CN103215454A - Rhodium reduction activation dissolution method - Google Patents
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Abstract
The invention discloses a rhodium reduction activation dissolution method, and relates to the technical field of noble metal metallurgy. The rhodium reduction activation dissolution method can be used for overcoming the defects of the prior art and aims at achieving a rhodium dissolution method which has the advantages of high dissolution efficiency, wet method normal-pressure dissolution, easiness for operation, short process flow, low production cost and wide rhodium waste dissolution range. The technical scheme is as follows: the rhodium reduction activation dissolution method comprises the following steps of: A, crushing and grinding rhodium wastes; B, mixing with an activating agent; C, carrying out acid-soluble activation; D, filtering; and E, dissolving. According to the invention, because zinc powder and a hydrochloric acid solution generate chemical reaction in the step C to generate H2, rhodium oxide contained in the solution can be reduced into metal rhodium through H2 at 100 DEG C, the dissolution activity of rhodium can not be reduced and can be enhanced so as to be favorable to subsequent dissolution, and the rhodium oxide is reduced into the metal rhodium without being dissolved by hydrochloric acid in the activated process. Thus, the rhodium reduction activation dissolution method disclosed by the invention has the advantages of high rhodium dissolution efficiency, rhodium normal-pressure dissolution, low dissolution temperature, easiness for operation, short process flow, low production cost and wide rhodium waste dissolution range.
Description
Technical field
The present invention relates to the precious metals metallurgy technical field, particularly a kind of dissolved method of rhodium.
Background technology
Platinum metals fusing point height, intensity are big, electric heating is stable, anti-electrical spark lose height, erosion resistance is good, high-temperature oxidation resistance is strong, catalytic activity is good, be widely used in fields such as purifying vehicle exhaust, chemical industry, aerospace, glass industry, electronics and electrical industry, though consumption is few, but play keying action, have the title of " industrial VITAMIN ".In six platinum family elements, the rhodium price is once the most expensive, reaches 2,500,000 yuan/kilogram, and price volalility is big, and the chemical property of rhodium in solution is very complicated, in the refining process, be placed on last recovery usually, so the production cycle is longer, and commercial risks is also bigger.The dissolving of rhodium and refining are that the difficult problem in refining and the chemical analysis is extracted in the platinum metals always.
80%～90% rhodium with the form of compound (as RhCl
3NH
2O, Rh
2(SO
4)
3, Rh (NO
3)
3, RhI
3, Rh (OA
c)
x, RhH (CO) (PPh
3)
3Deng) being applied to cleaning catalyst for tail gases of automobiles, jewellery rhodanizing, medicine and petrochemical industry catalyzer, rhodium must be converted into the basic compound of rhodium earlier, is reprocessed into coated material, rhodanizing liquid, organic rhodium compound etc.The dissolving of rhodium is the prerequisite of using, and the dissolving of the recovery of rhodium and the more too busy to get away rhodium of purifying, so the dissolving technology of rhodium is extremely important.
Take diverse ways dissolving according to content, existence, the active difference of rhodium, roughly can be divided into: 1. chemistry of aqueous solution dissolution method, 2. in warm scorification, 3. high melt method, 4. electrochemical solution.
Can be oxidized to rhodium oxide because of melting, roasting rhodium in the rhodium waste material in collection process, rhodium oxide is difficult to must be reduced into metal rhodium to rhodium oxide by chemical agent dissolves before the dissolving.600～800 ℃ of logical hydrogen reducings of being everlasting, because the reduction temperature height, rhodium can sintering under hot conditions, the active reduction, solute effect is poor.
For the higher material of rhodium content, the normal pressure dissolving not exclusively can be strengthened dissolving by pressurization.The dissolved under pressure method originates from tube sealing dissolving technology and the microwave dissolving technology in the rhodium analysis.In airtight container, add thermogenesis pressure, quicken the dissolving of rhodium.Hydrochloric acid corrosion resistance is very strong under the high pressure, and existing pressure exerting device is difficult to the erosion of opposing hydrochloric acid, does not also have the report of suitability for industrialized production in this France.
Chinese patent CN101319278A(application number 200810058706.8) the rapidly-soluble method of a kind of high-purity rhodium material is disclosed, precious metal indissoluble rhodium material mixed with acid solution and oxygenant to size mixing according to a certain percentage place special pressurized vessel, controlled temperature is at 160～300 ℃, oxygen partial pressure is 0～3.0MPA, reaction times is 1～8 hour, under High Temperature High Pressure the Noble Metal Rhodium material is dissolved fast and obtain acid rhodium solution, dissolution rate is greater than 98%, and yield is greater than 99%.
