CN104532011A - Method for separating and purifying platinum metals through solvent extraction - Google Patents

Method for separating and purifying platinum metals through solvent extraction Download PDF

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Publication number
CN104532011A
CN104532011A CN201410749722.7A CN201410749722A CN104532011A CN 104532011 A CN104532011 A CN 104532011A CN 201410749722 A CN201410749722 A CN 201410749722A CN 104532011 A CN104532011 A CN 104532011A
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China
Prior art keywords
platinum
palladium
rhodium
iridium
solvent extraction
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CN201410749722.7A
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Chinese (zh)
Inventor
马玉天
潘从明
冯岩
郭晓辉
李明
陈云峰
刘林
孙渊君
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Jinchuan Group Co Ltd
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Jinchuan Group Co Ltd
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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 provides a method for separating and purifying platinum metals through solvent extraction, relates to a metal separating and purifying method, and particularly relates to a method for separating platinum, palladium, rhodium and iridium from a solution, slag or secondary resource containing platinum metals. The method is characterized in that the purifying process comprises the following steps: (1) chloridizing and dissolving materials containing platinum metals; (2) adding ammonium oxalate to perform copper-nickel precipitation separation; (3) adding organic reducing agent vitamin C to perform platinum-palladium precipitation reaction; (4) performing aqua regia dissolution and denitration on the platinum-palladium-containing precipitation slag, and feeding into a diisoamyl thioether platinum-palladium extraction separation procedure; and (5) adding manganese dioxide and introducing chlorine gas into the rhodium-iridium-containing filtrate, reacting, and feeding into a tributyl phosphate rhodium-iridium extraction separation procedure. According to the method provided by the invention, the platinum-palladium and rhodium-iridium separation rates are high, and further platinum-palladium separation and rhodium-iridium separation can be realized easily through subsequent extraction; after conventional refining, platinum black and palladium black of which the purities are above 99.99% can be produced, and spongy platinum and spongy palladium products meeting the national standard have been produced after treatment of subsequent procedures; and the purities of the produced rhodium powder and iridium powder can be up to 99.95%.

