CN102703711B - 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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- CN102703711B CN102703711B CN2012102167537A CN201210216753A CN102703711B CN 102703711 B CN102703711 B CN 102703711B CN 2012102167537 A CN2012102167537 A CN 2012102167537A CN 201210216753 A CN201210216753 A CN 201210216753A CN 102703711 B CN102703711 B CN 102703711B
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- rhenium
- filtrate
- 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
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 technique of extracting rhenium from the rhenium-containing waste liquid.
Background technology
The mineral of rhenium seldom, have only been found out brightness rhenium ore deposit, molybdenum glance and copper rhenium sulfide mineral so far, and mainly with micro-association in the mineral such as molybdenum, copper, lead, zinc, platinum, niobium.Rhenium-containing mineral with economic worth are molybdenum glance.In general brightness concentrated molybdenum ore, the content of rhenium is between 0.001～0.031%.When oxidizing roasting brightness concentrated molybdenum ore, produce a large amount of waste liquids, the rhenium resource in waste liquid is the resource that can not despise.If the rhenium in waste liquid is extracted, can bring huge economic benefit, social benefit and environmental benefit.
The existing method of extracting rhenium mainly contains: the USSR (Union of Soviet Socialist Republics) cemented carbide works adopts oxidizing roasting-precipitation rhenium method, containing Re
2o
7flue gas through eluting column and wet electrical dust precipitator, gather dust, the Re in flue gas
2o
7water-soluble and generate perrhenic acid, be dissolved in Re
2o
7the aqueous solution in order to the cycling elution flue gas, be enriched to finite concentration, extract a part of solution out concentrated, add Repone K, reclaim rhenium.The subject matter existed is often can produce third phase, and the rhenium rate of recovery is low, is only 75%.In addition, primary isoamyl alcohol water-soluble large, volatile, the reagent consumption is large, 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, the method complexity.
Summary of the invention
The object of the present invention is to provide a kind of method simple, the technique of extracting rhenium from the rhenium-containing waste liquid that the rate of recovery is high.
For achieving the above object, the technical solution used in the present invention is: a kind of method of extracting rhenium from the rhenium-containing waste liquid: the rhenium-containing waste liquid is heated under 20-80 ℃ to 30-90 minute, then to the bittern that adds waste liquid volume 1%-20% in waste liquid, stir, after being cooled to room temperature, filter, after the filtrate heating evaporation is removed to most of moisture content, to precipitation agent 5-acetamido-3-(the 4-acetamido phenyl) azo that adds filtrate volume 1%-10% in residual filtrate-4-hydroxyl naphthalene-2, the 7-disulfonic acid disodium salt, stir 30 minutes, filter, add excess of ammonia water in filter cake, stir 30-90 minute, filter, filtrate placement is spent the night, collect the white crystal of bottom, dry, obtain 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 rhenium that the present invention is China rare precious metal manufacturing enterprise to reclaim the easy method of having founded that develops.The present invention be take the rhenium-containing waste liquid as raw material, by method of the present invention, makes the enrichment of rhenium improve nearly 100 times, has realized the quick recovery of rhenium, realizes that the rate of recovery of rhenium is greater than 90%, economic benefit, social benefit and obvious environment benefit.
Embodiment
1 one kinds of methods of extracting rhenium from the rhenium-containing waste liquid of embodiment
The rhenium-containing waste liquid that certain A of company provides of take is 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 is heated 90 minutes under 20 ℃, then the bittern that adds waste liquid volume 20%, to be cooled to room temperature, filter, remove precipitation, after the filtrate heating evaporation is removed to most of moisture content, to precipitation agent 5-acetamido-3-(the 4-acetamido phenyl) azo that adds filtrate volume 10% in residual filtrate-4-hydroxyl naphthalene-2, the 7-disulfonic acid disodium salt, mechanical stirring 30 minutes, filter, add excessive ammonia in filter cake, vigorous stirring 60 minutes, filter, filtrate placement is spent the night, collect the white crystal of bottom, dry, both obtained rehenic acid ammonium product, the rate of recovery 92%.
The gravimetric determination rehenic acid ammonium density of take is 3.97g/cm
3, with the rehenic acid ammonium, conform to.It is 95% that the ICP of take measures rehenic acid ammonium purity.
2 one kinds of methods of extracting rhenium from the rhenium-containing waste liquid of embodiment
The rhenium-containing waste liquid that certain B of company provides of take is raw material, in the rhenium-containing waste liquid, and rhenium-containing 0.4 g/L, nickeliferous 235g/L, containing molybdenum 65g/L, iron content 268g/L, containing zinc 97g/L.
