CN109136533A - The method that quick separating extracts ruthenium from low content waste material containing ruthenium - Google Patents
The method that quick separating extracts ruthenium from low content waste material containing ruthenium Download PDFInfo
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- CN109136533A CN109136533A CN201811221967.7A CN201811221967A CN109136533A CN 109136533 A CN109136533 A CN 109136533A CN 201811221967 A CN201811221967 A CN 201811221967A CN 109136533 A CN109136533 A CN 109136533A
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- ruthenium
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/005—Preliminary treatment of scrap
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
- C01G55/005—Halides
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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
- C22B11/042—Recovery of noble metals from waste materials
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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
- C22B11/06—Chloridising
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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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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- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
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- Environmental & Geological Engineering (AREA)
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- Geochemistry & Mineralogy (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The method that the invention discloses a kind of to separate ruthenium from low content waste material containing ruthenium is soaked in water using low content secondary resource containing ruthenium as raw material, and dispersing agent is added and stirs evenly, filtration washing；Slag after scattered is put into reaction kettle, hydrochloric acid is added, heating stirring leads to chlorine reaction for a period of time after reaching temperature, has reacted rear and has stopped reaction.Filtering, solution alkaline chemical precipitation, oxidation distillation obtain product ruthenium trichloride.Feature of the present invention is that process flow is simple, and low energy consumption, and efficiency is fast, ruthenium high income, clean and environmental protection.
Description
Technical field
The invention belongs to technical field of noble metal metallurgy, and in particular to a kind of side that ruthenium is separated from low content waste material containing ruthenium
Method.
Background technique
Ruthenium is that one kind is hard and crisp in grayish multivalence yttrium, has chemical catalysis activity and good conduction
Performance is widely used in field of fine chemical and hard disc of computer sputtering target material, and wherein ruthenium trichloride is ruthenium most importantization
One of object is closed, is the important industrial chemicals in the fields such as heterogeneous catalysis, homogeneous catalysis, coating, plating.
Ruthenium in traditional separation and Extraction low content waste material containing ruthenium extracts ruthenium using dissolution carrier enrichment ruthenium or directly melting,
Concentration method generates the three wastes, not environmentally, long flow path, and and the directly melting method time is long, low efficiency.
Summary of the invention
The problem of present invention mainly solves the time of separation and Extraction ruthenium in the prior art length, low efficiency provides a kind of clear
The method of the separation and Extraction ruthenium of clean environmental protection, ruthenium leaching rate is high, and yield is up to 99% or more.
The technical solution adopted by the present invention is that:
The method that ruthenium is separated from low content waste material containing ruthenium, the method comprising the steps of:
(1) low content waste material containing ruthenium is taken, is soaked in water, dispersing agent is added and stirs evenly, filters, obtains scattered slag
Material；
(2) hydrochloric acid is added into above-mentioned scattered slag charge, heating stirring is passed through chlorine reaction；
(3) discharging and filtering after step (2) has been reacted, solution alkaline chemical precipitation；
(4) after precipitating, oxidation distillation extracts ruthenium, is prepared into ruthenium trichloride product.
Wherein, the above-mentioned method that ruthenium is separated from low content waste material containing ruthenium, dispersing agent barium stearate described in step (1),
At least one of zinc stearate and polyethylene glycol.The dosage of the dispersing agent is the 1.0-1.8% of the quality of waste material containing ruthenium, such as
1.2-1.5%.
Wherein, the above-mentioned method that ruthenium is separated from low content waste material containing ruthenium, the time of stirring described in step (1) are 15-
30 minutes.
Wherein, the above-mentioned method that ruthenium is separated from low content waste material containing ruthenium, the solid-liquid of slag charge and hydrochloric acid described in step (2)
It is 1:1-3 than (g/mL).
Wherein, the above-mentioned method that ruthenium is separated from low content waste material containing ruthenium, the concentration of hydrochloric acid described in step (2) are 4-
9mol/L, such as 5-8mol/L, preferably 8mol/L.
Wherein, the above-mentioned method that ruthenium is separated from low content waste material containing ruthenium, the temperature of reaction described in step (2) are 60-
100 DEG C, such as 70-90 DEG C, preferably 75 DEG C；The time of reaction is 0.5-1.5h, such as 1h.
Wherein, the above-mentioned method that ruthenium is separated from low content waste material containing ruthenium, alkali described in step (3) can be hydroxide
At least one of sodium, potassium hydroxide, sodium bicarbonate, sodium carbonate, saleratus, potassium carbonate etc., preferably sodium hydroxide, it is described
The mass fraction of alkali is 15-45%.
Wherein, the above-mentioned method that ruthenium is separated from low content waste material containing ruthenium, oxidation distillation described in step (4) extract ruthenium
Condition are as follows: the NaOH solution that mass fraction is 10-40% is added in negative pressure under air-tight state, is heated to 50-80 DEG C, is passed through
Chlorine controls reaction temperature at 80-105 DEG C, generates the RuO of yellow4Gas is passed through in multistage absorption by Hydrochloric Acid liquid, salt through negative pressure
For sour absorbing liquid constant temperature to 15-25 DEG C, reaction generates brownish red H2RuCl5Solution.
