CN102776526A - Recovery method of fine catalyst metal obtained after electrolysis and purification of synthetic diamond powder - Google Patents
Recovery method of fine catalyst metal obtained after electrolysis and purification of synthetic diamond powder Download PDFInfo
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- CN102776526A CN102776526A CN201210265805XA CN201210265805A CN102776526A CN 102776526 A CN102776526 A CN 102776526A CN 201210265805X A CN201210265805X A CN 201210265805XA CN 201210265805 A CN201210265805 A CN 201210265805A CN 102776526 A CN102776526 A CN 102776526A
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Abstract
The invention discloses a recovery method of fine catalyst metal obtained after electrolysis and purification of synthetic diamond powder, which comprises the following steps of: 1, filling a mixture containing catalyst metal into a filter cloth bag and placing into an electrobath; 2, injecting a hydrochloric acid into the electrobath; 3, utilizing an electrolyte to cyclically heat an acid solution through a pipeline; and finally, pumping the acid solution into the electrobath for electrolysis recovery. According to the method, the mixed materials are soaked in the acid solution with intermediate concentration at a constant intermediate temperature, metals in the mixed materials are changed into a free ion state by a chemical reaction, and the metal ions are enriched on a cathode plate by a rapid electrolysis method so as to achieve the purpose of recovery of catalyst metal, accordingly, the phenomena that the anode is seriously passivated and precious metals are seriously corroded can be avoided, the fine catalyst metal can be recovered at high efficiency and high recovery rate, the labor intensity of staff is reduced, the side reaction occurring in the electrolysis process can be avoided, and the method has the advantages of safety and environmental protection.
Description
Technical field
The present invention relates to a kind of thin catalyst metal recovery method, relate in particular to thin catalyst metal recovery method behind a kind of powder diamond synthesis refining.
Background technology
After the synthetic completion of superhard material, need the broken pack of the synthetic pellet of powder catalyst diamond be carried out electrolysis as anode.This material is in electrolytic process, and the inner catalyst metal of PM for particulate matter is progressively peeled off electrolysis from outside to inside, reaches the purpose that reclaims metal solvent.The once electrolytic catalyst metal recovery is about 85%; Residual metallic concentrates in the high magnetic mixture material after handling through follow-up a series of physical methods; This high magnetic mixture material mainly is made up of graphite, diamond, catalyst metal, and its metal content is about 70%.Catalyst metal in will this high magnetic mixture material is purified when reclaiming, and people generally adopt traditional " re-electrolysis " process method.But there is following shortcoming in this method:
Since mixture be discrete particulate form, particle diameter is 0.035 millimeter, in anode bag for electrolyzing because gravitational compaction, the conduction specific surface area little; Cause circulation of elecrolyte to be obstructed; Anode passivation is serious, constitutes anodic noble metal seriously corroded, has a strong impact on carrying out smoothly of refining.
2. because mixture rapid oxidation of catalyst metal particle when physical purification, cause its poorly conductive in electrolytic process, the metal ion exchanged obstacle has a strong impact on electrolysis speed, and equipment, power consumption, consumption acid are with high costs.Simultaneously, the side reaction in the electrolytic process (evolving hydrogen reaction etc.) is serious, the severe exacerbation workshop condition.
3. traditional " re-electrolysis " process method metal recovery rate is low, and utilization rate of electrical is low, staff labor intensity is big, time-consuming.
Summary of the invention
The purpose of this invention is to provide thin catalyst metal recovery method behind a kind of powder diamond synthesis refining, can high-level efficiency, the thin catalyst metal of completion of high-recovery reclaims, and reduces staff's labour intensity, has the advantage of safety and environmental protection simultaneously.
The present invention adopts following technical proposals:
Thin catalyst metal recovery method may further comprise the steps behind a kind of powder diamond synthesis refining
A: the mixture that will contain catalyst metal is packed into behind the filter cloth bag, puts into electrolyzer;
B: in electrolyzer, inject hydrochloric acid;
C: utilize circulation of elecrolyte heating acid solution through pipeline;
D: acid solution suction electrolyzer is carried out electrolytic recovery.
In the said B step, according to the acid material than in electrolyzer, injecting hydrochloric acid to the ratio between the 4:1 at 2:1.
In the said B step, in electrolyzer, inject hydrochloric acid than the ratio of 3:1 according to the acid material.
