CN101658942A - Method for extracting rhodium powder from waste platinum nets - Google Patents

Method for extracting rhodium powder from waste platinum nets Download PDF

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Publication number
CN101658942A
CN101658942A CN200910075588A CN200910075588A CN101658942A CN 101658942 A CN101658942 A CN 101658942A CN 200910075588 A CN200910075588 A CN 200910075588A CN 200910075588 A CN200910075588 A CN 200910075588A CN 101658942 A CN101658942 A CN 101658942A
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rhodium
solution
powder
platinum
acid
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CN101658942B (en
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姚素玲
刘学忠
张桂香
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Zhang Guixiang
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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 extracting rhodium powder from waste platinum nets. According to an actual condition that much noble metal of rhodium exists in aqua regia insoluble matters in the processing course of the waste platinum nets, the rhodium is extracted from the aqua regia insoluble matters, then rhodium complexing liquid is prepared by mechanical crushing, grinding, screening,roasting by barium peroxide, dissolving, precipitating, filtering, heating and concentrating, washing, platinum removing, complexing with sodium nitrite, heating and boiling, vacuum pump filtering andrapid cooling, and the off-white rhodium powder is finally prepared by heating and dissolving, ion exchanging, hydrazine hydrate reducing, distilling, drying and roasting and reducing by hydrogen. The preparing method is advanced and reasonable, the parameters are accurate, and the method makes possible extracting of the rhodium from the aqua regia insoluble matters of the waste platinum nets, the rhodium content in the extracted rhodium powder can reach 99.95 percent, the quality is steady, and the method is an ideal method for extracting the rhodium powder from the waste platinum nets.

Description

A kind of method of from waste platinum nets, extracting the rhodium powder
Technical field
The present invention relates to a kind of method of from waste platinum nets, extracting the rhodium powder, belong to the technical field that the utilization of noble metal slag liquid is extracted.
Background technology
Noble metal is meant gold, silver, platinum, ruthenium, rhodium, palladium, iridium, osmium, particularly difficulty because content is low in the earth's crust, reserves are few, is extracted in the platinum group metal, the production cost height, thereby being worth costliness, the platinum group metal has the d electronic shell of underfill, and high temperature resistant, anti-oxidant, corrosion resistance is strong, and activity and selectivity are good, and the Chang Zuowei catalyst is in industrial application.
Nitric acid is important inorganic acid, the platinum alloy net is the catalyst of preparing nitric acid by ammonia oxidation, pressure difference according to ammoxidation, ternary net and binary net are arranged, the ternary net is by 92.5% platinum, 3.5% rhodium, 4.0% palladium is formed, the binary net is made up of platinum and rhodium, rhodium content is respectively 5%, 7%, 8%, 10%, the platinum alloy net uses after a period of time because the noble metal loss, surface texture changes, influence catalytic performance, and the platinum group metal costs an arm and a leg, resource scarcity, reclaim the platinum group metal and become important secondary resource, from waste platinum nets, reclaim the production cost of platinum group metal and extract low doubly much than primary metal production, also can reduce energy resource consumption and the harm of environment.
The waste platinum nets recovery method has wet method, dry method and gas phase volatility process, and wet method often is widely adopted owing to low, the mild condition of cost; The one, platinum guaze reclaims, be with batching, wire drawing, knitmesh etc. again after platinum guaze dissolving, purification, the reduction, the 2nd, the platinum ash reclaims, be with the roasting of platinum ash, molten material, separation, purification, though be platinum guaze, or platinum ash removal process in all to use aqua regia dissolution, noble metal is entered in the solution handles, undissolvable is waste residue, the indissoluble of rhodium is separated, thereby often contains a large amount of rhodiums in the aqua regia insoluble thing, how to handle, extract, utilize the rhodium in the aqua regia insoluble thing to become a new research topic.