Chinese patent CN101476044 has announced a kind of method of handling Pt-Rh binary alloy net aqua regia insoluble slag (rhodium content is 30%～80%) with the barium peroxide scorification.Detailed process is: with the abundant mixing of barium peroxide of aqua regia insoluble slag and 4～6 times of amounts, be warming up to 800 ℃～950 ℃, constant temperature for some time, make rhodium be converted into acid-soluble compound.But this method can be introduced a large amount of barium impurity, brings difficulty, SO for the separation purification of rhodium
4 2-Precipitation is removed in the process of barium, and precipitation is carried secretly, the absorbed portion rhodium, has reduced the rate of recovery of rhodium, and therefore domestic only have minority producer to use.
The fragmentation method is mainly used in the dissolving of rhodium content than higher platinum rhodium (as PtRh20, PtRh30) and rhodium ingot.Chinese patent application number (87105623.2) application number (90104468.7) has been announced a kind of method of fragmentation dissolving rhodium, under hot conditions, material is with the fusion of base metal aluminum or aluminum alloy, form alloy, then with acid dissolving base metal, just obtain active very high Powdered rhodium powder, water chloride solution dissolving again.
Chinese patent CN1136595 has announced a kind of method with sulfonium capture-aluminothermy active dissolution rhodium, and this method is applicable to the enrichment and the dissolving of the material that platinum metals content is lower.Base metal sulfide (FeS, Ni
2S
3, CuS etc.) to the avidity of platinum metals the platinum metals is enriched in the sulfonium, and base metal oxide MgO, Al
2O
3, CaO, Fe
2O
3, SiO
2Stay slag mutually in, the platinum metals is effectively separated with base metal oxide, and obtains enrichment.Adopt the aluminothermy activating technology again, use the dissolving with hydrochloric acid base metal, the platinum metals is further separated with base metal, obtain active high platinum metals powder, dissolve with the aqueous solution chlorination method.
Electrochemical solution is usually used in dissolving pure rhodium powder, produces the compound R hCl of rhodium
3NH
2O.Generally be in the concentrated hydrochloric acid medium, dissolve rhodium with alternating-current.Dissolution rate and current density, material table area, electrolyte concentration, temperature are relevant.Chinese patent CN101100756A, Chinese patent CN101503220A adopt electrochemical process dissolving rhodium, the preparation Trichlororhodium, and dissolution rate reaches 99.95%.The advantage of electrochemical solution is that dissolution process is not introduced new impurity, and electrolytic solution can directly enter the postorder refinery practice, and shortcoming is that dissolution rate is slow.
Summary of the invention
The present invention overcomes the deficiencies in the prior art, and a kind of dissolved efficiency height, wet method normal pressure dissolving, simple to operate are provided, and technical process is short, manufacturing cost is low, can dissolve the wide rhodium reduction activation dissolving method of rhodium waste material scope.
For achieving the above object, the technology used in the present invention solution comprises following processing step:
A, rhodium waste material pulverizing and jevigating: with rhodium content greater than 10% rhodium waste material pulverizing and jevigating, to granularity be 200～400 orders, the rhodium waste material after broken, optimum condition is: particle size after cracking is 280～320 orders.
B and activator mix: rhodium waste material and granularity after the fragmentation that steps A is made are that 200～300 purpose zinc powders are even by 1:1～10 thorough mixing, must activate powder mix, and optimum condition is: rhodium waste material and zinc powder weight ratio are 1:2～4.
C, sour molten activation: adding concentration in an airtight reactor is the hydrochloric acid of 10～12mol/L, and activation powder mix liquid-solid ratio (L/S)=1～10:1 that hydrochloric acid and step B make is under 60～100 ℃ the condition in temperature; Add the activation powder mix that step B makes while stirring, stirring velocity is 80～200 rev/mins, reacts 40～80 minutes; Optimum condition is: activation powder mix liquid-solid ratio (L/S)=4～10:1 that hydrochloric acid and step B make is under 85～90 ℃ the condition in temperature; Add the activation powder mix that step B makes while stirring, stirring velocity is 110～130 rev/mins, reacts 55～65 minutes.
Wherein L/S is that the meaning of liquid-solid ratio is the meaning of liquid volume than solid weight.
D, filtration: the solution after step C reaction finished filter filter residue, filter residue is with the hot wash of 8～12 times 75～85 ℃ of filter residues 1～5 time, the rhodium material of reduction activation.