The present invention provides a kind of methods of rapid cleaning separation and Extraction ruthenium, and simple process, low energy consumption, oxidation distillation raffinate
Neutralization is discharged into neutralization precipitation pond, and this method ruthenium high income has the advantages that low-consumption high-efficiency environmental protection.
Specific embodiment
Further detailed description is done to technical solution of the present invention below in conjunction with specific embodiment.The following example
It is merely illustrative the ground description and interpretation present invention, and is not necessarily to be construed as limiting the scope of the invention.It is all to be based on this hair
In the range of the technology that bright above content is realized is encompassed by the present invention is directed to protect.
Unless otherwise indicated, raw materials and reagents used in the following embodiment are commercial goods, or can be by
Perception method preparation.
Embodiment 1
The 10kg of waste material containing ruthenium is weighed, 15L water is added and impregnates, the polyethylene glycol for being added 1.2% stirs evenly dispersion 20 minutes, mistake
The hydrochloric acid of 30L 6mol/L is added into 50L reaction kettle for filter, and scattered ruthenium waste material, heating stirring is added, and temperature reaches 65
DEG C, start logical chlorine reaction, react 1 hour, discharging and filtering, the alkali neutralization of mass fraction 15% is added in solution.
The NaOH solution that mass fraction is 10% is added in negative pressure under air-tight state, is heated to 60 DEG C, is passed through chlorine,
Reaction temperature is controlled at 95 DEG C, generates the RuO of yellow4Gas is passed through in multistage absorption by Hydrochloric Acid liquid through negative pressure, and absorption by Hydrochloric Acid liquid is permanent
For temperature to 25 DEG C, reaction generates brownish red H2RuCl5Solution, analysis ruthenium content is 0.08% in slag, ruthenium yield 99.1%.
Embodiment 2
The 10kg of waste material containing ruthenium is weighed, 15L water is added and impregnates, the zinc stearate for being added 1.5% stirs evenly dispersion 20 minutes, mistake
The hydrochloric acid of 30L 8mol/L is added into 50L reaction kettle for filter, and scattered ruthenium waste material, heating stirring is added, and temperature reaches 65
DEG C, start logical chlorine reaction, react 1 hour, discharging and filtering, the alkali neutralization of mass fraction 20% is added in solution.
The NaOH solution that mass fraction is 20% is added in negative pressure under air-tight state, is heated to 80 DEG C, is passed through chlorine,
Reaction temperature is controlled at 105 DEG C, generates the RuO of yellow4Gas is passed through in multistage absorption by Hydrochloric Acid liquid, absorption by Hydrochloric Acid liquid through negative pressure
For constant temperature to 25 DEG C, reaction generates brownish red H2RuCl5Solution, analysis ruthenium content is 0.01% in slag, ruthenium yield 99.3.
Embodiment 3
The 10kg of waste material containing ruthenium is weighed, 15L water is added and impregnates, the polyethylene glycol for being added 1.2% stirs evenly dispersion 20 minutes, mistake
The hydrochloric acid of 30L6mol/L is added into 50L reaction kettle for filter, and scattered ruthenium waste material, heating stirring is added, and temperature reaches 80 DEG C,
Start logical chlorine reaction, react 1 hour, discharging and filtering, the alkali neutralization of mass fraction 30% is added in solution.
The NaOH solution that mass fraction is 30% is added in negative pressure under air-tight state, is heated to 70 DEG C, is passed through chlorine,
Reaction temperature is controlled at 100 DEG C, generates the RuO of yellow4Gas is passed through in multistage absorption by Hydrochloric Acid liquid, absorption by Hydrochloric Acid liquid through negative pressure
For constant temperature to 25 DEG C, reaction generates brownish red H2RuCl5Solution, analysis ruthenium content is 0.006% in slag, ruthenium yield 99.8%.
Embodiment 4
The 15kg of waste material containing ruthenium is weighed, 25L water is added and impregnates, the polyethylene glycol for being added 1.2% stirs evenly dispersion 30 minutes, mistake
The hydrochloric acid of 40L6mol/L is added into 50L reaction kettle for filter, and scattered ruthenium waste material, heating stirring is added, and temperature reaches 80 DEG C,
Start logical chlorine reaction, react 1 hour, discharging and filtering, the alkali neutralization of mass fraction 45% is added in solution.
The NaOH solution that mass fraction is 25% is added in negative pressure under air-tight state, is heated to 75 DEG C, is passed through chlorine,
Reaction temperature is controlled at 95 DEG C, generates the RuO of yellow4Gas is passed through in multistage absorption by Hydrochloric Acid liquid through negative pressure, and absorption by Hydrochloric Acid liquid is permanent
For temperature to 25 DEG C, reaction generates brownish red H2RuCl5Solution, analysis ruthenium content is 0.02% in slag, ruthenium yield 98.5%.
More than, embodiments of the present invention are illustrated.But the present invention is not limited to above embodiment.It is all
Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done should be included in guarantor of the invention
Within the scope of shield.