Summary of the invention
Goal of the invention
Purpose of the present invention is exactly the actual conditions at prior art, rhodium is reclaimed in proposition from waste platinum nets, waste platinum nets is ground the adding aqua regia dissolution, and generation insoluble matter, adopt new extracting method, in the insoluble matter of waste platinum nets, extract rhodium element, become possibility so that in the aqua regia insoluble thing of waste platinum nets, extract rhodium.
Technical scheme
The chemical substance material that the present invention uses is: waste platinum nets, barium peroxide, natrium nitrosum, sodium chloride, hydrochloric acid, nitric acid, sulfuric acid, hydrazine hydrate, ammonium chloride, silver nitrate, NaOH, deionized water, hydrogen, nitrogen, its combination consumption is as follows: with gram, milliliter, centimetre 3Be measurement unit
Waste platinum nets: Pt Rh Pd 10000g ± 10g
Barium peroxide: BaO 2500g ± 10g
Natrium nitrosum: NaNO 2550g ± 10g
Sodium chloride: NaCl 250g ± 10g
Hydrochloric acid: HCl 52000ml ± 100ml
Nitric acid: HNO 313000ml ± 100ml
Sulfuric acid: H 2SO 4200ml ± 10ml
Hydrazine hydrate: N 2H 4H 2O 600ml ± 10ml
NaOH: NaOH 10g ± 1g
Ammonium chloride: NH 4Cl 300g ± 10g
Silver nitrate: AgNO 310g ± 1g
Deionized water: H 2O 30000ml ± 100ml
Hydrogen: H 210000cm 3± 100cm 3
Nitrogen: N 210000cm 3± 100cm 3
Rhodium powder extracting method is as follows:
(1) selected chemical substance material
To carry out selectedly to the chemical substance material that extract to use, and carry out quality purity control:
Waste platinum nets: solid-state solid platinum 92.5%, rhodium 3.5%, palladium 4.0%
Barium peroxide: solid-state solid 99.0%
Inferior sodium nitrate: solid-state solid 99.0%
Sodium chloride: solid-state solid 99.0%
Hydrochloric acid: liquid strength of fluid 20%, 36%
Sulfuric acid: liquid strength of fluid 98%, 10%
Nitric acid: liquid strength of fluid 65%
Sal-ammoniac: solid-state solid 99.5%
Hydrazine hydrate: liquid liquid 64%
NaOH: solid-state solid 99.0%
Silver nitrate: solid-state solid 99.0%
Deionized water:: liquid liquid 99.5%
Hydrogen: gaseous state gas 99.0%
Nitrogen: gaseous state gas 99.0%
(2) mechanical crushing waste platinum nets
Waste platinum nets is placed in the pulverizer, carry out mechanical crushing, become the platinum powder, powder average grain diameter 0.5mm;
(3) mechanical lapping, sieve
Platinum powder after pulverizing is carried out mechanical lapping, and sieve, grind, sieve and carry out repeatedly, become: platinum fine powder, powder diameter≤0.074mm with 100 purpose screen clothes;
(4) preparation chloroazotic acid, dissolving platinum fine powder
With platinum fine powder 10000g, place ceramic vessel, adding concentration is 36% hydrochloric acid 50000ml, 65% nitric acid 12500ml, stirs, and becomes: wang aqueous solution;
Platinum, the dissolving of palladium element, the rhodium element oligodynamical;
(5) filter
Wang aqueous solution is placed on the filtering flask, filter, retain on the filter paper: aqua regia insoluble rhodium slag with one deck middling speed qualitative filter paper;
(6) add the barium peroxide roasting
100g places crucible with aqua regia insoluble rhodium slag, adds barium peroxide 500g then, stirs after the mixing, becomes aqua regia insoluble rhodium slag+barium peroxide mixture;
The crucible that fills aqua regia insoluble slag+barium peroxide mixture is placed roaster, and temperature rises to 900 ℃ ± 5 ℃ by 20 ℃, at this temperature constant temperature, insulation, roasting time 90min ± 2min;
After the roasting, close roaster, make it cool to 20 ℃ with the furnace, become: the aqua oxidation rhodium;
(7) dissolving aqua oxidation rhodium
600g places in the ceramic cylinder with the aqua oxidation rhodium, adds 20% watery hydrochloric acid 1000ml, places on the electric heater then, 95 ℃ of heating-up temperatures, heat time heating time, 210min ± 5min closed heater then, make it naturally cool to 20 ℃, become: rhodium complex solution, that is: H3RhCl6;