Description

A kind of method of Solvent Extraction Separation purification platinum metals
Technical field
A method for Solvent Extraction Separation purification platinum metals, relates to a kind of metal separation and purifies, from platinum group metallic solution, slag or secondary resource, be particularly separated the method for platinum, palladium, rhodium iridium.
Background technology
Because platinum in platinum metals, palladium, rhodium, iridium character are close, there is larger difficulty in sepn process, being especially separated of platinum and rhodium, is generally acknowledged world-famous puzzle.The selective precipitator method of separation method of usual employing, solvent extration and molecular recognition method etc.Selective precipitation is simple to operate but separation efficiency is not high, solvent extration has higher separation efficiency but requires height, liquid waste disposal amount large to liquid before extraction and organic phase is detrimental to health, molecular recognition technology is the high and new separation technology that development in recent years is got up, separation efficiency is high but high to the requirement of Partial Elements in solution as iron, sodium, material adaptive faculty is limited, not yet realizes industrial applications.
At present, adopt in the process of extracting and separating platinum, palladium, part rhodium, iridium are also total to extraction and enter in load organic phases, enter in strip liquor in company with platinum, palladium in stripping process, the rhodium iridium entered in this process in platinum palladium product arrives about 30%, reduce the yield of rhodium, iridium product, have impact on the quality of platinum, palladium product.
Summary of the invention
Object of the present invention is exactly the deficiency existed for above-mentioned prior art, provides a kind of and can reduce the impurity content made before extraction in liquid widely, improve the method for the product yield of platinum metals and the Solvent Extraction Separation purification platinum metals of quality.
The object of the invention is to be achieved through the following technical solutions.
A method for Solvent Extraction Separation purification platinum metals, is characterized in that the step of its purification process comprises:
(1) material of platinum group metal is carried out chlorinating dissolution, chlorinating dissolution product is carried out filtration and obtains chlorinating dissolution liquid;
(2) add ammonium oxalate at chlorinating dissolution liquid, carry out copper nickel precipitate and separate;
(3) liquid after precipitated copper nickel step (2) precipitated and isolated, add organic reducing agent vitamins C and carry out the precipitin reaction of platinum palladium, filtering separation obtains the filtrate of platiniferous palladium precipitation slag and rhodium-containing iridium;
(4) platiniferous palladium precipitation slag step (3) obtained through aqua regia dissolution, catch up with nitre, enter isoamyl sulfide extracting and separating platinum palladium operation;
(5) filtrate of rhodium-containing iridium step (3) obtained passes into chlorine react through adding Manganse Dioxide, enters TBP calcium phosphate+ forage separate rhodium iridium operation.
The method of a kind of Solvent Extraction Separation purification platinum metals of the present invention, it is characterized in that described step (1) be platinum group metalliferous material is sized mixing to solid-liquid weight ratio be 4-5:1, be 2.5-3mol/L by hydrochloric acid conditioning solution acidity, be 75-80 DEG C in temperature to pass into chlorine and carry out chlorinating dissolution liquid making, its dissolution time is 8-12 hour, and chlorine intake is 15 ~ 25L/h.
The method of a kind of Solvent Extraction Separation purification platinum metals of the present invention, it is characterized in that described step (2) is is 1-1.5 by the pH value that the chlorinating dissolution liquid of step adjusts, add ammonium oxalate and carry out precipitated copper nickel reactant, temperature of reaction is 90-95 DEG C, and the reaction times is 0.5-1h; The add-on of ammonium oxalate is 35-40g/L.
The method of a kind of Solvent Extraction Separation purification platinum metals of the present invention, it is characterized in that liquid after the precipitated copper nickel that described step (3) precipitates and isolates, adding the temperature that organic reducing agent vitamins C carries out the precipitin reaction of platinum palladium is 70-75 DEG C, and the reaction times is 0.5-1h; Ascorbic add-on is 45-60g/L.
The method of a kind of Solvent Extraction Separation purification platinum metals of the present invention, the filtrate that it is characterized in that the rhodium-containing iridium that step (3) obtains by described step (5) passes into chlorine react through adding Manganse Dioxide, the add-on of Manganse Dioxide is 2-3.5g/L, reaction times 25-40min, chlorine intake 15 ~ 25L/h.
The method of a kind of Solvent Extraction Separation purification platinum metals of the present invention, platinum group metal concentrate (solution, slag, secondary resource etc.) is carried out chlorinating dissolution, lysate acid adjustment degree carries out heavy copper, nickel reactant, carry out heavy platinum, palladium again, filtering separation platinum palladium and rhodium iridium.Heavy platinum palladium filter residue aqua regia dissolution is connected isoamyl sulfide extraction palladium separating platinum palladium after catching up with nitre to regulate acidity, filtrate is connected TBP and extracts iridium separate rhodium iridium.
Because reaction is carried out in the liquid phase, platinum group metal solid material needs the liquid making process of step (1), if material is originally as liquid, does not then need step (1).
Method of the present invention, the impurity contents such as the copper before 1. can making extraction in liquid, nickel reduce widely, and copper nickel average deposition rate is more than 95%; 2. after platinum palladium is separated with rhodium iridium, platinum palladium and rhodium iridium obtain further enrichment, are conducive to the further separating-purifying platinum of follow-up extraction process, palladium, rhodium, iridium.3. this method can improve product yield and the quality of platinum metals greatly.