E, dissolving: the rhodium material of the reduction activation that step D is made is put into glass reactor, 10～15% concentration that add rhodium material weight earlier are the hydrochloric acid of 10～12mol/L, 3～10 times of concentration that add rhodium material weight again are 95～98% the vitriol oil, dissolved 4～8 hours under 140～200 ℃ of conditions of temperature, cold filtration obtains the rhodium sulfate sulphuric acid soln; Optimum condition is: 5～8 times of concentration that add rhodium material weight are 95～98% the vitriol oil, dissolve 5～7 hours under 160～180 ℃ of conditions of temperature.
Beneficial effect of the present invention:
Zinc powder and hydrochloric acid soln generation chemical reaction in the C step of the present invention generate H
2, under 60～100 ℃, H
2Can be reduced to metal rhodium to the rhodium oxide in the solution, the lytic activity of rhodium can not reduce, and can improve, and is very beneficial for follow-up dissolving like this, and rhodium oxide is reduced into metal rhodium in the reactivation process, not by dissolving with hydrochloric acid.Other base metal and oxide compound major part thereof are not reduced into activated metal by the base metal oxidation of dissolving with hydrochloric acid by dissolving with hydrochloric acid, further by dissolving with hydrochloric acid, improve the content of rhodium in the reduction activation rhodium waste material greatly, and the separation that helps the postorder rhodium is purified.Rhodium material with reduction activation in the step e adopts hydrochloric acid+concentrated sulfuric acid dissolution, adds hydrochloric acid earlier, and hydrochloric acid is solubility promoter, can quicken the dissolving of rhodium, and 95% rhodium is generated the rhodium sulfate sulphuric acid soln by sulfuric acid dissolution in the rhodium waste material.So the present invention owing to having above advantage aggregate performance is: one, the dissolved efficiency height of rhodium; Two, normal pressure dissolving rhodium and solvent temperature are low, simple to operate; Three, technical process is short, and manufacturing cost is low; Four, it is wide to dissolve rhodium waste material scope.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Embodiment
Embodiment 1
A, rhodium waste material pulverizing and jevigating: platinum catalysis net aqua regia insoluble slag 100 grams that will give up, rhodium content is 82.23%, rhodium 82.23 grams are used the grinder pulverizing and jevigating, cross 300 mesh sieves.
B and activator mix: rhodium waste material after the fragmentation that steps A is made and 300 grams, 200 purpose zinc powder thorough mixing are even.
C, sour molten activation: in the reactor of an airtight 2L glass, add technical hydrochloric acid 800ml earlier, concentration of hydrochloric acid is 10mol/L, adds compound while stirring, 120 rev/mins of stirring velocitys, and reaction rises to 95 ℃, is incubated 60 minutes.
D, filtration: the solution after step C reaction finished filter filter residue, filter residue is with the hot wash of 8 times 75 ℃ of filter residues 3 times, the rhodium material of reduction activation.
E, dissolving: the rhodium material that step D is made reduction activation is put into glass reactor, adds 12mol/L hydrochloric acid 15ml earlier, and the back adds 98% vitriol oil 500ml, and heating for dissolving is warming up to 160 ℃, airtight backflow dissolving 6 hours, and cold filtration gets the rhodium sulfate sulphuric acid soln; Analyze rhodium sulfate sulphuric acid soln rhodium-containing 76.5 grams, 93.04% rhodium is generated the rhodium sulfate sulphuric acid soln by sulfuric acid dissolution.
Embodiment 2:
A, rhodium waste material pulverizing and jevigating: organic rhodium waste material is burnt slag 100 grams, and rhodium content is 18.67%, and rhodium-containing 18.67 grams are used the grinder pulverizing and jevigating, cross 280 mesh sieves.
B and activator mix: rhodium waste material after the fragmentation that steps A is made and 200 grams, 250 purpose zinc powder thorough mixing are even.
C, sour molten activation: in the reactor of an airtight 2L glass, add technical hydrochloric acid 500ml earlier, concentration of hydrochloric acid is 12mol/L, adds compound while stirring, 80 rev/mins of stirring velocitys, and reaction rises to 60 ℃, is incubated 80 minutes.
D, filtration: the solution after step C reaction finished overanxious filter residue, filter residue is with the hot wash of 12 times 85 ℃ of filter residues 2 times, the rhodium material of reduction activation.
E, dissolving: the rhodium material of the reduction activation that step D is made is put into glass reactor, add 12mol/L hydrochloric acid 3ml earlier, the back adds 98% vitriol oil 200ml, heating for dissolving, be warming up to 200 ℃, airtight backflow dissolving 4 hours, cold filtration, analyze rhodium sulfate sulphuric acid soln rhodium-containing 18.04 grams, 96.6% rhodium is generated the rhodium sulfate sulphuric acid soln by sulfuric acid dissolution.