(8) filter
The rhodium complex solution is placed filter tunnel, filter, retain impurity on the filter paper, in the filter flask be: the rhodium complex solution with three layers of middling speed qualitative filter paper;
(9) precipitate, leave standstill
The rhodium complex solution is placed ceramic vessel, add 10% sulfuric acid 1600ml, leave standstill, precipitate 720min;
(10) cross filtering barium
With the rhodium complex solution that leaves standstill, filter with three layers of middling speed qualitative filter paper, retain barium sulfate BaSO on the filter paper 4Impurity is the rhodium complex solution in the filter flask;
(11) heating, concentrated
The rhodium complex solution is placed beaker, place then on the electric heater, 95 ℃ ± 2 ℃ of heating-up temperatures add sodium chloride 80g, continue heating, add deionized water 2000ml when being pulpous state, make solution concentration reach 45g/L, become: rhodium complex solution Na 3RhCl 6
(12) remove platinum
Add ammonium chloride 15g ± 1g in the rhodium complex solution, stir, the platinum in the solution becomes the ammonium chloroplatinate yellow mercury oxide, sediment after filtration, dry, purify, become: spongy platinum, and removing, retain the rhodium complex liquid;
(13) inferior sodium nitrate complexing
To place ceramic cylinder except that the rhodium complex solution behind the platinum, and add deionized water 1800ml, making solution concentration is 25g/L, and adjusting the pH value with 10% sodium hydroxide solution is 1.5;
Heat temperature raising places ceramic cylinder on the electric heater, and 95 ℃ ± 2 ℃ of heating-up temperatures heat while stirring, and adds 50% sodium nitrite solution 1400ml of preparation in advance then, makes its boiling, boils 60min ± 2min, and making the pH value is 5.5;
Close heater, make it be cooled to 20 ℃ naturally;
Na 3RhCl 6Solution transfers Na to 3Rh (NO 2) 6Solution;
Materials such as Fe, Al, Ca, Zn generate precipitation of hydroxide in the solution;
(14) suction filtration is removed base metals such as Fe, Al, Ca, Zn
Solution is placed Buchner funnel, carry out suction filtration with three layers of middling speed qualitative filter paper, retain base metal Fe, Al, Ca, Zn etc. on the filter paper, filtrate is Na in the filter flask 3Rh (NO 2) 6Solution;
(15) rhodium of cooling precipitation fast
Filtrate is placed the ice bath cylinder, be quickly cooled to 18 ℃, add ammonium chloride 240g, stirring, ageing 30min generate milky six nitroso rhodiums acid ammonium, and precipitation, that is: mixed liquor (NH 4) 3Rh (NO 2) 6↓
(16) vacuum filtration
Mixed liquor is placed on the vacuum filtration bottle, with three layers of middling speed qualitative filter paper suction filtration, retain six nitroso rhodiums acid ammonium on the filter paper, filtrate is the rhodium mother liquor, and the rhodium-containing amount is low in the rhodium mother liquor, and after three circular treatment, the rhodium-containing amount is 0.005%, can discard;
(17) heating for dissolving is removed nitro
Six nitroso rhodiums acid ammonium is placed ceramic cylinder, add 20% hydrochloric acid 2500ml, be heated to 95 ℃, until there not being brown gas HNO 3Overflow, become: chlordene rhodium acid ammonium solution, that is: (NH 4) 3RhCl 6
(18) change sodium salt
When the heating of chlordene rhodium acid ammonium solution is concentrated into 1000ml, slowly add sodium chloride 120g, heating, be stirred to solution in the pasty state the time, divide respectively to add deionized water 200ml three times, be heated to 95 ℃ of evaporations then, remove unnecessary hydrochloric acid, when steaming again to pulpous state, add deionized water 1000ml, become chlordene rhodium acid sodium solution, i.e. Na 3RhCl 6
(19) ion-exchange
