CN103882242A - Method for utilizing chelate resin to realize separation of platinum, palladium and rhodium - Google Patents
Method for utilizing chelate resin to realize separation of platinum, palladium and rhodium Download PDFInfo
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- CN103882242A CN103882242A CN201210552408.0A CN201210552408A CN103882242A CN 103882242 A CN103882242 A CN 103882242A CN 201210552408 A CN201210552408 A CN 201210552408A CN 103882242 A CN103882242 A CN 103882242A
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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
A method for utilizing chelate resin to realize separation of platinum, palladium and rhodium is characterized by: (1) performing fragmentation, grinding and high-temperature roasting to obtain solid platinum metals, adding 2% by mass of an aqueous solution of sodium borohydride, boiling for reducing, and for enhancing the activity of platinum group metals; (2) filtering the reducing solution obtained in the step (1), adding a small amount of a hydrochloric acid solution of sodium chloride and sodium chlorite, mixing uniformly and transferring to a leaching apparatus, then leaching at 85 DEG C, washing a solid catalyst obtained by filtering with 10% HCl for two times, washing with water for one time, merging the washing liquids and the leaching liquid, concentrating and testing; (3) pre-processing separated resin; and (4) adding chelate resin subjected to preprocessing and accounting for 1.5 times of the theoretical amount into the leaching liquid obtained in the step (2), heating to 65 DEG C, adjusting the pH value of the solution, stirring for separating platinum group metal, and purifying to obtain high-purity platinum group metals. The method helps to effectively shorten the conventional flow of separation of platinum group metals, and the separation operation is green and environment-friendly.
Description
Technical field
the present invention relates to a kind of method that platinum, palladium separate with rhodium, particularly relate to a kind of resin that utilizes and realize the method that platinum, palladium separate with rhodium, belong to precious metals metallurgy field.
Background technology
at present, Separation and Recovery platinum, palladium mainly contain with the method for rhodium: aqua regia dissolution method coordinates sodium pyrosulfate melting-water seaoning.But this separation platinum family metal process complex process, energy and raw material consumption are large, and equipment requirements is high, and the difficult solution of problem of environmental pollution, should not promote and the deficiency of technique is that the extraction yield of rhodium is low, is generally about 65-80%, and the rate of recovery is on the low side.
publication number is that the Chinese invention patent application of CN 1609241 has provided a kind of " process for mutual separation of platinum family element ", it is the method that platinum family element from containing impurity element contains thing and be separated from each other platinum family element, it is characterized in that comprising following operation,, (1) the 1st operation, above-mentioned platinum family element is contained to thing and be suspended in hydrochloric acid soln, after interpolation oxygenant, carry out lixiviate, the lixiviate that obtains containing platinum family element generates liquid; (2) the 2nd operations, generate liquid by above-mentioned lixiviate and contact and carry out solvent extraction with glycol ether dibutyl ether, form the organic phase and the raffinate that contain impurity element; (3) the 3rd operations, contact with dialkyl group sulphur the raffinate being obtained by above-mentioned the 2nd operation carry out solvent extraction, after extraction of palladium, strip, and form the reextraction that contains palladium and generate liquid and raffinate; (4) the 4th operations, contact with two (2-ethylhexyl) phosphoric acid the raffinate being obtained by above-mentioned the 3rd operation carry out solvent extraction, form the organic phase and the raffinate that contain cationic impurity element; (5) the 5th operations, become 5～12 by the pH regulator of the raffinate being obtained by above-mentioned the 4th operation, after interpolation oxygenant, are hydrolyzed, and form the precipitation that contains iridium, ruthenium and rhodium and the aqueous solution that contains platinum; (6) the 6th operations, are not less than the above-mentioned pH of being deposited in and in 12 strong alkali aqueous solution, add oxygenant and carry out lixiviate, form the residue and the ruthenium lixiviate that contain iridium and rhodium and generate liquid; (7) the 7th operations, the aqueous solution that contains above-mentioned residue and be dissolved in iridium that hydrochloric acid soln obtains and rhodium is contacted with tributyl phosphate and carries out solvent extraction, after extraction iridium, strip, form the reextraction that contains iridium and generate liquid and the raffinate that contains rhodium.The shortcoming that this separation platinum family metal process exists: the shortcomings such as technical process is long, energy consumption is large, environmental pollution is serious.
publication number is that the Chinese invention patent application of CN 102586607A has provided and " a kind of from inefficacy platinum alloy net, extracts platinum, rhodium, the method of palladium ", it is separation and Extraction noble metal platinum from inefficacy platinum alloy net, rhodium, palladium, by hydrochloric acid+nitric acid dissolve, except nitro, turn sodium type, suction filtration, obtain platinum rhodium palladium complex solution, adopt chloride precipitation method Separation of Platinum, with Sodium Nitrite complexing seperation palladium, rhodium, with six nitroso-group rhodium acid ammonium method purification rhodiums, with the sub-palladium method of dichloro two amminos purification palladium, through adding hydrazine hydrate reduction to obtain spongy platinum, palladium sponge and rhodium powder, through vacuum-drying, roasting, again purify, the spongy platinum extracting, the purity > 99.9% of palladium sponge and rhodium powder.The shortcoming that this separation platinum family metal process exists: technical process exists the shortcomings such as limitation, platinum metals separation rate are not high.
in sum, in the method for existing Separation of Platinum, palladium and rhodium, all or have the problems such as operating environment is poor, platinum metals yield is low, energy expenditure is large, further Improvement and perfection needs.