Described hydrochloric acid mass concentration is constant to be 10%-15%.
In the said C step, acid liquor temperature is remained between 30 ° to 50 ° through heating.
In the said C step, make acid liquor temperature remain on 40 ℃ through heating.
In the said D step, reacted 3-4 days, treat acid solution pH value be not less than 1 and be not more than 2 after, again acid solution suction electrolyzer is carried out electrolytic recovery.
Described filter cloth bag is 200 order filter cloth bags.
Described filter cloth bag is the dacron terylene pocket.
The present invention under the temperature soaks mixture in constant in middle concentration acid solution; Make the metal in the mixture become the dissociated ion attitude through chemical reaction; And utilize quick electrolysis method enriched in metals ion on negative plate, to reach the purpose that reclaims catalyst metal, avoid occurring the serious and noble metal seriously corroded phenomenon of anode passivation; Can high-level efficiency, the thin catalyst metal of completion of high-recovery reclaims; Reduce staff's labour intensity, avoid simultaneously side reaction takes place in the electrolytic process, have the advantage of safety and environmental protection.
Description of drawings
Fig. 1 is a schema of the present invention.
Embodiment
As shown in Figure 1, the present invention includes following steps:
A: the mixture that will contain catalyst metal is packed into behind the filter cloth bag, puts into electrolyzer;
B: in electrolyzer, inject hydrochloric acid;
C: utilize circulation of elecrolyte heating acid solution through pipeline;
D: acid solution suction electrolyzer is carried out electrolytic recovery.
The present invention under the temperature soaks mixture in constant in middle concentration acid solution, make the metal in the mixture be transformed into the dissociated ion attitude from chemical combination states of matter, elemental through chemical reaction, and this acid solution is used for electrolytic solution pH regulator liquid.And then pass through quick electrolysis method enriched in metals ion on negative plate, to reach the purpose that reclaims catalyst metal.
For reaching better recovering effect, in the said A step, the filter cloth bag is 200 purpose dacron terylene pockets; In the B step, be the hydrochloric acid of 10%-15% than ratio implantation quality constant concentration in electrolyzer of 3:1 according to the acid material; In the C step, make acid liquor temperature remain on 40 ℃ through heating; In the D step, reacted 3-4 days, treat acid solution pH value be not less than 1 and be not more than 2 after, again acid solution suction electrolyzer is carried out electrolytic recovery.
Embodiment 1
1. the mixture that contains catalyst metal with 300Kg is divided in 60 dacron terylene pockets, puts into electrolyzer after oral area is tightened;
2. implantation quality concentration is 10% hydrochloric acid 600Kg in electrolyzer, and concentration of hydrochloric acid keeps constant through under meter;
3. utilize circulation of elecrolyte heating acid solution through pipeline, make acid liquor temperature remain on 30 ℃;
4. reaction was carried out 4 days, and recording the pH value is 1.12, and acid solution suction electrolyzer is carried out electrolytic recovery.
Handle the metal content in the dacron terylene pocket of back through physico-chemical analysis, record metal content and have only 9% of virgin metal content, prove that 91% metal is dissolved in the acid solution.
Embodiment 2
1. the mixture that contains catalyst metal with 300Kg is divided in 60 dacron terylene pockets, puts into electrolyzer after oral area is tightened;
2. implantation quality concentration is 10% hydrochloric acid 900Kg in electrolyzer, and concentration of hydrochloric acid keeps constant through under meter;
3. utilize circulation of elecrolyte heating acid solution through pipeline, make acid liquor temperature remain on 40 ℃;
4. reaction was carried out 4 days, and recording the pH value is 1.12, and acid solution suction electrolyzer is carried out electrolytic recovery.
Handle the metal content in the dacron terylene pocket of back through physico-chemical analysis, record metal content and have only 8% of virgin metal content, prove that 92% metal is dissolved in the acid solution.
Embodiment 3
1. the mixture that contains catalyst metal with 400Kg is divided in 60 dacron terylene pockets, puts into electrolyzer after oral area is tightened;
2. implantation quality concentration is 15% hydrochloric acid 1600Kg in electrolyzer, and concentration of hydrochloric acid keeps constant through under meter;
3. utilize circulation of elecrolyte heating acid solution through pipeline, make acid liquor temperature remain on 50 ℃;
4. reaction was carried out 3 days, and recording the pH value is 1.12, and acid solution suction electrolyzer is carried out electrolytic recovery.