With the NaOH that adds 10% in the chlordene rhodium acid sodium solution, regulating the pH value is 1.5, behind cationic ion-exchange resin, remove trace impurity, the chlordene rhodium acid sodium solution of Cheng Chun is then with five flushing washings of deionized water, each water consumption 100ml makes rhodium all enter solution;
(20) hydrazine hydrate reduction
Chlordene rhodium acid sodium solution with behind cation exchange, the deionized water rinsing is heated to 95 ℃ of boilings, drips 64% hydrazine hydrate solution 600ml then, and rate of addition 5ml/min becomes white to solution, till the rhodium powder sinks;
(21) washing, filtration, detection
White solution is added deionized water 100ml, and agitator treating filters with one deck middling speed qualitative filter paper then, and washing, filtration repeat five times, then with till the no white precipitate of 10% silver nitrate check;
(22) vacuum filtration
With three layers of qualitative filter paper suction filtration, retain product on the filter paper, that is: rhodium powder filter cake;
(23) vacuum drying
Place vacuum drying chamber dry rhodium powder filter cake product, vacuum 10Pa, 115 ℃ of baking temperatures, drying time, 180min promptly got product: black rhodium powder after the drying;
(24) rhodium powder roasting, hydrogen reducing
Dried black rhodium powder is placed crucible, place roaster then, use earlier nitrogen flooding removing and harmful gas, nitrogen input speed 40cm 3/ min, roasting reduction under hydrogen shield then, hydrogen input speed 40cm 3/ min, 800 ℃ ± 2 ℃ of sintering temperatures, time 60min ± 2min naturally cools to 20 ℃ ± 3 ℃ then, and behind the roasting reduction, product becomes: canescence rhodium powder;
(25) detect, chemically examine, analyze, characterize
Pattern, color and luster, purity, the rhodium content of canescence rhodium powder to preparation chemically examined, analyzes, characterized;
Carry out constituent content analysis with Atomic Absorption Spectrometer;
Carry out morphology analysis with SEM;
(26) store
Canescence rhodium powder to preparation places water white glass container, is stored in cool place, drying, clean environment, waterproof, protection against the tide, acid-proof alkali salt to corrode, storage temperature≤20 ℃ ± 3 ℃, relative humidity≤10%.
Beneficial effect
The present invention compares with background technology has tangible advance, it is the actual conditions that have more Noble Metal Rhodium element at the aqua regia insoluble thing in the waste platinum nets process, in the aqua regia insoluble thing of waste platinum nets, extract rhodium element, pass through mechanical crushing, grind, sieve, the barium peroxide roasting, dissolving, through precipitation, filter, the heating thickening and washing, remove platinum, again through the natrium nitrosum complexing, heating is boiled, vacuum filtration, quicken cooling, make six nitroso rhodiums acid ammonium, again through heating for dissolving, ion-exchange, hydrazine hydrate reduction, dry, the hydrogen firing reduction, finally make canescence rhodium powder, this preparation method is rationally advanced, parameter is accurate, make in the aqua regia insoluble thing in the waste platinum nets process and to extract rhodium and become possibility, the rhodium content of the canescence rhodium powder that extracts reaches 99.95%, is the very good method of extracting rhodium in waste platinum nets.
Description of drawings
Fig. 1 is rhodium slag+barium peroxide roasting state diagram
Fig. 2 is the state diagram of rhodium powder roasting hydrogen reducing
Fig. 3 is a rhodium powder roasting hydrogen reducing temperature and time coordinate graph of a relation
Fig. 4 is a canescence rhodium powder shape appearance figure
Shown in the figure, list of numerals is as follows:
1, roaster, 2, furnace chamber, 3, electric heater, 4, base, 5, bell, 6, ceramic crucible, 7, platinum+barium peroxide mixed powder, 8, hydrogen, 9, hydrogen cylinder, 10, the hydrogen pipe, 11, hydrogen valve, 12, rhodium powder, 13, pore, 14, nitrogen cylinder, 15, nitrogen tube, 16, nitrogen valve.