Method platinum palladium of the present invention and rhodium iridium separation rate high, the further separating platinum of easy follow-up extraction and palladium, rhodium and iridium.Not only make rhodium iridium obtain high efficiente callback, and reduce the loss of platinum palladium.Because reductive agent vitamins C is organic reagent, solution system can not be changed, new metallic impurity can not be brought in reaction process, therefore can not to platinum metals be separated and refining impact, output purity be greater than 99.99% platinum black and palladium black produced through the process of subsequent handling the spongy platinum and palladium sponge product that meet national standard; The rhodium powder produced through this method and iridium powder purity also reach 99.95%.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention.
Embodiment
A method for Solvent Extraction Separation purification platinum metals, the step of its purification process comprises: the material of platinum group metal is carried out chlorinating dissolution by (1), chlorinating dissolution product is carried out filtration and obtains chlorinating dissolution liquid; (2) add ammonium oxalate at chlorinating dissolution liquid, carry out copper nickel precipitate and separate; (3) liquid after precipitated copper nickel step (2) precipitated and isolated, add organic reducing agent vitamins C and carry out the precipitin reaction of platinum palladium, filtering separation obtains the filtrate of platiniferous palladium precipitation slag and rhodium-containing iridium; (4), after the platiniferous palladium precipitation slag that step (3) obtains being carried out aqua regia dissolution, catching up with nitre, isoamyl sulfide extracting and separating platinum palladium operation is entered; (5) filtrate of rhodium-containing iridium step (3) obtained adds Manganse Dioxide and passes into after chlorine reacts, and enters calcium phosphate+ forage separate rhodium iridium operation.
The step of concrete operations comprises:
Platinum group metalliferous material is carried out chlorinating dissolution by step (1), and liquid-solid mass ratio is 4-5:1; Be 2.5-3mol/L by hydrochloric acid conditioning solution acidity, be 75-80 DEG C in temperature and pass into chlorine (15-25L/h) and dissolve, dissolution time is 8-12 hour;
Step (2) lysate is after secondary filter, adding solid caustic soda adjustment filtrate pH value is 1-1.5, if there is precipitation, then by filtrate secondary filter, filter residue is deposited separately, and in 1-2 minute, add ammonium oxalate precipitated copper nickel when the filtrate of adjusting being heated to 90 DEG C, ammonium oxalate add-on is 35-40g/L, be cooled to less than 30 DEG C after insulated and stirred 0.5-1h after continuing to be heated to 95 DEG C to filter, and filter residue is washed;
Organic reducing agent vitamins C platinum precipitation, palladium is added in 1-2 minute when filtrate and washings are stirred and is heated to 70-75 DEG C by step (3), vitamins C add-on is 45-60g/L, be incubated and be cooled to less than 30 DEG C after stirring 0.5-1h and filter, and filter residue is washed;
Step (4) filter residue aqua regia dissolution send isoamyl sulfide to extract palladium operation separating platinum, palladium after catching up with nitre to regulate acidity;
Step (5) filtrate adds Manganse Dioxide and passes into chlorine and react, and the add-on of Manganse Dioxide is 2-3.5g/L, reaction times 25-40min, and chlorine intake 15 ~ 25L/h, filters after completion of the reaction, and filtrate send TBP to extract iridium operation separate rhodium, iridium.
Embodiment 1
Precious metal concentrate leads to chlorine (23L/h) chlorination 40 minutes, and liquid-solid mass ratio is 4:1, then regulates acidity to be 2.5mol/L with hydrochloric acid, is heated to the dissolving of 80 DEG C of logical chlorine (25L/h), dissolution time 8 hours.After lysate secondary filter elimination insoluble slag, filtrate volume is 400L(bullion content is 18g/L), it is 1 that solution adds solid caustic soda adjust ph, 14kg ammonium oxalate is added under stirring when being heated to 90 DEG C, light blue precipitation is produced immediately in solution, and continue to add 0.5kg ammonium oxalate when being heated with stirring to 95 DEG C, generate without obvious sediment.Be incubated after 30 minutes and be cooled to 30 DEG C of filtrations, filter residue 20L deionization moisture 4 washings, filtrate is stirred and adds 24kg organic reducing agent vitamins C after being heated to 70 DEG C, now have a large amount of grey black to precipitate to generate, be incubated and be cooled to 30 DEG C of blowings after stirring 20 minutes and filter, filter residue 30L deionized water wash 3 times, filter residue aqua regia dissolution extracts palladium separating platinum, palladium through isoamyl sulfide after catching up with nitre to regulate acidity, 1kg Manganse Dioxide is added under filtrate normal temperature, stir lower logical chlorine 25 minutes, then extract iridium separate rhodium iridium through TBP.
Embodiment 2
The remaining liquid of extraction gold amasss as 500L(bullion content is 20g/L), it is 1.05 that solution adds solid caustic soda adjust ph, adds 14kg ammonium oxalate, produce light blue precipitation immediately in solution when being heated to 92 DEG C under stirring, and continue to add 0.6kg ammonium oxalate when being heated with stirring to 95 DEG C, generate without obvious sediment.Be incubated after 35 minutes and be cooled to 25 DEG C of filtrations, filter residue 30L deionization moisture 3 washings, filtrate is stirred and adds 24kg organic reducing agent vitamins C after being heated to 74 DEG C, now have a large amount of grey black to precipitate to generate, be incubated and be cooled to 23 DEG C of blowings after stirring 25 minutes and filter, filter residue 30L deionized water wash 3 times, filter residue aqua regia dissolution extracts palladium separating platinum, palladium through isoamyl sulfide after catching up with nitre to regulate acidity, 1.1kg Manganse Dioxide is added under filtrate normal temperature, stir lower logical chlorine 30 minutes, then extract iridium separate rhodium iridium through TBP.

