CN103555937B - Two sections of sedimentations refine platinum technique - Google Patents
Two sections of sedimentations refine platinum technique Download PDFInfo
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- CN103555937B CN103555937B CN201310545925.XA CN201310545925A CN103555937B CN 103555937 B CN103555937 B CN 103555937B CN 201310545925 A CN201310545925 A CN 201310545925A CN 103555937 B CN103555937 B CN 103555937B
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Abstract
The invention discloses two sections of sedimentations and refine platinum technique, it comprises: (1), hydrazine hydrate reduction: add water platinum concentrate pulp, is warming up to 50 ± 5 DEG C, adds hydrazine hydrate and ammonium chloroplatinate is reduced into platina; (2), aqua regia dissolution: the platina leached is put into glass cylinder and to be added water pulp, adds aqua regia dissolution until platinum is molten to the greatest extent; (3), one section of non-oxidation sinks platinum-boil molten palladium: control solution platiniferous 50g/l, be warmed up to 60 DEG C, adds NH4Cl and sinks platinum, after reaction terminates, and heated and boiled, cooled and filtered, washing; (4), two sections of heavy platinum palladiums of oxidation: one section of heavy platinum filtrate is warmed up to 60 DEG C, adds the ammonium chloride of 10:1 and sodium chlorate and sink platinum palladium, after reaction terminates, cold filtration, washing; (5), the molten palladium of ammonification: will filter after one section of platinum salt obtaining and two sections of platinum palladium salt use pure water pulp respectively, (6), calcining: the platinum salt putting into porcelain crucible, at retort furnace heating and calcining, takes out washing and drying after Slow cooling.
Description
Technical field
The present invention relates to refining platinum technique, particularly relate to two sections of sedimentations and refine platinum technique.
Background technology
The method the most general on metallurgy of platreating has: 1, ammonium chloride repeated precipitation process.2, sodium bromate hydrolysis method.
Traditional chloride precipitation method, in the process of deposition platinum salt, first needs first pass into chlorine or add oxygenant, makes platinum palladium keep high-valence state, common deposition is got off, separation difficulty, and secondly deposition slag needs to boil to cool palladium removing rapidly, high to equipment requirements, energy consumption is large, and operation easier is large.
Sodium bromate hydrolysis method utilizes sodium bromate as oxygenant, the platinum ion in solution is made to keep high-valence state, control suitable Ph value, rhodium in solution, iridium and various expensive, base metal are hydrolyzed as early as possible and generate stable oxyhydroxide removing, platiniferous solution is purified, but because of some palladium content carried in platinum raw material high, in liquid making process, palladium and platinum enter solution simultaneously, during hydrolysis operation, because platinum palladium character is similar, be difficult to removing.
Platinum is carried according to ammonium chloride repeated precipitation process is refining, guarantee that system is in strong oxidizing atmosphere state owing to needing constantly to be equipped with strong oxidizer sodium chlorate in process, thus acquisition high deposition rate, there is coprecipitated situation in the inevitable like this platinum palladium that causes, cool more difficult control rapidly simultaneously, cause how many times of no matter repeatedly purifying, in the refining product spongy platinum obtained, always there is the problem that palladium exceeds standard, the main grade of product spongy platinum does not reach more than 99.9%, and selling price is on the low side.
Summary of the invention
The technical problem to be solved in the present invention is: for containing palladium high carry platinum raw material, in existing refining platinum technique, chloride precipitation method platinum palladium separation difficulty, high to equipment requirements, and energy consumption is large, and operation easier is large; There is palladium and exceed standard in sodium bromate hydrolysis method, direct yield is low.There is provided two sections of sedimentations that a kind of technique is simple, easy to operate, metal is combined and the rate of recovery is high to refine platinum technique for this reason.
Technical scheme of the present invention is: two sections of sedimentations refine platinum technique, and it comprises the following steps: (1), hydrazine hydrate reduction: add water platinum concentrate pulp, is warming up to 50 ± 5 DEG C, adds hydrazine hydrate and ammonium chloroplatinate is reduced into platina, and reaction terminates rear cold filtration;
(2), aqua regia dissolution: the platina leached is put into 80l ceramic whiteware cylinder and to be added water pulp, adds aqua regia dissolution, until platinum is molten to the greatest extent, leaves standstill and filters, washing, and filtrate, washing lotion merge catches up with nitre;
(3), one section of non-oxidation sinks platinum-boil molten palladium: control solution platiniferous 50g/l, be warmed up to 60 DEG C, add NH4Cl and sink platinum, now a large amount of platinum and a small amount of palladium can deposit with the form of ammonium chloroplatinate and ammonium palladic chloride and obtain bisque solids, after reaction terminates, heated and boiled, cooled and filtered, washing;
(4), two sections of heavy platinum palladiums of oxidation: one section of heavy platinum filtrate is warmed up to 60 DEG C, adds the ammonium chloride of 10:1 and sodium chlorate and sink platinum palladium, after reaction terminates, cold filtration, washing;
(5), the molten palladium of ammonification: by filtering after one section of platinum salt obtaining and two sections of platinum palladium salt use pure water pulp respectively, adding ammonia solvent palladium, and being merged by platinum slags after two sections of washings, repeat 1-3 process repeatedly after three times, the platinum salt obtained loads crucible and prepares calcining;
(6), calcine: pure platinum salt is put into porcelain crucible, and heating and calcining in retort furnace, takes out washing and drying after Slow cooling.