The specific embodiment
The present invention will be further described below in conjunction with accompanying drawing:
Shown in Figure 1, be rhodium+barium peroxide roasting state diagram, be that heater 3, stove seat 4, top are bell 5, innerly are furnace chamber 2 in the bottom of roaster 1, ceramic crucible 6 is put in the bottom in the furnace chamber 2, ceramic crucible 6 tops are rhodium+barium peroxide mixed powder 7, the baking heat temperature is 900 ℃ ± 5 ℃, and roasting time is 90min ± 2min.
Shown in Figure 2, be the state diagram of rhodium powder roasting hydrogen reducing, put ceramic crucible 6 in the furnace chamber 2 in roaster 1, put rhodium powder 12 on the ceramic crucible 6, the left part of roaster 1 is provided with hydrogen cylinder 9, hydrogen pipe 10, hydrogen valve 11, in the hydrogen 8 input furnace chambers 2, form hydrogen reducing atmosphere, leave pore 13 on the furnace wall of roaster 1, be provided with nitrogen cylinder 14, nitrogen tube 15, nitrogen valve 16 in the left outside of roaster 1, and UNICOM's furnace chamber 2, remove pernicious gas in the furnace chamber with nitrogen flooding earlier, and then reduce with hydrogen.
Shown in Figure 3, be the roasting of rhodium powder, hydrogen reducing temperature and time coordinate graph of a relation, temperature is since 20 ℃ of intensifications, and promptly the A point rises to 800 ℃, and promptly the B point is incubated 60min at this temperature constant temperature, and promptly the B-C section cools to 20 ℃ then with the furnace, i.e. the D point.
Shown in Figure 4, be canescence rhodium powder shape appearance figure, the rhodium powder is the graininess powder, and there is silvery white gloss on the surface, and powder granule is irregular alignment.
The value of the chemical substance material that preparation is used is to determine by the scope that sets in advance, and each value is wanted strict Weighting and Controlling.
The roaster that uses in the preparation process, crucible, drying baker, container, agitator, beaker etc. will keep clean, prevent that harmful substance from getting involved.
Want strict in the preparation process and undertaken, operation according to the order of sequence by technological process.
The product of preparation is: canescence rhodium powder, rhodium content are 99.95%, steady quality.

Claims (4)

1, a kind of method of from waste platinum nets, extracting the rhodium powder, it is characterized in that: the chemical substance material of use is: waste platinum nets, barium peroxide, natrium nitrosum, sodium chloride, hydrochloric acid, nitric acid, sulfuric acid, hydrazine hydrate, ammonium chloride, silver nitrate, NaOH, deionized water, hydrogen, nitrogen, its combination consumption is as follows: with gram, milliliter, centimetre 3Be measurement unit
Waste platinum nets: Pt Rh Pd 10000g ± 10g
Barium peroxide: BaO 2500g ± 10g
Natrium nitrosum: NaNO 2550g ± 10g
Sodium chloride: NaCl 250g ± 10g
Hydrochloric acid: HCl 52000ml ± 100ml
Nitric acid: HNO 313000ml ± 100ml
Sulfuric acid: H 2SO 4200ml ± 10ml
Hydrazine hydrate: N 2H 4H 2O 600ml ± 10ml
NaOH: NaOH 10g ± 1g
Ammonium chloride: NH 4Cl 300g ± 10g
Silver nitrate: AgNO 310g ± 1g
Deionized water: H 2O 30000ml ± 100ml
Hydrogen: H 210000cm 3± 100cm 3
Nitrogen: N 210000cm 3± 100cm 3
Rhodium powder extracting method is as follows:
(1) selected chemical substance material
To carry out selectedly to the chemical substance material that extract to use, and carry out quality purity control:
Waste platinum nets: solid-state solid platinum 92.5%, rhodium 3.5%, palladium 4.0%
Barium peroxide: solid-state solid 99.0%
Inferior sodium nitrate: solid-state solid 99.0%
Sodium chloride: solid-state solid 99.0%
Hydrochloric acid: liquid strength of fluid 20%, 36%
Sulfuric acid: liquid strength of fluid 98%, 10%
Nitric acid: liquid strength of fluid 65%
Sal-ammoniac: solid-state solid 99.5%
Hydrazine hydrate: liquid liquid 64%
NaOH: solid-state solid 99.0%
Silver nitrate: solid-state solid 99.0%