Summary of the invention
object of the present invention is just to overcome the deficiency that prior art exists, the problem existing for existing platinum, palladium and rhodium separation method, has proposed to utilize resin to realize the method that platinum, palladium separate with rhodium separating add in platinum family metal flow journey that resin separates a kind of new.
the technical solution that the present invention provides is: this resin that utilizes is realized the method that platinum, palladium separate with rhodium, be characterized in: first to the solid-phase that contains platinum metals is leached and transferred platinum, palladium, rhodium to liquid phase by chlorination, in order to ensure resin, the front reply of the best effect experiment resin of platinum metals absorption is soaked 30min and washed 2 times in 4%HCl, stand-by after drying.
the present invention provides, and this resin that utilizes is realized the method that platinum, palladium separate with rhodium, is characterized in: be made up of following steps.
(1) the solid platinum metals obtaining through crushing grinding, high-temperature roasting, adds the sodium borohydride aqueous solution of 2% mass ratio to boil reduction, and platinum metals activity is enhanced.
(2) reduced liquid 1 step being obtained filters, allocate the hydrochloric acid soln of a small amount of sodium-chlor and Textone into, after mixing, proceed to leaching device, then carry out extraction time 180min at 85 DEG C, filtration obtains solid catalyst and adds 10%HCl pickling 2 times (80 DEG C, 20min), wash 1 time (80 DEG C, 20min) washing lotion and leach liquor are merged, concentrated, chemical examination.
(3) separation resin pre-treatment: before experiment, reply resin soaks 30min and washes 2 times in 4%HCl.
(4) leach liquor (2) being obtained, adds the resin of 1.5 times of theoretical amount after pretreatment, is heated to 65 DEG C,, stirs and carries out platinum metals and separate 80min to pH value 2.5～3 by 5%HCl regulator solution acidity, purifies, and obtains high-purity platinum metals.
compared with prior art, the invention has the beneficial effects as follows: effectively shortened the existing procedure that platinum metals separates, energy efficient, realizes lock out operation environmental protection, and platinum metals separation rate is improved.
Specific embodiments
embodiment 1.
get the leach liquor 2000ml containing three kinds of precious metal elements of platinum, palladium, rhodium, in stirring water-bath, be heated to 65 DEG C, in backward leach liquor, drop into 130g resin, by 5%HCl regulator solution acidity; Disengaging time 60min, then suction filtration, chemically examines leach liquor and resin isolation liquid.
result.
platinum content in leach liquor: 0.15%, the purity 99.95 of output spongy platinum.
palladium content in leach liquor: 0.12%, output palladium sponge purity 99.96.
rhodium content in leach liquor: 98.5%, output sponge rhodium purity 99.95.
embodiment 2.
get the leach liquor 2000ml containing three kinds of precious metal elements of platinum, palladium, rhodium, in stirring water-bath, be heated to 70 DEG C, in backward leach liquor, drop into 150g resin, use 5%HCl regulator solution acidity to PH=3; Disengaging time 60min, then suction filtration, chemically examines leach liquor and resin isolation liquid.
result.
platinum content in leach liquor: 0.14%, the purity 99.95 of output spongy platinum.
palladium content in leach liquor: 0.10%, output palladium sponge purity 99.96.
rhodium content in leach liquor: 98.7%, output sponge rhodium purity 99.95.
embodiment 3.
get the leach liquor 2000ml containing three kinds of precious metal elements of platinum, palladium, rhodium, in stirring water-bath, be heated to 65 DEG C, in backward leach liquor, drop into 150g resin, use 5%HCl regulator solution acidity 5%HCl regulator solution acidity to PH=3; Disengaging time 80min, then suction filtration, detects leach liquor and resin isolation liquid.
result.
platinum content in leach liquor: 0.11%, the purity 99.95 of output spongy platinum.
palladium content in leach liquor: 0.10%, output palladium sponge purity 99.95.
rhodium content in leach liquor: 98.7%, output sponge rhodium purity 99.95.