Handle the metal content in the dacron terylene pocket of back through physico-chemical analysis, record metal content and have only 9% of virgin metal content, prove that 91% metal is dissolved in the acid solution.
Claims (9)
1. thin catalyst metal recovery method behind the powder diamond synthesis refining is characterized in that: may further comprise the steps
A: the mixture that will contain catalyst metal is packed into behind the filter cloth bag, puts into electrolyzer;
B: in electrolyzer, inject hydrochloric acid;
C: utilize circulation of elecrolyte heating acid solution through pipeline;
D: acid solution suction electrolyzer is carried out electrolytic recovery.
2. thin catalyst metal recovery method behind the powder diamond synthesis refining according to claim 1 is characterized in that: in the said B step, according to the acid material than in electrolyzer, injecting hydrochloric acid to the ratio between the 4:1 at 2:1.
3. thin catalyst metal recovery method is characterized in that: in the said B step, in electrolyzer, inject hydrochloric acid according to the acid material than the ratio of 3:1 behind the powder diamond synthesis refining according to claim 2.
4. thin catalyst metal recovery method behind the powder diamond synthesis refining according to claim 3 is characterized in that: the constant 10%-15% of being of described hydrochloric acid mass concentration.
5. according to thin catalyst metal recovery method behind claim 1,2, the 3 or 4 described powder diamond synthesis refinings, it is characterized in that: in the said C step, acid liquor temperature is remained between 30 ° to 50 ° through heating.
6. thin catalyst metal recovery method is characterized in that: in the said C step, make acid liquor temperature remain on 40 ℃ through heating behind the powder diamond synthesis refining according to claim 5.
7. thin catalyst metal recovery method behind the powder diamond synthesis refining according to claim 6 is characterized in that: in the said D step, reacted 3-4 days, treat acid solution pH value be not less than 1 and be not more than 2 after, again acid solution suction electrolyzer is carried out electrolytic recovery.
8. thin catalyst metal recovery method behind the powder diamond synthesis refining according to claim 7, it is characterized in that: described filter cloth bag is 200 order filter cloth bags.
9. thin catalyst metal recovery method behind the powder diamond synthesis refining according to claim 8, it is characterized in that: described filter cloth bag is the dacron terylene pocket.
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| CN201210265805XA CN102776526A (en) | 2012-07-30 | 2012-07-30 | Recovery method of fine catalyst metal obtained after electrolysis and purification of synthetic diamond powder |
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| CN201210265805XA CN102776526A (en) | 2012-07-30 | 2012-07-30 | Recovery method of fine catalyst metal obtained after electrolysis and purification of synthetic diamond powder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103361672A (en) * | 2013-07-04 | 2013-10-23 | 河南金六方超硬材料有限公司 | Recovery method for electrolytically extracting metal from catalyst after synthesizing diamonds from powder |
| CN108277500A (en) * | 2018-04-14 | 2018-07-13 | 新郑市新材料专业孵化器服务中心 | A kind of diamond electrorefining device |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1802458A (en) * | 2003-05-30 | 2006-07-12 | 约瑟夫·利奥波德·斯坦凯维奇 | A process for the recovery of synthetic diamonds |
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- 2012-07-30 CN CN201210265805XA patent/CN102776526A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1802458A (en) * | 2003-05-30 | 2006-07-12 | 约瑟夫·利奥波德·斯坦凯维奇 | A process for the recovery of synthetic diamonds |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103361672A (en) * | 2013-07-04 | 2013-10-23 | 河南金六方超硬材料有限公司 | Recovery method for electrolytically extracting metal from catalyst after synthesizing diamonds from powder |
| CN108277500A (en) * | 2018-04-14 | 2018-07-13 | 新郑市新材料专业孵化器服务中心 | A kind of diamond electrorefining device |
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Address after: Fangcheng County of Nanyang City, Henan province 473264 box 101 Applicant after: ZHONGNAN DIAMOND CO., LTD. Address before: Fangcheng County of Nanyang City, Henan province 473264 box 101 Applicant before: Zhongnan Diamond Co., Ltd. |
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Free format text: CORRECT: APPLICANT; FROM: ZHONGNAN DIAMOND CO., LTD. TO: ZHONGNAN DIOMAND CO., LTD. |
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Application publication date: 20121114 |