Deionized water:: liquid liquid 99.5%
Hydrogen: gaseous state gas 99.0%
Nitrogen: gaseous state gas 99.0%
(2) mechanical crushing waste platinum nets
Waste platinum nets is placed in the pulverizer, carry out mechanical crushing, become the platinum powder, powder average grain diameter 0.5mm;
(3) mechanical lapping, sieve
Platinum powder after pulverizing is carried out mechanical lapping, and sieve, grind, sieve and carry out repeatedly, become: platinum fine powder, powder diameter≤0.074mm with 100 purpose screen clothes;
(4) preparation chloroazotic acid, dissolving platinum fine powder
With platinum fine powder 10000g, place ceramic vessel, adding concentration is 36% hydrochloric acid 50000ml, 65% nitric acid 12500ml, stirs, and becomes: wang aqueous solution;
Platinum, the dissolving of palladium element, the rhodium element oligodynamical;
(5) filter
Wang aqueous solution is placed on the filtering flask, filter, retain on the filter paper: aqua regia insoluble rhodium slag with one deck middling speed qualitative filter paper;
(6) add the barium peroxide roasting
100g places crucible with aqua regia insoluble rhodium slag, adds barium peroxide 500g then, stirs after the mixing, becomes aqua regia insoluble rhodium slag+barium peroxide mixture;
The crucible that fills aqua regia insoluble slag+barium peroxide mixture is placed roaster, and temperature rises to 900 ℃ ± 5 ℃ by 20 ℃, at this temperature constant temperature, insulation, roasting time 90min ± 2min;
After the roasting, close roaster, make it cool to 20 ℃ with the furnace, become: the aqua oxidation rhodium;
(7) dissolving aqua oxidation rhodium
600g places in the ceramic cylinder with the aqua oxidation rhodium, adds 20% watery hydrochloric acid 1000ml, place then on the electric heater, and 95 ℃ of heating-up temperatures, heat time heating time, 210min ± 5min closed heater then, made it naturally cool to 20 ℃, became: rhodium complex solution, that is: H 3RhCl 6
(8) filter
The rhodium complex solution is placed filter tunnel, filter, retain impurity on the filter paper, in the filter flask be: the rhodium complex solution with three layers of middling speed qualitative filter paper;
(9) precipitate, leave standstill
The rhodium complex solution is placed ceramic vessel, add 10% sulfuric acid 1600ml, leave standstill, precipitate 720min;
(10) cross filtering barium
With the rhodium complex solution that leaves standstill, filter with three layers of middling speed qualitative filter paper, retain barium sulfate BaSO on the filter paper 4Impurity is the rhodium complex solution in the filter flask;
(11) heating, concentrated
The rhodium complex solution is placed beaker, place then on the electric heater, 95 ℃ ± 2 ℃ of heating-up temperatures add sodium chloride 80g, continue heating, add deionized water 2000ml when being pulpous state, make solution concentration reach 45g/L, become: rhodium complex solution Na 3RhCl 6
(12) remove platinum
Add ammonium chloride 15g ± 1g in the rhodium complex solution, stir, the platinum in the solution becomes the ammonium chloroplatinate yellow mercury oxide, sediment after filtration, dry, purify, become: spongy platinum, and removing, retain the rhodium complex liquid;
(13) inferior sodium nitrate complexing
To place ceramic cylinder except that the rhodium complex solution behind the platinum, and add deionized water 1800ml, making solution concentration is 25g/L, and adjusting the pH value with 10% sodium hydroxide solution is 1.5;
Heat temperature raising places ceramic cylinder on the electric heater, and 95 ℃ ± 2 ℃ of heating-up temperatures heat while stirring, and adds 50% sodium nitrite solution 1400ml of preparation in advance then, makes its boiling, boils 60min ± 2min, and making the pH value is 5.5;
Close heater, make it be cooled to 20 ℃ naturally;
Na 3RhCl 6Solution transfers Na to 3Rh (NO 2) 6Solution;
Materials such as Fe, Al, Ca, Zn generate precipitation of hydroxide in the solution;
(14) suction filtration is removed base metals such as Fe, Al, Ca, Zn