Embodiment 3:
A, rhodium waste material pulverizing and jevigating: with thick rhodium powder 100 grams, content 98.10%, rhodium-containing 98.1 grams are used the grinder pulverizing and jevigating, cross 200 mesh sieves.
B and activator mix: rhodium waste material after the fragmentation that steps A is made and 500 grams, 300 purpose zinc powder thorough mixing are even.
C, sour molten activation: in the reactor of an airtight 3L glass, add technical hydrochloric acid 1000ml earlier, concentration of hydrochloric acid is 11mol/L, adds compound while stirring, 80 rev/mins of stirring velocitys, and reaction rises to 80 ℃, is incubated 40 minutes.
D, filtration: the solution after step C reaction finished filter filter residue, filter residue is with the hot wash of 10 times 80 ℃ of filter residues 1 time, the rhodium material of reduction activation.
E, dissolving: the rhodium material of the reduction activation that step D is made is put into glass reactor, adds 12mol/L hydrochloric acid 20ml earlier, and the back adds 98% vitriol oil 1000ml, heating for dissolving, be warming up to 140 ℃, airtight backflow dissolving 8 hours, cold filtration gets the rhodium sulfate sulphuric acid soln; Analyze rhodium sulfate sulphuric acid soln rhodium-containing 93.26 grams, 95.1% rhodium is generated the rhodium sulfate sulphuric acid soln by sulfuric acid dissolution.
Embodiment 4:
A, rhodium waste material pulverizing and jevigating: organic rhodium waste liquid is burnt slag 2000 grams, content 18.67%, rhodium-containing 373.4 grams are used the grinder pulverizing and jevigating, cross 400 mesh sieves.
B and activator mix: rhodium waste material after the fragmentation that steps A is made and 2000 grams, 250 purpose zinc powder thorough mixing are even.
C, sour molten activation: in the reactor of an airtight 20L glass, add technical hydrochloric acid 12L earlier, concentration of hydrochloric acid is 10mol/L, adds compound while stirring, 80 rev/mins of stirring velocitys, and reaction rises to 95 ℃, is incubated 90 minutes.
D, filtration: the solution after step C reaction finished filter filter residue, filter residue is with the hot wash of 12 times 75 ℃ of filter residues 5 times, the rhodium material of reduction activation.
E, dissolving: the rhodium material of the reduction activation that step D is made is put into glass reactor, add 10mol/L hydrochloric acid 200ml earlier, the back adds 95% vitriol oil 12l, heating for dissolving, be warming up to 160 ℃, airtight backflow dissolving 8 hours, cold filtration gets the rhodium sulfate sulphuric acid soln, analyze rhodium sulfate sulphuric acid soln rhodium-containing 358.64 grams, 96.05% rhodium is generated the rhodium sulfate sulphuric acid soln by sulfuric acid dissolution.
Claims (7)
1. rhodium reduction activation dissolving method, technical scheme is as follows:
A, rhodium waste material pulverizing and jevigating: with rhodium content greater than 10% rhodium waste material pulverizing and jevigating, to granularity be 200～400 orders, the rhodium waste material after broken;
B and activator mix: rhodium waste material and granularity after the fragmentation that steps A is made are that 200～300 purpose zinc powders are even by 1:1～10 thorough mixing, must activate powder mix;
C, sour molten activation: adding concentration in an airtight reactor is the hydrochloric acid of 10～12mol/L, activation powder mix liquid-solid ratio (L/S)=1～10:1 that hydrochloric acid and step B make, be under 60～100 ℃ the condition in temperature, add the activation powder mix that step B makes while stirring, stirring velocity is 80～200 rev/mins, reacts 40～80 minutes;
D, filtration: the solution after step C reaction finished filter filter residue, filter residue is with the hot wash of 8～12 times 75～85 ℃ of filter residues 1～5 time, the rhodium material of reduction activation;
E, dissolving: the rhodium material of the reduction activation that step D is made is put into glass reactor, 10～15% concentration that add rhodium material weight earlier are the hydrochloric acid of 10～12mol/L, 3～10 times of concentration that add rhodium material weight again are 95～98% the vitriol oil, dissolved 4～8 hours under 140～200 ℃ of conditions of temperature, cold filtration obtains the rhodium sulfate sulphuric acid soln.
2. rhodium reduction activation dissolving method according to claim 1 is characterized in that, described steps A is changed into rhodium waste material pulverizing and jevigating: with rhodium content greater than 10% rhodium waste material pulverizing and jevigating, to granularity be 280～320 orders, the rhodium waste material after broken.