Claims (10)
1. separating the method for ruthenium from low content waste material containing ruthenium, which is characterized in that the method comprising the steps of:
(1) low content waste material containing ruthenium is taken, is soaked in water, dispersing agent is added and stirs evenly, filters, obtains scattered slag charge；
(2) hydrochloric acid is added into above-mentioned scattered slag charge, heating stirring is passed through chlorine reaction；
(3) discharging and filtering after step (2) has been reacted, solution alkaline chemical precipitation；
(4) after precipitating, oxidation distillation extracts ruthenium, is prepared into ruthenium trichloride product.
2. the method according to claim 1 for separating ruthenium from low content waste material containing ruthenium, which is characterized in that in step (1)
At least one of the dispersing agent barium stearate, zinc stearate and polyethylene glycol.
3. the method according to claim 1 for separating ruthenium from low content waste material containing ruthenium, which is characterized in that the dispersing agent
Dosage be the quality of waste material containing ruthenium 1.0-1.8%.
4. the method according to claim 1 for separating ruthenium from low content waste material containing ruthenium, which is characterized in that in step (1)
The time of the stirring is 15-30 minutes.
5. the method according to claim 1 for separating ruthenium from low content waste material containing ruthenium, which is characterized in that in step (2)
The solid-to-liquid ratio (g/mL) of the slag charge and hydrochloric acid is 1:1-3.
6. the method according to claim 1 for separating ruthenium from low content waste material containing ruthenium, which is characterized in that in step (2)
The concentration of the hydrochloric acid is 4-9mol/L.
7. the method according to claim 1 for separating ruthenium from low content waste material containing ruthenium, which is characterized in that in step (2)
The temperature of the reaction is 60-100 DEG C, and the time of reaction is 0.5-1.5h.
8. the method according to claim 1 for separating ruthenium from low content waste material containing ruthenium, which is characterized in that in step (3)
The alkali can be at least one of sodium hydroxide, potassium hydroxide, sodium bicarbonate, sodium carbonate, saleratus, potassium carbonate etc..
9. the method according to claim 1 for separating ruthenium from low content waste material containing ruthenium, which is characterized in that the matter of the alkali
Amount score is 15-45%.
10. the method according to claim 1 for separating ruthenium from low content waste material containing ruthenium, which is characterized in that in step (4)
The oxidation distillation extracts the condition of ruthenium are as follows: the NaOH solution that mass fraction is 10-40% is added in negative pressure under air-tight state, adds
Heat is warming up to 50-80 DEG C, is passed through chlorine, controls reaction temperature at 80-105 DEG C, generates the RuO of yellow4Gas is passed through through negative pressure
In multistage absorption by Hydrochloric Acid liquid, for absorption by Hydrochloric Acid liquid constant temperature to 15-25 DEG C, reaction generates brownish red H2RuCl5Solution.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811221967.7A CN109136533A (en) | 2018-10-19 | 2018-10-19 | The method that quick separating extracts ruthenium from low content waste material containing ruthenium |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811221967.7A CN109136533A (en) | 2018-10-19 | 2018-10-19 | The method that quick separating extracts ruthenium from low content waste material containing ruthenium |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110423896A (en) * | 2019-08-13 | 2019-11-08 | 江苏理工学院 | A method of ruthenium trichloride in recycling plating ruthenium waste liquid |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103626240A (en) * | 2013-12-15 | 2014-03-12 | 郴州高鑫铂业有限公司 | Method for preparing ruthenium trichloride with low-concentration complicated ruthenium-containing waste liquid |
-
2018
- 2018-10-19 CN CN201811221967.7A patent/CN109136533A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103626240A (en) * | 2013-12-15 | 2014-03-12 | 郴州高鑫铂业有限公司 | Method for preparing ruthenium trichloride with low-concentration complicated ruthenium-containing waste liquid |
Non-Patent Citations (1)
| Title |
|---|
| 黄礼煌: "《贵金属提取新技术》", 30 November 2016, 冶金工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110423896A (en) * | 2019-08-13 | 2019-11-08 | 江苏理工学院 | A method of ruthenium trichloride in recycling plating ruthenium waste liquid |
| CN110423896B (en) * | 2019-08-13 | 2021-11-16 | 江苏理工学院 | Method for recovering ruthenium trichloride from ruthenium plating waste liquid |
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Address after: 423000 wanhuayan industrial community, Beihu District, group 11, leidaqiao village, Baohe Town, Beihu District, Chenzhou City, Hunan Province Applicant after: Hunan Gaoxin platinum industry Co.,Ltd. Applicant after: CHENZHOU GAOXIN MATERIAL Co.,Ltd. Address before: 423000 wanhuayan industrial community, Beihu District, group 11, leidaqiao village, Baohe Town, Beihu District, Chenzhou City, Hunan Province Applicant before: CHENZHOU GAOXIN PLATINUM Co.,Ltd. Applicant before: CHENZHOU GAOXIN MATERIAL Co.,Ltd. |
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Application publication date: 20190104 |