Solution is placed Buchner funnel, carry out suction filtration with three layers of middling speed qualitative filter paper, retain base metal Fe, Al, Ca, Zn etc. on the filter paper, filtrate is Na in the filter flask 3Rh (NO 2) 6Solution;
(15) rhodium of cooling precipitation fast
Filtrate is placed the ice bath cylinder, be quickly cooled to 18 ℃, add ammonium chloride 240g, stirring, ageing 30min generate milky six nitroso rhodiums acid ammonium, and precipitation, that is: mixed liquor (NH 4) 3Rh (NO 2) 6↓
(16) vacuum filtration
Mixed liquor is placed on the vacuum filtration bottle, with three layers of middling speed qualitative filter paper suction filtration, retain six nitroso rhodiums acid ammonium on the filter paper, filtrate is the rhodium mother liquor, and the rhodium-containing amount is low in the rhodium mother liquor, and after three circular treatment, the rhodium-containing amount is 0.005%, can discard;
(17) heating for dissolving is removed nitro
Six nitroso rhodiums acid ammonium is placed ceramic cylinder, add 20% hydrochloric acid 2500ml, be heated to 95 ℃, until there not being brown gas HNO 3Overflow, become: chlordene rhodium acid ammonium solution, that is: (NH 4) 3RhCl 6
(18) change sodium salt
When the heating of chlordene rhodium acid ammonium solution is concentrated into 1000ml, slowly add sodium chloride 120g, heating, be stirred to solution in the pasty state the time, divide respectively to add deionized water 200ml three times, be heated to 95 ℃ of evaporations then, remove unnecessary hydrochloric acid, when steaming again to pulpous state, add deionized water 1000ml, become chlordene rhodium acid sodium solution, i.e. Na 3RhCl 6
(19) ion-exchange
With the NaOH that adds 10% in the chlordene rhodium acid sodium solution, regulating the pH value is 1.5, behind cationic ion-exchange resin, remove trace impurity, the chlordene rhodium acid sodium solution of Cheng Chun is then with five flushing washings of deionized water, each water consumption 100ml makes rhodium all enter solution;
(20) hydrazine hydrate reduction
Chlordene rhodium acid sodium solution with behind cation exchange, the deionized water rinsing is heated to 95 ℃ of boilings, drips 64% hydrazine hydrate solution 600ml then, and rate of addition 5ml/min becomes white to solution, till the rhodium powder sinks;
(21) washing, filtration, detection
White solution is added deionized water 100ml, and agitator treating filters with one deck middling speed qualitative filter paper then, and washing, filtration repeat five times, then with till the no white precipitate of 10% silver nitrate check;
(22) vacuum filtration
With three layers of qualitative filter paper suction filtration, retain product on the filter paper, that is: rhodium powder filter cake;
(23) vacuum drying
Place vacuum drying chamber dry rhodium powder filter cake product, vacuum 10Pa, 115 ℃ of baking temperatures, drying time, 180min promptly got product: black rhodium powder after the drying;
(24) rhodium powder roasting, hydrogen reducing
Dried black rhodium powder is placed crucible, place roaster then, use earlier nitrogen flooding removing and harmful gas, nitrogen input speed 40cm 3/ min, roasting reduction under hydrogen shield then, hydrogen input speed 40cm 3/ min, 800 ℃ ± 2 ℃ of sintering temperatures, time 60min ± 2min naturally cools to 20 ℃ ± 3 ℃ then, and behind the roasting reduction, product becomes: canescence rhodium powder;
(25) detect, chemically examine, analyze, characterize
Pattern, color and luster, purity, the rhodium content of canescence rhodium powder to preparation chemically examined, analyzes, characterized;
Carry out constituent content analysis with Atomic Absorption Spectrometer;
Carry out morphology analysis with SEM;
(26) store
Canescence rhodium powder to preparation places water white glass container, is stored in cool place, drying, clean environment, waterproof, protection against the tide, acid-proof alkali salt to corrode, storage temperature≤20 ℃ ± 3 ℃, relative humidity≤10%.