Claims (5)

1. a method for Solvent Extraction Separation purification platinum metals, is characterized in that the step of its purification process comprises:
(1) material of platinum group metal is carried out chlorinating dissolution, chlorinating dissolution product is carried out filtration and obtains chlorinating dissolution liquid;
(2) add ammonium oxalate at chlorinating dissolution liquid, carry out copper nickel precipitate and separate;
(3) liquid after precipitated copper nickel step (2) precipitated and isolated, add organic reducing agent vitamins C and carry out the precipitin reaction of platinum palladium, filtering separation obtains the filtrate of platiniferous palladium precipitation slag and rhodium-containing iridium;
(4) platiniferous palladium precipitation slag step (3) obtained through aqua regia dissolution, catch up with nitre, enter isoamyl sulfide extracting and separating platinum palladium operation;
(5) filtrate of rhodium-containing iridium step (3) obtained passes into chlorine react through adding Manganse Dioxide, enters calcium phosphate+ forage separate rhodium iridium operation.
2. the method for a kind of Solvent Extraction Separation purification platinum metals according to claim 1, it is characterized in that described step (1) be platinum group metalliferous material is sized mixing to solid-liquid weight ratio be 4-5:1, be 2.5-3mol/L by hydrochloric acid conditioning solution acidity, be 75-80 DEG C in temperature to pass into chlorine and carry out chlorinating dissolution liquid making, its dissolution time is 8-12 hour, and chlorine intake is 15 ~ 25L/h.
3. the method for a kind of Solvent Extraction Separation purification platinum metals according to claim 1, it is characterized in that described step (2) is is 1-1.5 by the pH value that the chlorinating dissolution liquid of step adjusts, add ammonium oxalate and carry out precipitated copper nickel reactant, temperature of reaction is 90-95 DEG C, and the reaction times is 0.5-1h; The add-on of ammonium oxalate is 35-40g/L.
4. the method for a kind of Solvent Extraction Separation purification platinum metals according to claim 1, it is characterized in that liquid after the precipitated copper nickel that described step (3) precipitates and isolates, adding the temperature that organic reducing agent vitamins C carries out the precipitin reaction of platinum palladium is 70-75 DEG C, and the reaction times is 0.5-1h; Ascorbic add-on is 45-60g/L.
5. the method for a kind of Solvent Extraction Separation purification platinum metals according to claim 1, the filtrate that it is characterized in that the rhodium-containing iridium that step (3) obtains by described step (5) passes into chlorine react through adding Manganse Dioxide, the add-on of Manganse Dioxide is 2-3.5g/L, reaction times 25-40min, chlorine intake 15-25L/h.
CN201410749722.7A 2014-12-10 2014-12-10 Method for separating and purifying platinum metals through solvent extraction Pending CN104532011A (en)

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Cited By (6)

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Publication number Priority date Publication date Assignee Title
CN105219967A (en) * 2015-10-14 2016-01-06 云龙县铂翠贵金属科技有限公司 A kind of copper base plating palladium electronic waste moves back palladium and puies forward the method for copper
CN105296759A (en) * 2015-11-18 2016-02-03 金川集团股份有限公司 Method for selectively separating copper and nickel from platinum group metal feed liquid
CN105671304A (en) * 2016-02-25 2016-06-15 昆明贵金属研究所 Method for recycling rare earth and platinum group metal from spent automobile emission purification catalyst
CN107574314A (en) * 2017-08-25 2018-01-12 金川集团股份有限公司 A kind of method of refined platinum in strip liquor from platinum
CN108165743A (en) * 2017-12-28 2018-06-15 郴州雄风环保科技有限公司 A kind of full extraction and separation prepare high-purity Au, Pt, Pd technology
CN110592391A (en) * 2019-09-19 2019-12-20 李旭意 Method for purifying crude gold powder

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105219967A (en) * 2015-10-14 2016-01-06 云龙县铂翠贵金属科技有限公司 A kind of copper base plating palladium electronic waste moves back palladium and puies forward the method for copper
CN105296759A (en) * 2015-11-18 2016-02-03 金川集团股份有限公司 Method for selectively separating copper and nickel from platinum group metal feed liquid
CN105671304A (en) * 2016-02-25 2016-06-15 昆明贵金属研究所 Method for recycling rare earth and platinum group metal from spent automobile emission purification catalyst
CN107574314A (en) * 2017-08-25 2018-01-12 金川集团股份有限公司 A kind of method of refined platinum in strip liquor from platinum
CN107574314B (en) * 2017-08-25 2019-05-10 金川集团股份有限公司 A method of the refined platinum from platinum strip liquor
CN108165743A (en) * 2017-12-28 2018-06-15 郴州雄风环保科技有限公司 A kind of full extraction and separation prepare high-purity Au, Pt, Pd technology
CN110592391A (en) * 2019-09-19 2019-12-20 李旭意 Method for purifying crude gold powder

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Application publication date: 20150422