering to obtain dichlorodiamminepalladium; step 3, pulping dichlorodiamminepalladium, and adding analytically pure ammonia water until the pH value of the solution is 8-9 to obtain a pulping solution; step 4, repeating the steps 2 and 3 twice to obtain a dichlorotetra-ammine palladium solution, heating, adding analytically pure hydrazine hydrate, and standing to obtain a mixed solution; step 5, filtering the mixed solution to obtain sponge palladium, and washing and drying the sponge palladium to obtain a sponge palladium product; according to the invention, the dichlorotetraammine palladium solution is partially reduced by controlling the addition amount of hydrazine hydrate, so that impurity elements such as platinum and the like stay in the solution, and the quality stability of the sponge palladium can be improved.
Description
Technical Field
The invention belongs to the technical field of non-ferrous metal smelting, and particularly relates to a production method of refined palladium.
Background
The dichlorodiamminepalladium precipitation method is widely applied to the industrial production of sponge palladium, but the platinum element in a sponge palladium product often exceeds the standard in the production practice and is difficult to stably reach the 99.99 percent product standard. The starvation reduction method is widely applied to the gold chemical refining process, but is not applied to the sponge palladium production. Therefore, the starvation reduction method can be applied to sponge palladium production to ensure that the product quality stably reaches the 99.99 percent standard.
Disclosure of Invention
The invention aims to provide a production method of refined palladium, which can partially reduce a dichlorotetra-ammine palladium solution by controlling the addition amount of hydrazine hydrate, so that impurity elements such as platinum and the like can stay in the solution, and the quality stability of sponge palladium can be improved.
The technical scheme adopted by the invention is that the production method of the refined palladium is implemented according to the following steps:
step 1, slurrying ammonium chloropalladate, and adding analytically pure ammonia water under stirring until the pH value of the solution is 8-9 to obtain slurry;
step 2, heating and stirring the slurrying solution obtained in the step 1, then cooling and filtering to obtain a filtrate, adding analytically pure hydrochloric acid into the filtrate until the pH value of the filtrate is 0.5-1, and filtering to obtain dichlorodiamminepalladium;
step 3, pulping the dichlorodiamminepalladium in the step 2, and adding analytically pure ammonia water under the stirring condition until the pH value of the solution is 8-9 to obtain a pulping solution;
step 4, repeating the step 2 and the step 3 twice to obtain a dichlorotetra-ammine palladium solution, heating, adding analytically pure hydrazine hydrate, and standing to obtain a mixed solution;
and 5, filtering the mixed solution obtained in the step 4 to obtain sponge palladium, and washing and drying the sponge palladium to obtain a sponge palladium product.
The present invention is also characterized in that,
the specific method for slurrying ammonium chloropalladate in the step 1 comprises the following steps: mixing pure water according to the proportion of 5-10: adding the solution into ammonium chloropalladate according to the volume ratio of 1 for slurrying.
In the step 1, the mass of the analytically pure ammonia water added is 2-2.5 times of that of the ammonium chloropalladate.
In the step 2, the slurry is heated to 80-90 ℃ and stirred for 30-60 min.
In the step 2, the mass of the analytically pure hydrochloric acid added is 50-60% of the mass of the ammonium chloropalladate.
And in the step 3, the mass of the analytically pure ammonia water is 50-60% of the mass of the dichlorodiamineous palladium.
In the step 4, the heating temperature is 60-80 ℃, and the standing time is 1-2 h.
In the step 4, the concentration of the analytically pure hydrazine hydrate is 45-55%, and the mass of the hydrazine hydrate added is 8-12% of that of the ammonium chloropalladate.
And (5) after the sponge palladium is washed in the step (5), combining a washing liquid with the filtrate filtered in the step (5), adding analytically pure hydrochloric acid until the pH value of the combined solution is 0.5-1, and filtering to obtain the dichlorodiamminepalladium.