The invention has the beneficial effects as follows that the main grade of the spongy platinum obtained reaches 99.9%, technique is simple, easy to operate.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Embodiment 1:(1), hydrazine hydrate reduction: add water platinum concentrate pulp, is warming up to 45 DEG C, adds hydrazine hydrate and ammonium chloroplatinate is reduced into platina, reaction terminate rear cold filtration;
(2), aqua regia dissolution: the platina leached is put into 80l ceramic whiteware cylinder and to be added water pulp, adds aqua regia dissolution, if reaction is no longer carried out, sucking-off solution is poured new chloroazotic acid again into and continued to dissolve, until platinum is molten to the greatest extent, leaves standstill and filters, washing, and filtrate, washing lotion merge catches up with nitre;
(3), one section of non-oxidation sinks platinum-boil molten palladium: control solution platiniferous 50g/l, be warmed up to 60 DEG C, add NH4Cl and sink platinum, now a large amount of platinum and a small amount of palladium can deposit with the form of ammonium chloroplatinate and ammonium palladic chloride and obtain bisque solids, after reaction terminates, heated and boiled, cooled and filtered, washing;
(4), two sections of heavy platinum palladiums of oxidation: one section of heavy platinum filtrate is warmed up to 60 DEG C, add the ammonium chloride of 10:1 and sodium chlorate and sink platinum palladium, now a small amount of platinum and a large amount of palladiums can deposit with the form of ammonium chloroplatinate and ammonium palladic chloride and obtain bolarious solids, after reaction terminates, cold filtration, washing;
(5), the molten palladium of ammonification: after pure water pulp used respectively by the one section of platinum salt obtain filtration and two sections of platinum palladium salt, add ammonia solvent palladium, and by after after two sections of washings, platinum slags merge, successively repeating step (1), (2), after (3) three times, the platinum salt obtained loads porcelain crucible and prepares calcining;
(6), calcining: the platinum salt putting into porcelain crucible is at retort furnace in 200 DEG C of constant temperature 2h, and 450 DEG C of constant temperature 1h, 900 DEG C of constant temperature 2h, take out washing and drying after Slow cooling.
Embodiment 2:(1), hydrazine hydrate reduction: add water platinum concentrate pulp, is warming up to 55 DEG C, adds hydrazine hydrate and ammonium chloroplatinate is reduced into platina, reaction terminate rear cold filtration;
(2), aqua regia dissolution: the platina leached is put into glass cylinder and to be added water pulp, adds aqua regia dissolution, if reaction is no longer carried out, sucking-off solution is poured new chloroazotic acid again into and continued to dissolve, until platinum is molten to the greatest extent, leaves standstill and filters, washing, and filtrate, washing lotion merge catches up with nitre;
(3), one section of non-oxidation sinks platinum-boil molten palladium: control solution platiniferous 50g/l, be warmed up to 60 DEG C, add NH4Cl and sink platinum, now a large amount of platinum and a small amount of palladium can deposit with the form of ammonium chloroplatinate and ammonium palladic chloride and obtain bisque solids, after reaction terminates, heated and boiled, cooled and filtered, washing;
(4), two sections of heavy platinum palladiums of oxidation: one section of heavy platinum filtrate is warmed up to 60 DEG C, add the ammonium chloride of 10:1 and sodium chlorate and sink platinum palladium, now a small amount of platinum and a large amount of palladiums can deposit with the form of ammonium chloroplatinate and ammonium palladic chloride and obtain bolarious solids, after reaction terminates, cold filtration, washing;
(5), the molten palladium of ammonification: after pure water pulp used respectively by the one section of platinum salt obtain filtration and two sections of platinum palladium salt, add ammonia solvent palladium, and by after after two sections of washings, platinum slags merge, successively repeating step (1), (2), after (3) three times, the platinum salt obtained loads porcelain crucible and prepares calcining;
(6), calcining: the platinum salt putting into porcelain crucible is at retort furnace in 150 DEG C of constant temperature 2.5h, and 400 DEG C of constant temperature 1.5h, 850 DEG C of constant temperature 2.5h, take out washing and drying after Slow cooling.