2, a kind of method of from waste platinum nets, extracting the rhodium powder according to claim 1, it is characterized in that: the roasting of described rhodium powder, hydrogen reducing carries out in roaster, the bottom of roaster (1) is base (4), electric heater (3), top is bell (5), inside is furnace chamber (2), ceramic crucible (6) is put in bottom in furnace chamber (2), in ceramic crucible (6) rhodium powder (12), left part at roaster (1) is provided with hydrogen cylinder (9), hydrogen pipe (10), hydrogen valve (11), right upper portion at roaster (1) is provided with pore (13), be provided with nitrogen cylinder (14) in the left outside of roaster (1), nitrogen tube (15), nitrogen valve (16), and UNICOM's furnace chamber (2), remove pernicious gas in the chamber with nitrogen flooding earlier, and then reduce with hydrogen (8).
3, a kind of method of from waste platinum nets, extracting the rhodium powder according to claim 1, it is characterized in that: described rhodium slag+barium peroxide sintering temperature is 900 ℃ ± 2 ℃, roasting time 90min ± 2min; The roasting of rhodium powder, hydrogen reducing temperature are 800 ℃ ± 2 ℃, and the time is 60min ± 2min.
4, a kind of method of extracting the rhodium powder from waste platinum nets according to claim 1, it is characterized in that: the rhodium powder of described extraction is the canescence powder.
CN2009100755886A 2009-09-27 2009-09-27 Method for extracting rhodium powder from waste platinum nets Expired - Fee Related CN101658942B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102586607A (en) * 2012-03-06 2012-07-18 张桂香 Method for extracting platinum, rhodium and palladium from failed platinum alloy gauze
CN105177306A (en) * 2015-09-14 2015-12-23 昆明贵金属研究所 Method for recycling rhodium from sulfuric acid type rhodanized waste liquid
CN112705727A (en) * 2020-12-21 2021-04-27 无锡英特派金属制品有限公司 Preparation method of high-purity rhodium powder
CN112760488A (en) * 2020-12-28 2021-05-07 格林美股份有限公司 Separation method for iron in precious solution leached by automobile exhaust waste catalyst

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102586607A (en) * 2012-03-06 2012-07-18 张桂香 Method for extracting platinum, rhodium and palladium from failed platinum alloy gauze
CN102586607B (en) * 2012-03-06 2013-08-21 张桂香 Method for extracting platinum, rhodium and palladium from failed platinum alloy gauze
CN105177306A (en) * 2015-09-14 2015-12-23 昆明贵金属研究所 Method for recycling rhodium from sulfuric acid type rhodanized waste liquid
CN112705727A (en) * 2020-12-21 2021-04-27 无锡英特派金属制品有限公司 Preparation method of high-purity rhodium powder
CN112760488A (en) * 2020-12-28 2021-05-07 格林美股份有限公司 Separation method for iron in precious solution leached by automobile exhaust waste catalyst

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