The method has the beneficial effects that the method adopts a starvation reduction method, controls the addition amount of hydrazine hydrate, partially reduces the dichloro-tetra-ammino-palladium solution, enables impurity elements such as platinum and the like to stay in the solution, and enables the sponge palladium product to have higher quality stability.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a production method of refined palladium, which is implemented according to the following steps:
step 1, mixing pure water according to the ratio of 5-10: 1, adding the solution into ammonium chloropalladate for slurrying, and adding analytically pure ammonia water under the stirring condition until the pH value of the solution is 8-9 to obtain slurry; wherein, the mass of the analytically pure ammonia water added in the step 1 is 2 to 2.5 times of that of the ammonium chloropalladate;
step 2, heating the slurry obtained in the step 1 to 80-90 ℃, stirring for 30-60min, then cooling and filtering to obtain a filtrate, adding analytically pure hydrochloric acid into the filtrate until the pH value of the filtrate is 0.5-1, and filtering to obtain dichlorodiamminepalladium; wherein, the mass of the analytically pure hydrochloric acid added is 50-60% of the mass of the ammonium chloropalladate;
step 3, pulping the dichlorodiamminepalladium in the step 2, and adding analytically pure ammonia water under the stirring condition until the pH value of the solution is 8-9 to obtain a pulping solution; wherein, the mass of the analytically pure ammonia water added is 50-60% of the mass of the dichlorodiammine palladium-in-nickel;
step 4, repeating the step 2 and the step 3 twice to obtain a dichlorotetra-ammine palladium solution, heating to 60-80 ℃, adding analytically pure hydrazine hydrate, and standing for 1-2 hours to obtain a mixed solution; wherein, the concentration of analytically pure hydrazine hydrate is 45-55%, and the mass of hydrazine hydrate added is 8-12% of that of ammonium chloropalladate;
step 5, filtering the mixed solution obtained in the step 4 to obtain sponge palladium, and washing and drying the sponge palladium to obtain a sponge palladium product;
in addition, after the sponge palladium is washed in the step 5, the washing liquid is combined with the filtrate filtered in the step 5, analytically pure hydrochloric acid is added until the pH value of the combined solution is 0.5-1, dichlorodiamminepalladium complex is obtained by filtering, and the dichlorodiamminepalladium complex enters the ammonia dissolving process of the next batch of materials, so that the reutilization is realized, and the utilization rate of the raw materials is improved.
Compared with the existing preparation method, the invention mainly has the following technical advantages: the invention adopts a starvation reduction method to control the addition of hydrazine hydrate and partially reduce the dichloro-tetra-ammino-palladium solution, so that impurity elements such as platinum and the like stay in the solution, and the sponge palladium product has higher quality stability.
Example 1
The embodiment 1 of the invention provides a production method of refined palladium, which is implemented according to the following steps:
pulping 20kg ammonium chloropalladate with pure water, slowly adding 45L of analytically pure ammonia water under stirring, detecting the pH value of the solution to be 8, heating the slurried solution to 85 ℃, stirring for 30min under the condition of keeping the temperature until flesh red tetramino palladium chloropalladate is completely dissolved, cooling the solution, filtering, slowly adding 10L of analytically pure hydrochloric acid into the filtrate, detecting the pH value of the solution to be 0.5, filtering to obtain yellow diammine dichloropalladium, slurrying the diammine dichloropalladium with pure water, adding 11L of analytically pure ammonia water under stirring, detecting the pH value of the solution to be 9, repeating the acidification-ammonia dissolution process for 2 times to obtain a diammine dichloropalladium solution, heating to 60 ℃, adding 2L of 50 percent analytically pure hydrazine hydrate under stirring, standing for 2h, filtering to obtain sponge palladium, washing with hot water, drying to obtain a sponge palladium product, merging the filtrate and washing liquid, adding analytically pure hydrochloric acid 5L, detecting the pH value of the solution to be 0.5, filtering to obtain yellow dichlorodiamminepalladium, and entering the ammonia dissolving process of the next batch of materials.
Example 2
The embodiment 2 of the invention provides a production method of refined palladium, which is implemented according to the following steps:
22kg of ammonium chloropalladate is slurried with pure water, 48L of analytically pure ammonia water is slowly added under stirring, and the pH value of the solution is detected to be 9. Heating the slurry to 88 ℃, and stirring for 60min under the condition of keeping the temperature until the flesh red palladium chloride-palladium tetraammine palladium chloride is completely dissolved. And cooling the solution, filtering, slowly adding 12L of analytically pure hydrochloric acid into the filtrate, detecting the pH value of the solution to be 0.5, and filtering to obtain yellow dichlorodiamminepalladium. Slurrying dichlorodiamminepalladium with pure water, adding 12L of analytically pure ammonia water under the stirring condition, detecting the pH value of the solution to be 9, repeating the acidification-ammonia dissolution process for 2 times to obtain a dichlorotetramminepalladium solution, heating to 70 ℃, adding 2.5L of 50% analytically pure hydrazine hydrate under the stirring condition, standing for 1h, filtering to obtain sponge palladium, washing with hot water, and drying to obtain a sponge palladium product. And combining the filtrate and washing liquor, adding 6L of analytically pure hydrochloric acid, detecting the pH value of the solution to be 0.5, filtering to obtain yellow dichlorodiamminepalladium, and performing ammonia dissolving process of the next batch of materials.
