CN102517453A - Method for recycling platinum from waste platinum crucibles - Google Patents
Method for recycling platinum from waste platinum crucibles Download PDFInfo
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- CN102517453A CN102517453A CN201110415426XA CN201110415426A CN102517453A CN 102517453 A CN102517453 A CN 102517453A CN 201110415426X A CN201110415426X A CN 201110415426XA CN 201110415426 A CN201110415426 A CN 201110415426A CN 102517453 A CN102517453 A CN 102517453A
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- ammonium chloride
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention relates to a method for recycling platinum from waste platinum crucibles. The method comprises 5 steps that: waste platinum crucibles are dissolved by using aqua regia; lead is removed by using a lead removing agent; platinum is precipitated by using ammonium chloride; platinum is refined; and platinum is calcined. According to the invention, waste platinum crucibles containing impurities such as lead, niobium, silicon and sodium are recycled as a platinum raw material; the raw material is dissolved by using aqua regia; concentrated sulfuric acid or water-soluble sulfate is added to the material, such that lead is pre-removed, and the frequency of repeated platinum precipitation by using ammonium chloride is reduced. Therefore, a platinum refining period is shortened, an agent dosage is reduced, a purification cost is reduced, and the purity of platinum sponge can be improved.
Description
Technical field
The present invention is a kind of method that from useless platinum crucible, reclaims platinum, belongs to the metal recovery technical field, and this method is from the useless platinum crucible of impurity such as leaded, niobium, silicon, sodium, to reclaim spongy platinum.
Background technology
In mid-term the 1950's, famous vitrifying scholar and inventor S.D.Stookey at first make glass-ceramic, and to the seventies in 20th century, the research of glass-ceramic has obtained and further developed, and are described as the new ceramic material of 21 century at present by the expert.Glass-ceramic is a kind of matrix material that had not only contained crystalline phase but also contained glassy phase that has through control that the crystallization of proper composition mother glass obtains; Have the advantage of glass and pottery concurrently, often be superior to metal and organic polymer material aspect calorifics, chemistry, biology, optics and the electric property.
Because glass-ceramic has good composition and microstructure controllability, has bigger potentiality in the application aspect the high energy storage capacitor than sintered iron electric material.To be applied to the Nb of high energy storage capacitor
2O
5-PbO-Na
2O-SiO
2The quaternary system glass ceramic material is an example; Be with behind an amount of above-mentioned various oxide compound thorough mixing; Under 1400～1500 ℃ of hot conditionss, in platinum crucible, metal oxide powder is smelted into liquid; Cooling forms glassy phase fast then, crystallization and growth process through controlling ceramic phase effectively in annealing process subsequently, the fine and close glass ceramic material of final formation.The raising of the low disruptive strength that defective causes of higher dielectric constant that ceramic phase had in the glass ceramic material and material makes the energy storage density of material obtain significant raising.
Yet, because the existence of low melting material PbO (fusing point is 886 ℃) makes platinum crucible at Nb
2O
5-PbO-Na
2O-SiO
2Corrosion-vulnerable in the melting process of quaternary system glass ceramic material, and then influence the use of platinum crucible.
As everyone knows, the price of metal platinum is very expensive, and also very limited in the resource of whole occurring in nature platinum, and the high purity of therefore pursuing platinum is that platinum crucible realizes using long lifetime and the feasible way that reduces preparation cost in the glass ceramic material preparation with regeneration.
The method of refining of platinum has multiple, sums up to get up to have: chlorination carbonyl platinum method, fused salt electrolysis process, zone melting method, aqua regia dissolution-ammonium chloride repeated precipitation process, reduction of dissolved-ammonium chloride repeated precipitation process, oxidizing water solution (sodium bromate oxidation, chlorine oxidation, dioxygen oxidation, H
2O
2Oxidation, HNO
3Oxidation), carrier hydrolysis method, carrier hydrolysis-ion exchange method, alkali are dissolved-reduction method, dichloro two ammino platinum (II) methods, dinitroso two ammino platinum (II) methods, reduction-dissolution method, extracting refining method etc.Chlorination carbonyl platinum method, fused salt electrolysis process are owing to complex technical process, complex operation, and large-scale production is restricted, and in industry, is not applied.Zone melting method is mainly used in produces ultra-pure platinum, in large-scale industrial production, also seldom uses.In industry, using at present maximum is aqua regia dissolution-ammonium chloride repeated precipitation process, sodium bromate hydrolysis method, oxidation carrier hydrolysis method etc., and wherein hydrolysis method is compared with aqua regia dissolution-ammonium chloride repeated precipitation process, operate comparatively loaded down with trivial details, the most commonly used with the latter.And the preparation glass ceramic material use platinum crucible, owing to receive the erosion of low melting material, makes impurity such as leaded in the useless platinum crucible, niobium, silicon, sodium, for recovery platinum has brought difficulty.
