CN114686693A - Method for recovering ruthenium from ruthenium-containing material - Google Patents
Method for recovering ruthenium from ruthenium-containing material Download PDFInfo
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- CN114686693A CN114686693A CN202210234662.XA CN202210234662A CN114686693A CN 114686693 A CN114686693 A CN 114686693A CN 202210234662 A CN202210234662 A CN 202210234662A CN 114686693 A CN114686693 A CN 114686693A
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- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 229910052707 ruthenium Inorganic materials 0.000 title claims abstract description 108
- 239000000463 material Substances 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 75
- 238000010521 absorption reaction Methods 0.000 claims abstract description 55
- 239000002253 acid Substances 0.000 claims abstract description 28
- 239000002893 slag Substances 0.000 claims abstract description 16
- 229910019891 RuCl3 Inorganic materials 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- HYHCSLBZRBJJCH-UHFFFAOYSA-M sodium hydrosulfide Chemical compound [Na+].[SH-] HYHCSLBZRBJJCH-UHFFFAOYSA-M 0.000 claims abstract description 10
- 238000004821 distillation Methods 0.000 claims abstract description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 8
- 239000001257 hydrogen Substances 0.000 claims abstract description 8
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 57
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 56
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 23
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 10
- 230000001376 precipitating effect Effects 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000004537 pulping Methods 0.000 claims description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 2
- 239000011707 mineral Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000007800 oxidant agent Substances 0.000 abstract description 5
- 230000001590 oxidative effect Effects 0.000 abstract description 5
- 238000001556 precipitation Methods 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 238000011112 process operation Methods 0.000 abstract description 2
- 238000004073 vulcanization Methods 0.000 abstract description 2
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 abstract 1
- 229910000104 sodium hydride Inorganic materials 0.000 abstract 1
- 239000012312 sodium hydride Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 238000002156 mixing Methods 0.000 description 4
- 238000007865 diluting Methods 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229910001927 ruthenium tetroxide Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/02—Obtaining noble metals by dry processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/12—Dry methods smelting of sulfides or formation of mattes by gases
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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
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Abstract
The invention discloses a method for recovering ruthenium from ruthenium-containing materials, which comprises the steps of slurrying the ruthenium-containing materials to form feed liquid, distilling the feed liquid under the action of a strong oxidant, absorbing the feed liquid by acid absorption liquid to obtain primary ruthenium absorption liquid, adjusting acidity of the primary ruthenium absorption liquid, adding sodium hydrosulfide solution to precipitate to obtain ruthenium slag, dissolving the ruthenium slag in acid, adding an oxidant to the mixture, heating the mixture to perform secondary distillation, absorbing the mixture by the acid absorption liquid to obtain secondary ruthenium absorption liquid, and concentrating and crystallizing the secondary ruthenium absorption liquid to obtain RuCl3，RuCl3And calcining and hydrogen reducing to obtain ruthenium black, washing the ruthenium black, and drying to obtain ruthenium powder. The invention adds sulfurThe sodium hydride solution can greatly shorten the time of vulcanization and precipitation, and improve the production efficiency and the metal yield; the ruthenium is thoroughly sulfurized and precipitated, and the purity of the obtained ruthenium powder is more than 99.95 percent; the process operation is quick, the labor intensity is low, the operation efficiency is high, and the production cost is low.
Description
Technical Field
The invention belongs to the technical field of wet-process treatment of ruthenium-rich materials, and particularly relates to a method for recovering ruthenium from ruthenium-containing materials.
Background
At present, the ruthenium in ruthenium-containing materials is mainly recovered by wet treatment in China, and the main process is to firstly add strong oxidant into the slurried ruthenium-containing materials to oxidize the ruthenium in the feed liquid into RuO4And volatilizing from the feed liquid at high temperature, and absorbing by acid absorption liquid in an absorption device to obtain primary ruthenium absorption liquid. Adding Na after the acidity of the primary ruthenium absorption liquid is adjusted2S is precipitated, secondary oxidation distillation is carried out by adopting a selective distillation process, and RuCl is prepared by concentrating and crystallizing ruthenium secondary absorption liquid3，RuCl3Calcining according to a set program, reducing by hydrogen to obtain ruthenium black, washing the ruthenium black to be neutral by pure water, and drying in a tubular furnace to obtain ruthenium powder. However, Na is utilized in the process2The S precipitation method has low precipitation efficiency, restricts the production operation efficiency, and affects the yield index, and in order to solve the problem, the development of a method for efficiently recovering ruthenium from ruthenium-containing materials is very important.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for efficiently recovering ruthenium from ruthenium-containing materials, so that the precipitation efficiency and yield index of ruthenium are improved, the operation is quick, the operation efficiency is high, the labor intensity is low, and the production cost is low.