Claims (1)
1. one kind is utilized resin to realize the method that platinum, palladium separate with rhodium, it is characterized in that: first to the solid-phase that contains platinum metals is leached and transferred platinum, palladium, rhodium to liquid phase by chlorination, in order to ensure resin, the front reply of the best effect experiment resin of platinum metals absorption is soaked 30min and washed 2 times in 4%HCl, stand-by after drying, specifically there are following steps:
(1) the solid platinum metals obtaining through crushing grinding, high-temperature roasting, adds the sodium borohydride aqueous solution of 2% mass ratio to boil reduction, and platinum metals activity is enhanced;
(2) reduced liquid step (1) being obtained filters, allocate the hydrochloric acid soln of a small amount of sodium-chlor and Textone into, after mixing, proceed to leaching device, then carry out extraction time 180min at 85 DEG C, filtration obtains solid catalyst and adds 10%HCl pickling 2 times (80 DEG C, 20min), wash 1 time (80 DEG C, 20min) washing lotion and leach liquor are merged, concentrated, chemical examination;
(3) separation resin pre-treatment: before experiment, reply resin soaks 30min and washes 2 times in 4%HCl;
(4) leach liquor step (2) being obtained, adds the resin of 1.5 times of theoretical amount after pretreatment, is heated to 65 DEG C, by 5%HCl regulator solution acidity to pH value 2.5～3, stirring is carried out platinum metals and is separated 80min, purifies, and obtains high-purity platinum metals.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210552408.0A CN103882242A (en) | 2012-12-19 | 2012-12-19 | Method for utilizing chelate resin to realize separation of platinum, palladium and rhodium |
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| CN201210552408.0A CN103882242A (en) | 2012-12-19 | 2012-12-19 | Method for utilizing chelate resin to realize separation of platinum, palladium and rhodium |
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| CN103882242A true CN103882242A (en) | 2014-06-25 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105256136A (en) * | 2015-11-18 | 2016-01-20 | 金川集团股份有限公司 | Method of separating platinum group metals from platinum group metal feed liquid |
| CN106086452A (en) * | 2016-08-09 | 2016-11-09 | 成都虹华环保科技股份有限公司 | A kind of Palladium recovery device |
| CN106636647A (en) * | 2016-11-14 | 2017-05-10 | 中海油天津化工研究设计院有限公司 | Method for recycling rhodium carbonyl complex through chemical adsorption method |
| CN108265180A (en) * | 2017-12-28 | 2018-07-10 | 核工业北京化工冶金研究院 | The leaching method of platinum, palladium, rhodium in useless three-way catalyst |
| CN109402413A (en) * | 2018-10-30 | 2019-03-01 | 中国工程物理研究院核物理与化学研究所 | The recovery method of palladium in a kind of spent fuel element fission product |
| CN110760684A (en) * | 2019-12-04 | 2020-02-07 | 沈阳有色金属研究院有限公司 | Method for recovering platinum from platinum-containing organic matter |
| CN112899478A (en) * | 2021-01-13 | 2021-06-04 | 深圳市正力实业有限公司 | Device and method for efficiently purifying precious metals in waste automobile exhaust catalyst |
-
2012
- 2012-12-19 CN CN201210552408.0A patent/CN103882242A/en active Pending
Non-Patent Citations (1)
| Title |
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| 王大维等: "提高废三元催化剂铂族金属回收率工艺研究", 《有色矿冶》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105256136A (en) * | 2015-11-18 | 2016-01-20 | 金川集团股份有限公司 | Method of separating platinum group metals from platinum group metal feed liquid |
| CN106086452A (en) * | 2016-08-09 | 2016-11-09 | 成都虹华环保科技股份有限公司 | A kind of Palladium recovery device |
| CN106086452B (en) * | 2016-08-09 | 2017-11-07 | 成都虹华环保科技股份有限公司 | A kind of Palladium recovery device |
| CN106636647A (en) * | 2016-11-14 | 2017-05-10 | 中海油天津化工研究设计院有限公司 | Method for recycling rhodium carbonyl complex through chemical adsorption method |
| CN108265180A (en) * | 2017-12-28 | 2018-07-10 | 核工业北京化工冶金研究院 | The leaching method of platinum, palladium, rhodium in useless three-way catalyst |
| CN109402413A (en) * | 2018-10-30 | 2019-03-01 | 中国工程物理研究院核物理与化学研究所 | The recovery method of palladium in a kind of spent fuel element fission product |
| CN109402413B (en) * | 2018-10-30 | 2020-11-03 | 中国工程物理研究院核物理与化学研究所 | Method for recovering palladium in fission product of spent fuel element |
| CN110760684A (en) * | 2019-12-04 | 2020-02-07 | 沈阳有色金属研究院有限公司 | Method for recovering platinum from platinum-containing organic matter |
| CN112899478A (en) * | 2021-01-13 | 2021-06-04 | 深圳市正力实业有限公司 | Device and method for efficiently purifying precious metals in waste automobile exhaust catalyst |
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Application publication date: 20140625 |