Summary of the invention
The present invention designs a kind of method that from useless platinum crucible, reclaims platinum that provides to the problem that exists in the above-mentioned prior art just; Its objective is the recovery of platinum in the useless platinum crucible of impurity such as solving leaded, niobium, silicon, sodium; Simple, the processing ease of this method requirement equipment, the recovery of platinum is high.
The objective of the invention is to realize through following technical scheme:
This kind reclaims the method for platinum from useless platinum crucible, it is characterized in that: steps of the method are:
(1) the useless platinum crucible of aqua regia dissolution
The platinum crucible that will give up places beaker, adds aqua regia dissolution, and chloroazotic acid is the mixed solution of hydrochloric acid and salt made from earth containing a comparatively high percentage of sodium chloride, and both volume ratios are: V
Hydrochloric acid: V
Nitric acid=3: 1, treat platinum waste material dissolving fully after, add hydrochloric acid and catch up with nitre to there not being tobacco, add the deionized water dilution after, the heating dissolved salt;
(2) deleading agent deleading
With the resulting platinum solution of step (1) thin up to platiniferous 40～80g/L; Under whipped state, add deleading agent, continue to stir and leave standstill, filter with B above 12h; And use the washed with de-ionized water funnel, obtain the filter residue of impurity such as insolubles and lead sulfate;
(3) the heavy platinum of ammonium chloride
The resulting filter residue thin up of step (2) to platiniferous 35～70g/L, after the heated and boiled, is added the heavy platinum of capacity 25% ammonium chloride solution, leaves standstill, during stirred solution frequently, treat that solution is cooled to the room temperature after-filtration;
(4) refining
Step (3) is filtered the operation that the yellow ammonium chloroplatinate that obtains repeats above-mentioned steps (1)～(3);
(5) calcining
The ammonium chloroplatinate that step (4) is obtained after refining is put into crucible, in retort furnace, slowly heats up, and removes moisture earlier; At 350～400 ℃ of constant temperature, ammonium salt is decomposed then, treat not emit in the stove white cigarette; Elevated temperature to 900 ℃ calcining 1h, spongy platinum is taken out in the cooling back, treats sampling analysis qualified back bottling.
The preferably vitriol oil, sodium sulfate, vitriolate of tartar of employed deleading agent in the above-mentioned steps (2).
Description of drawings
Fig. 1 is the process flow sheet of the inventive method
Embodiment
Below will combine accompanying drawing and embodiment that technical scheme of the present invention is done to detail further:
Embodiment 1
The step of the inventive method is:
V nitric acid=3: 1) and place heating for dissolving on the electric furnace (1) the useless platinum crucible of 105g is placed the 4000mL beaker, add excessive chloroazotic acid (V hydrochloric acid:.After treating the dissolving fully of platinum waste material, continue heating, concentrate volume, add hydrochloric acid and catch up with nitre to there not being tobacco to 500mL.After adding the deionized water dilution, the heating dissolved salt.
(2) with (1) gained platiniferous solution thin up to 2000mL, under whipped state, add the 10mL vitriol oil, continue to stir and hold over night.Filter with B, and use the washed with de-ionized water funnel.Filter residue is impurity such as insolubles and lead sulfate.
(3) (2) gained is filtrated thin up to 2500mL, after the heated and boiled, add the heavy platinum of 950mL25% ammonium chloride solution.Leave standstill, during stirred solution frequently, treat solution room temperature cooled and filtered.
(4) return filter resulting yellow ammonium chloroplatinate in (3) to the 4000mL beaker, add aqua regia dissolution after, repeat the operation of (1)～(3) step.
(5) put into crucible after (4) refining back gained ammonium chloroplatinate sedimentation and filtration is drained, in retort furnace, slowly heat up, remove moisture earlier,, ammonium salt is decomposed then 350～400 ℃ of constant temperature for some time.Treat not emit in the stove white cigarette, elevated temperature, and temperature control after the cooling, gets spongy platinum 104.01g, productive rate 99.06%, sampling analysis, platinum content ≮ 99.99% at 900 ℃ of calcining 1h.
Embodiment 2
The process of the inventive method is:
The useless platinum crucible of 105g is placed the 4000mL beaker, change the 10mL vitriol oil among the embodiment 1 into the 25g SODIUM SULPHATE ANHYDROUS 99PCT, all the other conditions are all constant, get spongy platinum 103.91g, productive rate 98.96%, sampling analysis, platinum content ≮ 99.99%.
Embodiment 3
The process of the inventive method is:
The useless platinum crucible of 105g is placed the 4000mL beaker, change the 10mL vitriol oil among the embodiment 1 into the 31g vitriolate of tartar, all the other conditions are all constant, get spongy platinum 72.15g, productive rate 68.71%, sampling analysis, platinum content ≮ 99.99%.
Compared with prior art; Useless platinum crucible to impurity such as leaded, niobium, silicon, sodium is the platinum recovery of raw material, behind aqua regia dissolution, adopts the adding vitriol oil or the preparatory deleading of water soluble sulfate to reduce the ammonium chloride number of times of heavy platinum repeatedly; Promptly can shorten the refining cycle of platinum; Reduce reagent dosage, reduce the purifying cost, can improve the purity of spongy platinum again.