The heavy platinum palladium of two sections of oxidations of the present invention and general technology difference are segmented deposition, one section does not add any oxygenant, oxidizing atmosphere in solution is more weak, the palladium of the overwhelming majority keeps lower valency, directly with ammonium chloride deposits, the platinum slag platiniferous obtained one section of deposition is high only containing a small amount of palladium, and most of palladium stays in the solution, has well been separated platinum palladium; Two sections of depositions add strong oxidizer-sodium chlorate, and the oxidizing atmosphere improving solution makes the palladium in solution and residual a small amount of platinum all be in high-valence state, now, adds ammonium chloride deposits, guarantees that the platinum palladium in solution deposits completely.Advantage: segmented deposition, one section of platinum purity salt obtained is high, is conducive to next step separating-purifying; Two sections deposit the direct yield utilizing and improve platinum.
The molten palladium of ammonification and general technology difference in step (5): the feature high according to palladium in some raw material, increases this operation, removes the palladium in one section of platinum salt and two sections of platinum palladium salt.Advantage: 1, after the ammonification of one section of platinum salt, purity is higher, is conducive to next step and purifies; After the ammonification of two sections of platinum palladium salt, ammonification slag is platinum salt and one section of platinum salt merges, and can improve the direct yield of platinum; 2, in ammonification liquid, palladium content is high, can direct Recover palladium.
Above in conjunction with specific embodiments to invention has been exemplary description; obvious specific implementation of the present invention is not subject to the restrictions described above; as long as have employed the improvement of the various unsubstantialities that method of the present invention is conceived and technical scheme is carried out; or design of the present invention and technical scheme directly applied to other occasion, all within protection scope of the present invention without to improve.
Claims (1)
1. two sections of sedimentations refine platinum technique, it is characterized in that it comprises the following steps: (1), hydrazine hydrate reduction: add water platinum concentrate pulp, is warming up to 50 ± 5 DEG C, adds hydrazine hydrate and ammonium chloroplatinate is reduced into platina, and reaction terminates rear cold filtration;
(2), aqua regia dissolution: the platina leached is put into 80l ceramic whiteware cylinder and to be added water pulp, adds aqua regia dissolution until platinum is molten to the greatest extent, leaves standstill and filter, washing, and filtrate, washing lotion merge catches up with nitre;
(3), one section of non-oxidation sinks platinum-boil molten palladium: control solution platiniferous 50g/l, be warmed up to 60 DEG C, add NH4Cl and sink platinum, now a large amount of platinum and a small amount of palladium can deposit with the form of ammonium chloroplatinate and ammonium palladic chloride and obtain bisque solids, after reaction terminates, heated and boiled, cooled and filtered, washing;
(4), two sections of heavy platinum palladiums of oxidation: one section of heavy platinum filtrate is warmed up to 60 DEG C, adds ammonium chloride that mass ratio is 10:1 and sodium chlorate and sink platinum palladium, after reaction terminates, cold filtration, washing;
(5), the molten palladium of ammonification: after pure water pulp used respectively by the one section of platinum salt obtain filtration and two sections of platinum palladium salt, add ammonia solvent palladium, and by after after two sections of washings, platinum slags merge, successively repeating step (1), (2), after (3) three times, the platinum salt obtained loads porcelain crucible and prepares calcining;
(6), calcining: the platinum salt putting into porcelain crucible at retort furnace heating and calcining, in 150 DEG C of constant temperature 2.5h, 400 DEG C of constant temperature 1.5h, 850 DEG C of constant temperature 2.5h, or in 200 DEG C of constant temperature 2h, 450 DEG C of constant temperature 1h, 900 DEG C of constant temperature 2h, take out washing and drying after Slow cooling.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105177305B (en) * | 2014-11-01 | 2019-07-19 | 陕西华特新材料股份有限公司 | A kind of platinum wet-process purification method |
| CN106148724B (en) * | 2016-08-29 | 2018-04-10 | 金川集团股份有限公司 | A kind of platinum refinery practice |
| CN108950234B (en) * | 2018-08-15 | 2021-01-26 | 大冶有色金属有限责任公司 | Method for separating platinum and palladium from platinum-palladium mixture |
| CN110964920A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Method for recovering refined platinum from crude ammonium chloroplatinate |
| CN110964922A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Method for recovering refined platinum from crude ammonium chloroplatinate |
| CN110964919A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Preparation method of spongy platinum |
| CN114951688A (en) * | 2022-04-25 | 2022-08-30 | 金川集团股份有限公司 | Preparation method of high-purity platinum powder |
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