CN102703711A - Method for extracting rhenium from rhenium-containing waste liquor - Google Patents
Method for extracting rhenium from rhenium-containing waste liquor Download PDFInfo
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- CN102703711A CN102703711A CN2012102167537A CN201210216753A CN102703711A CN 102703711 A CN102703711 A CN 102703711A CN 2012102167537 A CN2012102167537 A CN 2012102167537A CN 201210216753 A CN201210216753 A CN 201210216753A CN 102703711 A CN102703711 A CN 102703711A
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- rhenium
- waste liquid
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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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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to a method for extracting rhenium from rhenium-containing waste liquor. According to the technical scheme, the method comprises the following steps of: heating the rhenium-containing waste liquor at the temperature of between 20 and 80 DEG C for 30 and 90 minutes; adding brine of which the volume is 1 to 20 percent of that of the waste liquor into the waste liquor; stirring, and cooling to a room temperature; filtering, and heating and evaporating filtrate to remove the most moisture; adding precipitating agents, 5-acetamido-3-(4-acetamido phenyl) azo-4-hydroxy-naphthalene-2, and 7-disulfonic acid disodium salt of which the volume is 1 to 10 percent of that of the filtrate into the residual filtrate, and stirring for 30 minutes; filtering, and inputting excessive ammonia water into filter cakes; stirring for 30 to 90 minutes; filtering, and overnight aging the filtrate; collecting white crystals at the bottom; and drying, and thus obtaining ammonium rhenate products. The method is simple, the enrichment of the rhenium is improved by nearly 100 times, the rhenium is quickly recovered, the recovery rate of the rhenium is more than 90 percent, and the economic benefit, the social benefit and the environmental benefit are obvious.
Description
Technical field
The invention belongs to field of inorganic chemical engineering, relate in particular to the technology of from the rhenium-containing waste liquid, extracting rhenium.
Background technology
The mineral of rhenium have seldom only been found out brightness rhenium ore deposit, molybdenum glance and copper rhenium sulfide mineral so far, and how with micro-association in mineral such as molybdenum, copper, lead, zinc, platinum, niobium.The rhenium-containing mineral of economically valuable are molybdenum glance.The content of rhenium is between 0.001～0.031% in the general brightness concentrated molybdenum ore.When oxidizing roasting brightness concentrated molybdenum ore, produce a large amount of waste liquids, the rhenium resource in the waste liquid is the resource that can not despise.If can the rhenium in the waste liquid be extracted, can bring huge economic benefit, social benefit and environmental benefit.
The existing method of extracting rhenium mainly contains: FSU's cemented carbide works adopts oxidizing roasting-deposition rhenium method, contains Re
2O
7Flue gas gather dust the Re in the flue gas through eluting column and wet electrical dust precipitator
2O
7Water-soluble and generate perrhenic acid, be dissolved in Re
2O
7The aqueous solution in order to the cycling elution flue gas, enrichment is extracted a part of solution concentration out to finite concentration, adds Repone K, reclaims rhenium.The subject matter that exists is that regular meeting produces third phase, and the rhenium recovery is low, is merely 75%.In addition, primary isoamyl alcohol water-soluble big, volatile, the reagent consumption is big, and cost is high, and sends pungent odour.U.S. Kenecott Research Centre adopts oxidizing roasting-ion exchange method to carry rhenium, adopts NH
4SCN replaces dangerous HClO
4, wash rhenium as elutriant, obtain ammonium perrhenate through cooling, crystallization, method is complicated.
Summary of the invention
The object of the present invention is to provide a kind of method simple, the technology of from the rhenium-containing waste liquid, extracting rhenium that the recovery is high.
For realizing above-mentioned purpose, the technical scheme that the present invention adopts is: a kind of method of from the rhenium-containing waste liquid, extracting rhenium: the rhenium-containing waste liquid was heated 30-90 minute down in 20-80 ℃, in waste liquid, add the bittern of waste liquid volume 1%-20% then; Stir, be cooled to room temperature after, filter; After the heating evaporation of will filtrating is removed most of moisture content, in residual filtrate, add precipitation agent 5-acetamido-3-(4-acetamido phenyl) azo-4-hydroxyl naphthalene-2 of filtrate volume 1%-10%, the 7-disulfonic acid disodium salt; Stirred 30 minutes, and filtered, in filter cake, add excess of ammonia water; Stirred 30-90 minute, and filtered, filtrating placement is spent the night; Collect the white crystal of bottom, oven dry gets rehenic acid ammonium product.
The invention has the beneficial effects as follows: the present invention adopts the precipitation agent of bittern as waste liquid, and the rhenium rate of loss is below 7%.Adopt the present invention to reclaim the easy method of having founded that develops for the rhenium of China rare precious metal manufacturing enterprise.The present invention is a raw material with the rhenium-containing waste liquid, through method of the present invention, makes the enrichment of rhenium improve nearly 100 times, has realized the quick recovery of rhenium, and the recovery that realizes rhenium is greater than 90%, economic benefit, social benefit and obvious environment benefit.