Claims (2)
1. method that from useless platinum crucible, reclaims platinum is characterized in that: steps of the method are:
(1) the useless platinum crucible of aqua regia dissolution
The platinum crucible that will give up places beaker, adds aqua regia dissolution, and chloroazotic acid is the mixed solution of hydrochloric acid and salt made from earth containing a comparatively high percentage of sodium chloride, and both volume ratios are: V
Hydrochloric acid: V
Nitric acid=3: 1, treat platinum waste material dissolving fully after, add hydrochloric acid and catch up with nitre to there not being tobacco, add the deionized water dilution after, the heating dissolved salt;
(2) deleading agent deleading
With the resulting platinum solution of step (1) thin up to platiniferous 40～80g/L; Under whipped state, add deleading agent, continue to stir and leave standstill, filter with B above 12h; And use the washed with de-ionized water funnel, obtain the filter residue of impurity such as insolubles and lead sulfate;
(3) the heavy platinum of ammonium chloride
The resulting filter residue thin up of step (2) to platiniferous 35～70g/L, after the heated and boiled, is added the heavy platinum of capacity 25% ammonium chloride solution, leaves standstill, during stirred solution frequently, treat that solution is cooled to the room temperature after-filtration;
(4) refining
Step (3) is filtered operation that the yellow ammonium chloroplatinate obtain repeats above-mentioned steps (1)～(3) once;
(5) calcining
The ammonium chloroplatinate that step (4) is obtained after refining is put into crucible, in retort furnace, slowly heats up, and removes moisture earlier; At 350～400 ℃ of constant temperature, ammonium salt is decomposed then, treat not emit in the stove white cigarette; Elevated temperature to 900 ℃ calcining 1h, spongy platinum is taken out in the cooling back, treats sampling analysis qualified back bottling.
2. the method that from useless platinum crucible, reclaims platinum according to claim 1, it is characterized in that: employed deleading agent is water dissolvable vitriol such as the vitriol oil, sodium sulfate, vitriolate of tartar in the step (2).
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| CN201110415426XA CN102517453A (en) | 2011-12-09 | 2011-12-09 | Method for recycling platinum from waste platinum crucibles |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104889413A (en) * | 2015-05-13 | 2015-09-09 | 贵研铂业股份有限公司 | Method for preparing high purity platinum powder for electronic component |
| CN107641721A (en) * | 2017-09-29 | 2018-01-30 | 云南驰宏锌锗股份有限公司 | A kind of method of thick gold purification |
| CN109387450A (en) * | 2017-08-08 | 2019-02-26 | 上海老凤祥首饰研究所有限公司 | Platinum content measuring method in a kind of platinum-nickel alloys ornaments |
| CN109530365A (en) * | 2018-11-26 | 2019-03-29 | 中国电子科技集团公司第十研究所 | Molecular beam epitaxy boron nitride crucible cleaning method |
| CN111455184A (en) * | 2020-06-02 | 2020-07-28 | 河南省岩石矿物测试中心 | Method for recovering platinum in laboratory waste noble metal material by potassium borohydride-ammonium chloride reduction |
| CN111676371A (en) * | 2020-04-27 | 2020-09-18 | 励福(江门)环保科技股份有限公司 | Method for separating and purifying platinum from tungsten crucible |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104889413A (en) * | 2015-05-13 | 2015-09-09 | 贵研铂业股份有限公司 | Method for preparing high purity platinum powder for electronic component |
| CN109387450A (en) * | 2017-08-08 | 2019-02-26 | 上海老凤祥首饰研究所有限公司 | Platinum content measuring method in a kind of platinum-nickel alloys ornaments |
| CN109387450B (en) * | 2017-08-08 | 2021-02-19 | 上海老凤祥首饰研究所有限公司 | Method for measuring platinum content in platinum-palladium alloy ornament |
| CN107641721A (en) * | 2017-09-29 | 2018-01-30 | 云南驰宏锌锗股份有限公司 | A kind of method of thick gold purification |
| CN107641721B (en) * | 2017-09-29 | 2019-10-18 | 云南驰宏锌锗股份有限公司 | A kind of method of thick gold purification |
| CN109530365A (en) * | 2018-11-26 | 2019-03-29 | 中国电子科技集团公司第十研究所 | Molecular beam epitaxy boron nitride crucible cleaning method |
| CN111676371A (en) * | 2020-04-27 | 2020-09-18 | 励福(江门)环保科技股份有限公司 | Method for separating and purifying platinum from tungsten crucible |
| CN111455184A (en) * | 2020-06-02 | 2020-07-28 | 河南省岩石矿物测试中心 | Method for recovering platinum in laboratory waste noble metal material by potassium borohydride-ammonium chloride reduction |
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Application publication date: 20120627 |