The purpose of the invention is realized by the following technical scheme:
a method for recovering ruthenium from ruthenium-containing materials comprises the steps of slurrying the ruthenium-containing materials to form feed liquid, distilling the feed liquid under the action of a strong oxidant, absorbing the feed liquid by an acid absorption liquid to obtain a primary ruthenium absorption liquid, adjusting acidity of the primary ruthenium absorption liquid, adding a sodium hydrosulfide solution to precipitate to obtain ruthenium slag, adding an oxidant to the ruthenium slag after the ruthenium slag is dissolved in the acid, heating the mixture to perform secondary distillation, absorbing the ruthenium slag by the acid absorption liquid to obtain a secondary ruthenium absorption liquid, and concentrating and crystallizing the secondary ruthenium absorption liquid to obtain RuCl3，RuCl3Calcining and hydrogen reducing to obtainRuthenium black is obtained, the ruthenium black is washed and dried to obtain ruthenium powder, and the method specifically comprises the following steps:
(1) pulping a ruthenium-containing material by sulfuric acid to form a feed liquid, adding a sodium chlorate solution, distilling at 90-95 ℃, and absorbing by an acid absorption liquid to obtain a primary ruthenium absorption liquid; the solid-to-liquid ratio of the ruthenium-containing mineral to the sulfuric acid is 1g: 5-6 mL.
(2) Adjusting the pH value of the primary ruthenium absorption liquid to 5-6, adding a sodium hydrosulfide solution until the pH value reaches 7-8, and precipitating after the reaction is finished to obtain ruthenium slag;
(3) dissolving ruthenium slag in sulfuric acid, controlling the solid-to-liquid ratio to be 1g: 4-5 mL, adding a sodium chlorate solution, heating to 90-95 ℃, carrying out secondary distillation, absorbing by an acid absorption solution to obtain a secondary ruthenium absorption solution, and concentrating and crystallizing the secondary ruthenium absorption solution to obtain RuCl3，RuCl3And calcining and hydrogen reducing to obtain ruthenium black, washing the ruthenium black to be neutral by using pure water, and drying to obtain ruthenium powder.
In the steps (1) and (3), the acid absorption solution is a mixed solution of a hydrochloric acid solution and absolute ethyl alcohol, and the mass fraction of HCl in the hydrochloric acid solution is 30%; in the mixed solution of the hydrochloric acid solution and the absolute ethyl alcohol, the mass fraction of the absolute ethyl alcohol is 2 percent.
In the steps (1) and (3), the mass fraction of the sodium chlorate solution is 35%; the rate of addition of sodium chlorate solution was 2L/h. The invention has the following advantages:
(1) the sodium hydrosulfide solution is added, so that the vulcanization and precipitation time is greatly shortened, and the production efficiency and the metal yield are improved;
(2) the ruthenium is thoroughly sulfurized and precipitated, and the purity of the obtained ruthenium powder is more than 99.95 percent;
(3) the invention has the advantages of quick process operation, low labor intensity, high operation efficiency and low production cost.
Drawings
FIG. 1 is a schematic process flow diagram of a process for recovering ruthenium from a ruthenium-containing material.
Detailed Description
The invention is further illustrated by the following examples:
example 1
(1) Mixing ruthenium-containing materials and sulfuric acid according to the proportion of 1g: pulping at a solid-to-liquid ratio of 5-6 mL to form a feed liquid, adding a 35% sodium chlorate solution at a rate of 2L/h, distilling at a high temperature of 93 ℃, and absorbing by an acid absorption liquid to obtain a primary ruthenium absorption liquid; wherein the acid absorption liquid is a mixed liquid of hydrochloric acid solution and absolute ethyl alcohol, and the mass fraction of HCl in the hydrochloric acid solution is 30%; in the mixed solution of the hydrochloric acid solution and the absolute ethyl alcohol, the mass fraction of the absolute ethyl alcohol is 2 percent.
(2) And (3) pumping the primary ruthenium absorption liquid into a 500L kettle for heating and concentrating, adjusting the pH of the ruthenium concentrated liquid to be 5-6, adding a sodium hydrosulfide solution, taking the addition of the sodium hydrosulfide solution as the standard that the reaction pH value reaches 7-8, precipitating to obtain ruthenium slag, and cleaning with pure water and draining.