The rhenium-containing waste liquid is heated 60 minutes under 50 ℃, then the bittern that adds waste liquid volume 12%, to be cooled to room temperature, filter, remove precipitation, after the filtrate heating evaporation is removed to most of moisture content, to precipitation agent 5-acetamido-3-(the 4-acetamido phenyl) azo that adds filtrate volume 5% in residual filtrate-4-hydroxyl naphthalene-2, the 7-disulfonic acid disodium salt, mechanical stirring 30 minutes, filter, add excessive ammonia in filter cake, vigorous stirring 30 minutes, filter, and filtrate placement is spent the night, collect the white crystal of bottom, dry, both obtained rehenic acid ammonium product, yield 90.8%.
With gravimetric determination rehenic acid ammonium density, be 3.97g/cm
3, with the rehenic acid ammonium, conform to.It is 95% that the ICP of take measures rehenic acid ammonium purity.
3 one kinds of methods of extracting rhenium from the rhenium-containing waste liquid of embodiment
The rhenium-containing waste liquid that certain C of company provides of take is raw material, in the rhenium-containing waste liquid, and containing molybdenum 0.5g/L, rhenium-containing 0.3g/L, iron content 3g/L.
The rhenium-containing waste liquid is heated 30 minutes under 80 ℃, then the bittern that adds waste liquid volume 1%, to be cooled to room temperature, filter, remove precipitation, after the filtrate heating evaporation is removed to most of moisture content, to precipitation agent 5-acetamido-3-(the 4-acetamido phenyl) azo that adds filtrate volume 1% in residual filtrate-4-hydroxyl naphthalene-2, the 7-disulfonic acid disodium salt, mechanical stirring 30 minutes, filter, add excessive ammonia in filter cake, vigorous stirring 90 minutes, filter, and filtrate placement is spent the night, collect the white crystal of bottom, dry, both obtained rehenic acid ammonium product, yield 95.7%.
With gravimetric determination rehenic acid ammonium density, be 3.97g/cm
3, with the rehenic acid ammonium, conform to.It is 95% that the ICP of take measures rehenic acid ammonium purity.
4 one kinds of methods of extracting rhenium from the rhenium-containing waste liquid of embodiment
The rhenium-containing waste liquid that certain D of company provides of take is raw material, in the rhenium-containing waste liquid, and rhenium-containing 0.3g/L, iron content 121g/L, platiniferous 2 g/L, containing aluminium 81g/L.
By rhenium-containing waste liquid heated and boiled 50 minutes, then the bittern that adds waste liquid volume 3%, to be cooled to room temperature, filter, remove precipitation, after the filtrate heating evaporation is removed to most of moisture content, to precipitation agent 5-acetamido-3-(the 4-acetamido phenyl) azo that adds filtrate volume 4% in residual filtrate-4-hydroxyl naphthalene-2, the 7-disulfonic acid disodium salt, mechanical stirring 30 minutes, filter, add excessive ammonia in filtrate, vigorous stirring 70 minutes, filter, and filtrate placement is spent the night, collect the white crystal of bottom, dry, both obtained rehenic acid ammonium product, yield 92.6%.
With gravimetric determination rehenic acid ammonium density, be 3.97g/cm
3, with the rehenic acid ammonium, conform to.It is 95% that the ICP of take measures rehenic acid ammonium purity.
Claims (1)
1. a method of extracting rhenium from the rhenium-containing waste liquid, it is characterized in that method is as follows: the rhenium-containing waste liquid is heated under 20-80 ℃ to 30-90 minute, then to the bittern that adds waste liquid volume 1%-20% in waste liquid, stir, after being cooled to room temperature, filter, after the filtrate heating evaporation is removed to most of moisture content, to precipitation agent 5-acetamido-3-(the 4-acetamido phenyl) azo that adds filtrate volume 1%-10% in residual filtrate-4-hydroxyl naphthalene-2, the 7-disulfonic acid disodium salt, stir 30 minutes, filter, add excess of ammonia water in filter cake, stir 30-90 minute, filter, filtrate placement is spent the night, collect the white crystal of bottom, dry, obtain 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 CN102703711A (en) | 2012-10-03 |
| CN102703711B true CN102703711B (en) | 2013-12-18 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9435006B2 (en) * | 2013-04-15 | 2016-09-06 | Kyushu University, National University Corporation | Extraction agent for precious metals and rhenium, and extraction method for precious metals and rhenium using same |
| CN103553139B (en) * | 2013-11-05 | 2015-09-30 | 辽宁石油化工大学 | Be separated and reclaim the method for rhenium |
| 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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| 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 |
| CN100420761C (en) * | 2007-05-18 | 2008-09-24 | 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 |
| US7763096B2 (en) * | 2008-05-06 | 2010-07-27 | Sd Lizenzverwertungsgesellschaft Mbh & Co. Kg | Recovery of rhenium |
| JP5355977B2 (en) * | 2008-09-26 | 2013-11-27 | Ｄｏｗａメタルマイン株式会社 | Method for treating materials containing platinum group elements, rhenium and arsenic |
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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. |