Embodiment
1 one kinds of methods of from the rhenium-containing waste liquid, extracting rhenium of embodiment
The rhenium-containing waste liquid that provides with certain A of company is a raw material, in the rhenium-containing waste liquid, and rhenium-containing 0.7 g/L, contaminating metal ion 635g/L.
The rhenium-containing waste liquid was heated 90 minutes down in 20 ℃, add the bittern of waste liquid volume 20% then, to be cooled to room temperature, filter; Remove deposition, after the heating evaporation of will filtrating is removed most of moisture content, in residual filtrate, add precipitation agent 5-acetamido-3-(the 4-acetamido phenyl) azo-4-hydroxyl naphthalene-2 of filtrate volume 10%, the 7-disulfonic acid disodium salt; Mechanical stirring 30 minutes is filtered, and in filter cake, adds excessive ammonia, vigorous stirring 60 minutes; Filter, filtrating placement is spent the night, and collects the white crystal of bottom; Oven dry had both got rehenic acid ammonium product, the recovery 92%.
With gravimetric determination rehenic acid ammonium density is 3.97g/cm
3, conform to the rehenic acid ammonium.Measuring rehenic acid ammonium purity with ICP is 95%.
2 one kinds of methods of from the rhenium-containing waste liquid, extracting rhenium of embodiment
The rhenium-containing waste liquid that provides with certain B of company is a raw material, in the rhenium-containing waste liquid, and rhenium-containing 0.4 g/L, nickeliferous 235g/L contains molybdenum 65g/L, and iron content 268g/L contains zinc 97g/L.
The rhenium-containing waste liquid was heated 60 minutes down in 50 ℃, add the bittern of waste liquid volume 12% then, to be cooled to room temperature, filter; Remove deposition, after the heating evaporation of will filtrating is removed most of moisture content, in residual filtrate, add precipitation agent 5-acetamido-3-(the 4-acetamido phenyl) azo-4-hydroxyl naphthalene-2 of filtrate volume 5%, the 7-disulfonic acid disodium salt; Mechanical stirring 30 minutes is filtered, and in filter cake, adds excessive ammonia, vigorous stirring 30 minutes; Filter, filtrating placement is spent the night, and collects the white crystal of bottom; Oven dry had both got rehenic acid ammonium product, yield 90.8%.
With gravimetric determination rehenic acid ammonium density, be 3.97g/cm
3, conform to the rehenic acid ammonium.Measuring rehenic acid ammonium purity with ICP is 95%.
3 one kinds of methods of from the rhenium-containing waste liquid, extracting rhenium of embodiment
The rhenium-containing waste liquid that provides with certain C of company is a raw material, in the rhenium-containing waste liquid, contains molybdenum 0.5g/L, rhenium-containing 0.3g/L, iron content 3g/L.
The rhenium-containing waste liquid was heated 30 minutes down in 80 ℃, add the bittern of waste liquid volume 1% then, to be cooled to room temperature, filter; Remove deposition, after the heating evaporation of will filtrating is removed most of moisture content, in residual filtrate, add precipitation agent 5-acetamido-3-(the 4-acetamido phenyl) azo-4-hydroxyl naphthalene-2 of filtrate volume 1%, the 7-disulfonic acid disodium salt; Mechanical stirring 30 minutes is filtered, and in filter cake, adds excessive ammonia, vigorous stirring 90 minutes; Filter, filtrating placement is spent the night, and collects the white crystal of bottom; Oven dry had both got rehenic acid ammonium product, yield 95.7%.
With gravimetric determination rehenic acid ammonium density, be 3.97g/cm
3, conform to the rehenic acid ammonium.Measuring rehenic acid ammonium purity with ICP is 95%.
4 one kinds of methods of from the rhenium-containing waste liquid, extracting rhenium of embodiment
The rhenium-containing waste liquid that provides with certain D of company is a raw material, in the rhenium-containing waste liquid, and rhenium-containing 0.3g/L, iron content 121g/L, platiniferous 2 g/L contain aluminium 81g/L.
With rhenium-containing waste liquid heated and boiled 50 minutes, add the bittern of waste liquid volume 3% then, to be cooled to room temperature, filter; Remove deposition, after the heating evaporation of will filtrating removes most of moisture content, in residual filtrate, add precipitation agent 5-acetamido-3-(the 4-acetamido phenyl) azo-4-hydroxyl naphthalene-2 of filtrate volume 4%, the 7-disulfonic acid disodium salt; Mechanical stirring 30 minutes is filtered, and in filtrating, adds excessive ammonia, vigorous stirring 70 minutes; Filter, filtrating placement is spent the night, and collects the white crystal of bottom; Oven dry had both got rehenic acid ammonium product, yield 92.6%.
With gravimetric determination rehenic acid ammonium density, be 3.97g/cm
3, conform to the rehenic acid ammonium.Measuring rehenic acid ammonium purity with ICP is 95%.