(3) Dissolving ruthenium slag by adding a proper amount of sulfuric acid, controlling the solid-to-liquid ratio to be 1g: 4-5 mL, adding a sodium chlorate solution with the mass fraction of 35% at the speed of 2L/h, heating to 91 ℃ for secondary distillation, absorbing by an acid absorption liquid to obtain a secondary ruthenium absorption liquid, concentrating the secondary ruthenium absorption liquid, diluting by adding pure water, concentrating to remove acid, drying and crystallizing to obtain RuCl3，RuCl3Ruthenium black is obtained through calcination and hydrogen reduction, the ruthenium black is washed by pure water until the pH is =6.5, and ruthenium powder with the purity of more than 99.96 percent is obtained after drying in a tubular furnace. Wherein the acid absorption liquid is a mixed liquid of hydrochloric acid solution and absolute ethyl alcohol, and the mass fraction of HCl in the hydrochloric acid solution is 30%; in the mixed solution of the hydrochloric acid solution and the absolute ethyl alcohol, the mass fraction of the absolute ethyl alcohol is 2 percent.
Example 2
(1) Mixing ruthenium-containing materials and sulfuric acid according to the proportion of 1g: slurrying at a solid-to-liquid ratio of 5-6 mL to form a feed liquid, adding a 35% sodium chlorate solution at a rate of 2L/h, distilling at a high temperature of 94 ℃, and absorbing by an acid absorption liquid to obtain a primary ruthenium absorption liquid; wherein the acid absorption liquid is a mixed liquid of hydrochloric acid solution and absolute ethyl alcohol, and the mass fraction of HCl in the hydrochloric acid solution is 30%; in the mixed solution of the hydrochloric acid solution and the absolute ethyl alcohol, the mass fraction of the absolute ethyl alcohol is 2 percent.
(2) And (3) pumping the primary ruthenium absorption liquid into a 500L kettle for heating and concentrating, adjusting the pH of the ruthenium concentrated liquid to be 5-6, adding a sodium hydrosulfide solution, taking the addition of the sodium hydrosulfide solution as the standard when the reaction pH value reaches 7-8, precipitating to obtain ruthenium slag, and cleaning with pure water and draining.
(3) Adding a proper amount of sulfuric acid into ruthenium slag for dissolving, controlling the solid-to-liquid ratio to be 1g: 4-5 mL, adding sodium chlorate with the mass fraction of 35% at the speed of 2L/h, heating to 92 ℃ for secondary distillation, absorbing by using acid absorption liquid to obtain secondary ruthenium absorption liquid, concentrating the secondary ruthenium absorption liquid, adding pure water for diluting, concentrating to remove acid, drying and crystallizing to obtain RuCl3，RuCl3Ruthenium black is obtained through calcination and hydrogen reduction, the ruthenium black is washed by pure water until the pH is =6, and ruthenium powder with the purity of more than 99.95 percent is obtained after drying in a tubular furnace. Wherein the acid absorption liquid is a mixed liquid of hydrochloric acid solution and absolute ethyl alcohol, and the mass fraction of HCl in the hydrochloric acid solution is 30%; in the mixed solution of the hydrochloric acid solution and the absolute ethyl alcohol, the mass fraction of the absolute ethyl alcohol is 2 percent.
Example 3
(1) Mixing ruthenium-containing materials and sulfuric acid according to the proportion of 1g: pulping at a solid-to-liquid ratio of 5-6 mL to form a feed liquid, adding a 35% sodium chlorate solution at a rate of 2L/h, distilling at a high temperature of 92 ℃, and absorbing by an acid absorption liquid to obtain a primary ruthenium absorption liquid; wherein the acid absorption liquid is a mixed liquid of hydrochloric acid solution and absolute ethyl alcohol, and the mass fraction of HCl in the hydrochloric acid solution is 30%; in the mixed solution of the hydrochloric acid solution and the absolute ethyl alcohol, the mass fraction of the absolute ethyl alcohol is 2 percent.
(2) And (3) pumping the primary ruthenium absorption liquid into a 500L kettle, heating and concentrating, adjusting the pH of the ruthenium concentrated liquid to be 5-6, adding a sodium hydrosulfide solution, precipitating to obtain ruthenium slag, and washing and draining with pure water.