3. rhodium reduction activation dissolving method according to claim 1, it is characterized in that, to change and activator mix among the described step B into: rhodium waste material and granularity after the fragmentation that steps A is made are that 200～300 purpose zinc powders are even by 1:2～4 thorough mixing, must activate powder mix.
4. rhodium reduction activation dissolving method according to claim 2, it is characterized in that, to change and activator mix among the described step B into: rhodium waste material and granularity after the fragmentation that steps A is made are that 200～300 purpose zinc powders are even by 1:2～4 thorough mixing, must activate powder mix.
5. according to the rhodium reduction activation dissolving method of claim 1,2,3,4 described in each, it is characterized in that, described step C is changed into, the molten activation of acid: adding concentration in an airtight reactor is the hydrochloric acid of 10～12mol/L, activation powder mix liquid-solid ratio (L/S)=4～10:1 that hydrochloric acid and step B make is under 85～90 ℃ the condition, to add the activation powder mix that step B makes while stirring in temperature, stirring velocity is 110～130 rev/mins, reacts 55～65 minutes;
6. according to the rhodium reduction activation dissolving method of claim 1,2,3,4 described in each, it is characterized in that, described step e is changed into, dissolving: the rhodium material of the reduction activation that step D is made is put into glass reactor, 10～15% concentration that add rhodium material weight earlier are the hydrochloric acid of 10～12mol/L, 5～8 times of concentration that add rhodium material weight again are 95～98% the vitriol oil, dissolve 5～7 hours under 160～180 ℃ of conditions of temperature, and cold filtration obtains the rhodium sulfate sulphuric acid soln.
7. rhodium reduction activation dissolving method according to claim 5, it is characterized in that, described step e is changed into, dissolving: the rhodium material of the reduction activation that step D is made is put into glass reactor, 10～15% concentration that add rhodium material weight earlier are the hydrochloric acid of 10～12mol/L, 5～8 times of concentration that add rhodium material weight again are 95～98% the vitriol oil, dissolve 5～7 hours under 160～180 ℃ of conditions of temperature, and cold filtration obtains the rhodium sulfate sulphuric acid soln.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103526033A (en) * | 2013-10-21 | 2014-01-22 | 昆明贵研催化剂有限责任公司 | Method for dissolving platinum group metals in automobile spent catalyst enrichment |
| CN110724822A (en) * | 2019-11-27 | 2020-01-24 | 北京科技大学 | Method for recovering platinum group metals by trapping-crushing iron-based alloy |
| CN113087027A (en) * | 2021-04-14 | 2021-07-09 | 成都光明派特贵金属有限公司 | Rhodium powder dissolving method |
| CN114525499A (en) * | 2022-01-11 | 2022-05-24 | 胜宏科技（惠州）股份有限公司 | Carrier rhodium activating solution and preparation method thereof |
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| CN101319278A (en) * | 2008-07-21 | 2008-12-10 | 昆明贵金属研究所 | Quick dissolution method for high-purity rhodium material |
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2013
- 2013-04-09 CN CN201310120933.XA patent/CN103215454B/en active Active
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| CN1048238A (en) * | 1990-06-14 | 1991-01-02 | 中国有色金属工业总公司昆明贵金属研究所 | The fragmentation dissolving methof of precious metal |
| CN101319278A (en) * | 2008-07-21 | 2008-12-10 | 昆明贵金属研究所 | Quick dissolution method for high-purity rhodium material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103526033A (en) * | 2013-10-21 | 2014-01-22 | 昆明贵研催化剂有限责任公司 | Method for dissolving platinum group metals in automobile spent catalyst enrichment |
| CN110724822A (en) * | 2019-11-27 | 2020-01-24 | 北京科技大学 | Method for recovering platinum group metals by trapping-crushing iron-based alloy |
| CN110724822B (en) * | 2019-11-27 | 2020-10-23 | 北京科技大学 | Method for recovering platinum group metals by trapping-crushing iron-based alloy |
| CN113087027A (en) * | 2021-04-14 | 2021-07-09 | 成都光明派特贵金属有限公司 | Rhodium powder dissolving method |
| CN114525499A (en) * | 2022-01-11 | 2022-05-24 | 胜宏科技（惠州）股份有限公司 | Carrier rhodium activating solution and preparation method thereof |
| CN114525499B (en) * | 2022-01-11 | 2023-11-17 | 胜宏科技（惠州）股份有限公司 | Rhodium activating solution for carrier plate and preparation method thereof |
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