Example 3
Embodiment 3 of the present invention provides a production method of refined palladium, which is specifically implemented according to the following steps:
slurrying 18kg of ammonium chloropalladate with pure water, slowly adding 40L of analytically pure ammonia water under the stirring condition, detecting the pH value of the solution to be 8, heating the slurried solution to 82 ℃, stirring for 45min under the condition of keeping the temperature until meat red tetraamminepalladium chloropalladate is completely dissolved, cooling the solution, filtering, slowly adding 9L of analytically pure hydrochloric acid into the filtrate, detecting the pH value of the solution to be 1, and filtering to obtain yellow dichlorodiamminepalladium. Pulping dichlorodiamminepalladium with pure water, adding 10L of analytically pure ammonia water under the stirring condition, detecting the pH value of the solution to be 8, repeating the acidification-ammonia dissolution process for 2 times to obtain a dichlorotetramminepalladium solution, heating to 80 ℃, adding 2L of 50% analytically pure hydrazine hydrate under the stirring condition, standing for 1h, filtering to obtain sponge palladium, washing with hot water, drying to obtain a sponge palladium product, combining the filtrate with a washing solution, adding 4L of analytically pure hydrochloric acid, detecting the pH value of the solution to be 0.5, filtering to obtain yellow dichlorodiamminepalladium, and performing ammonia dissolution on the next batch of materials.
Example 4
Embodiment 4 of the present invention provides a production method of refined palladium, which is specifically implemented according to the following steps:
pulping 18kg of ammonium chloropalladate with pure water, slowly adding 40L of analytically pure ammonia water under the stirring condition, detecting the pH value of the solution to be 8, heating the slurried solution to 84 ℃, stirring for 60min under the temperature maintaining condition until flesh red tetramino palladium chloropalladate is completely dissolved, cooling the solution, filtering, slowly adding 9L of analytically pure hydrochloric acid into the filtrate, detecting the pH value of the solution to be 0.8, filtering to obtain yellow diammine dichloropalladium, slurrying the diammine dichloropalladate with pure water, adding 10L of analytically pure ammonia water under the stirring condition, detecting the pH value of the solution to be 8.5, repeating the acidification-ammonia dissolution process for 2 times to obtain a diammine dichloropalladate solution, heating to 60 ℃, adding 2L of 55 percent analytically pure hydrazine hydrate under the stirring condition, standing for 1.2h, filtering to obtain sponge palladium, washing with hot water, and drying to obtain a sponge palladium product. And combining the filtrate and washing liquor, adding 4L of analytically pure hydrochloric acid, detecting the pH value of the solution to be 0.6, filtering to obtain yellow dichlorodiamminepalladium, and performing ammonia dissolving process of the next batch of materials.
Example 5
Embodiment 5 of the present invention provides a production method of refined palladium, which is specifically implemented according to the following steps:
19kg of ammonium chloropalladate is slurried with pure water, 40L of analytically pure ammonia water is slowly added under the stirring condition, and the pH value of the detection solution is 8.8. Heating the slurry to 89 ℃, stirring for 50min under the condition of keeping the temperature until flesh red palladium chloride tetraammine palladium chloride is completely dissolved, cooling the solution, filtering, slowly adding 9L of analytically pure hydrochloric acid into the filtrate, detecting the pH value of the solution to be 0.5, and filtering to obtain yellow palladium dichloride tetraammine palladium chloride. Pulping dichlorodiamminepalladium with pure water, adding 11L of analytically pure ammonia water under the stirring condition, detecting the pH value of the solution to be 8, repeating the acidification-ammonia dissolution process for 2 times to obtain a dichlorotetramminepalladium solution, heating to 80 ℃, adding 2L of 45% analytically pure hydrazine hydrate under the stirring condition, standing for 1h, filtering to obtain sponge palladium, washing with hot water, drying to obtain a sponge palladium product, combining the filtrate with a washing solution, adding 4L of analytically pure hydrochloric acid, detecting the pH value of the solution to be 1, filtering to obtain yellow dichlorodiamminepalladium, and entering the ammonia dissolution process of the next batch of materials.