(3) Dissolving ruthenium slag by adding a proper amount of sulfuric acid, controlling the solid-to-liquid ratio to be 1g: 4-5 mL, adding a 35% sodium chlorate solution at the speed of 2L/h, heating to 93 ℃, carrying out secondary distillation, absorbing by using an acid absorption solution to obtain a secondary ruthenium absorption solution, concentrating the secondary ruthenium absorption solution, diluting by adding pure water, concentrating to remove acid, drying and crystallizing to obtain RuCl3，RuCl3Ruthenium black is obtained through calcination and hydrogen reduction, the ruthenium black is washed by pure water until the pH is =7, and ruthenium powder with the purity of more than 99.97 percent is obtained after drying in a tubular furnace. Wherein the acid absorption liquid is a mixed liquid of hydrochloric acid solution and absolute ethyl alcohol, and the mass fraction of HCl in the hydrochloric acid solution is 30%; mixing of hydrochloric acid solution with absolute ethyl alcoholIn the mixed solution, the mass fraction of the absolute ethyl alcohol is 2 percent.
The embodiment is successfully applied to the recovery of ruthenium in ruthenium-containing materials, and the ruthenium powder with the purity of more than 99.95 percent is produced and meets the quality standard YS/T682-2008 of the ruthenium powder industry.
Claims (4)
1. A process for recovering ruthenium from a ruthenium-containing feed comprising the steps of:
(1) pulping a ruthenium-containing material by sulfuric acid to form a feed liquid, adding a sodium chlorate solution, distilling at 90-95 ℃, and absorbing by an acid absorption liquid to obtain a primary ruthenium absorption liquid;
(2) adjusting the pH value of the primary ruthenium absorption liquid to 5-6, adding a sodium hydrosulfide solution until the pH value reaches 7-8, and precipitating after the reaction is finished to obtain ruthenium slag;
(3) dissolving ruthenium slag in sulfuric acid, controlling the solid-to-liquid ratio to be 1g: 4-5 mL, adding a sodium chlorate solution, heating to 90-95 ℃, carrying out secondary distillation, absorbing by an acid absorption solution to obtain a secondary ruthenium absorption solution, and concentrating and crystallizing the secondary ruthenium absorption solution to obtain RuCl3，RuCl3And calcining and hydrogen reducing to obtain ruthenium black, washing the ruthenium black, and drying to obtain ruthenium powder.
2. The process according to claim 1, wherein the ruthenium-containing material is a ruthenium-containing material, and the process comprises the steps of: in the step (1), the solid-to-liquid ratio of the ruthenium-containing mineral to the sulfuric acid is 1g: 5-6 mL.
3. The method of claim 1 for recovering ruthenium from a ruthenium-containing feed comprising: in the steps (1) and (3), the acid absorption solution is a mixed solution of a hydrochloric acid solution and absolute ethyl alcohol, and the mass fraction of HCl in the hydrochloric acid solution is 30%; in the mixed solution of the hydrochloric acid solution and the absolute ethyl alcohol, the mass fraction of the absolute ethyl alcohol is 2 percent.
4. The method of claim 1 for recovering ruthenium from a ruthenium-containing feed comprising: in the steps (1) and (3), the mass fraction of the sodium chlorate solution is 35%; the rate of addition of sodium chlorate solution was 2L/h.
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Citations (6)
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| CN101797649A (en) * | 2010-01-19 | 2010-08-11 | 兰州大学 | Method and device for preparing high-purity ruthenium |
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| CN205205206U (en) * | 2015-11-18 | 2016-05-04 | 金川集团股份有限公司 | Novel device of ruthenium is drawed in distillation |
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- 2022-03-10 CN CN202210234662.XA patent/CN114686693B/en active Active
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| JP2012167367A (en) * | 2011-01-28 | 2012-09-06 | Mitsubishi Materials Corp | Recovery method of platinum group metal |
| JP2013112857A (en) * | 2011-11-29 | 2013-06-10 | Jx Nippon Mining & Metals Corp | Method of recovering iridium |
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| CN205205206U (en) * | 2015-11-18 | 2016-05-04 | 金川集团股份有限公司 | Novel device of ruthenium is drawed in distillation |
| CN109055738A (en) * | 2018-08-27 | 2018-12-21 | 浙江特力再生资源有限公司 | Noble metal recoverying and utilizing method in a kind of osmium iridium ruthenium mine |
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| Title |
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