Claims (1)
1. a method of from the rhenium-containing waste liquid, extracting rhenium is characterized in that method is following: the rhenium-containing waste liquid was heated 30-90 minute down in 20-80 ℃, in waste liquid, add the bittern of waste liquid volume 1%-20% then, stir; After being cooled to room temperature, filter, after the heating evaporation of will filtrating is removed most of moisture content, in residual filtrate, add precipitation agent 5-acetamido-3-(4-acetamido phenyl) azo-4-hydroxyl naphthalene-2 of filtrate volume 1%-10%; The 7-disulfonic acid disodium salt stirred 30 minutes, filtered, and in filter cake, added excess of ammonia water; Stirred 30-90 minute, and filtered, filtrating placement is spent the night; Collect the white crystal of bottom, oven dry gets rehenic acid ammonium product.
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| CN2012102167537A CN102703711B (en) | 2012-06-28 | 2012-06-28 | Method for extracting rhenium from rhenium-containing waste liquor |
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| CN2012102167537A CN102703711B (en) | 2012-06-28 | 2012-06-28 | Method for extracting rhenium from rhenium-containing waste liquor |
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| CN102703711A true CN102703711A (en) | 2012-10-03 |
| CN102703711B CN102703711B (en) | 2013-12-18 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103553139A (en) * | 2013-11-05 | 2014-02-05 | 辽宁石油化工大学 | Method for separating and recovering rhenium |
| CN103773963A (en) * | 2014-01-28 | 2014-05-07 | 白银有色集团股份有限公司 | Method for efficiently recovering copper and rhenium from copper smelting waste acid |
| CN105074023A (en) * | 2013-04-15 | 2015-11-18 | 国立大学法人九州大学 | Extraction agent for precious metals and rhenium, and extraction method for precious metals and rhenium using same |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3932579A (en) * | 1973-12-06 | 1976-01-13 | Universal Oil Products Company | Recovery of rhenium |
| CN1342779A (en) * | 2000-12-29 | 2002-04-03 | 张方宇 | Process for recovering metals Pt, Re and Al from waste reforming catalyst |
| CN101050489A (en) * | 2007-05-18 | 2007-10-10 | 锦州沈宏集团股份有限公司 | Method for extracting rhenium from eluate of flue ash generated by baking enriched ore of molybdenum |
| JP2010077499A (en) * | 2008-09-26 | 2010-04-08 | Dowa Metals & Mining Co Ltd | Method for treating substance to be treated containing platinum group element, rhenium and arsenic |
| CN102057066A (en) * | 2008-05-06 | 2011-05-11 | 科学设计公司 | Recovery of rhenium |
-
2012
- 2012-06-28 CN CN2012102167537A patent/CN102703711B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3932579A (en) * | 1973-12-06 | 1976-01-13 | Universal Oil Products Company | Recovery of rhenium |
| CN1342779A (en) * | 2000-12-29 | 2002-04-03 | 张方宇 | Process for recovering metals Pt, Re and Al from waste reforming catalyst |
| CN101050489A (en) * | 2007-05-18 | 2007-10-10 | 锦州沈宏集团股份有限公司 | Method for extracting rhenium from eluate of flue ash generated by baking enriched ore of molybdenum |
| CN102057066A (en) * | 2008-05-06 | 2011-05-11 | 科学设计公司 | Recovery of rhenium |
| JP2010077499A (en) * | 2008-09-26 | 2010-04-08 | Dowa Metals & Mining Co Ltd | Method for treating substance to be treated containing platinum group element, rhenium and arsenic |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105074023A (en) * | 2013-04-15 | 2015-11-18 | 国立大学法人九州大学 | Extraction agent for precious metals and rhenium, and extraction method for precious metals and rhenium using same |
| CN105074023B (en) * | 2013-04-15 | 2016-09-14 | 国立大学法人九州大学 | Noble metal and rhenium extractant and use the noble metal of this extractant and the extracting method of rhenium |
| CN103553139A (en) * | 2013-11-05 | 2014-02-05 | 辽宁石油化工大学 | Method for separating and recovering rhenium |
| CN103553139B (en) * | 2013-11-05 | 2015-09-30 | 辽宁石油化工大学 | Be separated and reclaim the method for rhenium |
| CN103773963A (en) * | 2014-01-28 | 2014-05-07 | 白银有色集团股份有限公司 | Method for efficiently recovering copper and rhenium from copper smelting waste acid |
| CN103773963B (en) * | 2014-01-28 | 2015-09-30 | 白银有色集团股份有限公司 | A kind of method of efficient controlled recovery copper rhenium from the dirty acid of Copper making |
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| CN102703711B (en) | 2013-12-18 |
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Address after: Dong Jia Duan high-tech park in Hunan province 412000 Zhuzhou city Lusong District Patentee after: Re in New Material Co. Ltd. Address before: 412000 Hunan city of Zhuzhou province Dong Jia Duan aviation hi tech Park Road No. 3 Patentee before: Zhuzhou Kate High-Tech Materials Co., Ltd. |