Example 6
Embodiment 6 of the present invention provides a production method of refined palladium, which is specifically implemented according to the following steps:
slurrying 18.5kg of ammonium chloropalladate with pure water, slowly adding 43L of analytically pure ammonia water under the stirring condition, detecting the pH value of the solution to be 8, heating the slurried solution to 90 ℃, and stirring for 60min under the condition of keeping the temperature until flesh red tetraammine palladium chloropalladate is completely dissolved. And cooling the solution, filtering, slowly adding 9L of analytically pure hydrochloric acid into the filtrate, detecting the pH value of the solution to be 1, and filtering to obtain yellow dichlorodiamminepalladium. Pulping dichlorodiamminepalladium with pure water, adding 10L of analytically pure ammonia water under the stirring condition, detecting the pH value of the solution to be 9, repeating the acidification-ammonia dissolution process for 2 times to obtain a dichlorotetramminepalladium solution, heating to 85 ℃, adding 2L of 48% analytically pure hydrazine hydrate under the stirring condition, standing for 1h, filtering to obtain sponge palladium, washing with hot water, drying to obtain a sponge palladium product, combining the filtrate with a washing solution, adding 4L of analytically pure hydrochloric acid, detecting the pH value of the solution to be 0.6, filtering to obtain yellow dichlorodiamminepalladium, and performing ammonia dissolution on the next batch of materials.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention.
Claims (9)
1. The production method of the refined palladium is characterized by comprising the following steps:
step 1, slurrying ammonium chloropalladate, and adding analytically pure ammonia water under stirring until the pH value of the solution is 8-9 to obtain slurry;
step 2, heating and stirring the slurrying solution obtained in the step 1, then cooling and filtering to obtain a filtrate, adding analytically pure hydrochloric acid into the filtrate until the pH value of the filtrate is 0.5-1, and filtering to obtain dichlorodiamminepalladium;
step 3, pulping the dichlorodiamminepalladium in the step 2, and adding analytically pure ammonia water under the stirring condition until the pH value of the solution is 8-9 to obtain a pulping solution;
step 4, repeating the step 2 and the step 3 twice to obtain a dichlorotetra-ammine palladium solution, heating, adding analytically pure hydrazine hydrate, and standing to obtain a mixed solution;
and 5, filtering the mixed solution obtained in the step 4 to obtain sponge palladium, and washing and drying the sponge palladium to obtain a sponge palladium product.
2. The method for producing refined palladium according to claim 1, wherein the specific method for slurrying ammonium chloropalladate in step 1 is as follows: mixing pure water according to the proportion of 5-10: adding the solution into ammonium chloropalladate according to the volume ratio of 1 for slurrying.
3. A refined palladium production method according to claim 2, characterized in that said analytically pure ammonia water added in step 1 is 2-2.5 times the mass of ammonium chloropalladate.
4. A refined palladium production method according to claim 3, wherein in step 2, the slurry is heated to 80-90 ℃ and stirred for 30-60 min.
5. The method for producing refined palladium according to claim 4, wherein the analytically pure hydrochloric acid is added in an amount of 50% -60% by mass of the ammonium chloropalladate in step 2.
6. A refined palladium production method as claimed in claim 5 wherein said analytically pure ammonia water in step 3 is added in an amount of 50% -60% by mass of dichlorodiamineous palladium.
7. A production method for refined palladium according to claim 6, wherein said heating temperature in step 4 is 60-80 ℃ and the standing time is 1-2 h.
8. A refined palladium production method as claimed in claim 7, wherein in step 4, the concentration of the analytically pure hydrazine hydrate is 45% -55%, and the added mass of the hydrazine hydrate is 8% -12% of the mass of the ammonium chloropalladate.
9. A refined palladium production method as claimed in any one of claims 1 to 8 wherein, after sponge palladium is washed in step 5, the washing solution is combined with the filtrate filtered in step 5, analytically pure hydrochloric acid is added until the pH value of the combined solution is 0.5 to 1, and then the combined solution is filtered to obtain dichlorodiamminepalladium, and the ammonia solution process of the next batch of materials is carried out.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113151678A (en) * | 2021-04-06 | 2021-07-23 | 贵溪华晋铜业有限公司 | Method for recovering noble metal from raw material containing noble metal |
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CN102242276A (en) * | 2011-06-13 | 2011-11-16 | 白银万山稀贵金属科技有限责任公司 | Process for extracting noble metal palladium from industrial solid wastes |
CN103014352A (en) * | 2013-01-08 | 2013-04-03 | 昆明贵金属研究所 | Method for smelting and extracting platinum metal from alumina-supported petrochemical catalyst |
CN103898325A (en) * | 2012-12-27 | 2014-07-02 | 深圳市格林美高新技术股份有限公司 | Method for recovering valuable metals from scraped auto parts |
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GB922021A (en) * | 1959-01-22 | 1963-03-27 | Laporte Chemical | Recovery of palladium from catalysts |
JPH10130703A (en) * | 1996-10-24 | 1998-05-19 | Sumitomo Metal Mining Co Ltd | Production of palladium powder |
CN102242276A (en) * | 2011-06-13 | 2011-11-16 | 白银万山稀贵金属科技有限责任公司 | Process for extracting noble metal palladium from industrial solid wastes |
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