CN102703737B - Method for extracting and separating rhenium from rhenium-containing slag - Google Patents
Method for extracting and separating rhenium from rhenium-containing slag Download PDFInfo
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- CN102703737B CN102703737B CN2012102167518A CN201210216751A CN102703737B CN 102703737 B CN102703737 B CN 102703737B CN 2012102167518 A CN2012102167518 A CN 2012102167518A CN 201210216751 A CN201210216751 A CN 201210216751A CN 102703737 B CN102703737 B CN 102703737B
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Abstract
The invention relates to a method for extracting and separating rhenium from rhenium-containing slag. According to the technical scheme, the method comprises the following steps of: adding acid solvent of which the volume is 10 times as that of the rhenium-containing slag into rhenium-containing slag; heating material liquid at the temperature of between 60 and 80 DEG C for 60 to 90 minutes after dissolving the rhenium-containing slag; adding sodium hydroxide of which the weight is 1 to 10 percent of that the material liquid in to the material liquid; cooling to a room temperature, filtering, and heating and evaporating filtrate to remove the most moisture; adding precipitating agents, aniline blue and aniline black, of which the weight is 1 to 5 percent of the residual filtrate into the residual filtrate, and stirring for 30 minutes; filtering, and inputting hydrogen sulfide into the filtrate; and stirring, overnight aging, collecting precipitate at the bottom, and thus obtaining rhenium products. The method is simple, the rhenium is quickly recovered, the recovery rate of the rhenium is more than 80 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 extraction separation rhenium from rhenium-containing material slag.
Background technology
Social now, along with the continuous exploitation of resource, the mineral products of former primary state have been on the verge of exhaustion, and people put into sight the exploitation of some rare precious metal secondary resources more, namely extract rare precious metal from waste residue, waste liquid, dust.
The mineral of rhenium have seldom only been found out brightness rhenium ore deposit, molybdenum glance and copper rhenium sulfide mineral (CuReS so far
4), 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.But can reach 0.16% from the concentrated molybdenum ore rhenium-containing that porphyry copper is selected.The main raw material of producing rhenium is the byproduct of molybdenum smelting process.Smelting smoke dust and the slag of some copper mine, platinum family ore deposit, niobium minerals even zink sulphide and the waste liquid of handling low-grade molybdenum ore can reclaim rhenium.
Rhenium and molybdenum symbiosis are in molybdenum glance.When oxidizing roasting brightness concentrated molybdenum ore, produce a large amount of waste residues, the rhenium resource in the waste residue also is the resource that can not despise.Rhenium in the waste residue if can be extracted, can bring huge economic benefit, social benefit and environmental benefit.The extraction and separation method of existing rhenium mainly contains extraction process and ion exchange method, the method complexity.
Summary of the invention
The object of the present invention is to provide a kind of method simple, the method for extraction separation rhenium from rhenium-containing material slag that the rate of recovery is high.
The technical solution used in the present invention is for achieving the above object: a kind of from rhenium-containing material slag the method for extraction separation rhenium: the sour solvent that adds 10 times of volumes in the rhenium-containing material slag, after the dissolving, feed liquid was heated 60-90 minute down in 60-80 ℃, the sodium hydroxide that adds feed liquid weight 1%-10% then, after being cooled to room temperature, filter, after the filtrate heating evaporation removed most of moisture content, add the precipitation agent aniline blue black of filtrate weight 1%-5% in the residual filtrate, stirred 30 minutes, filter, feed hydrogen sulfide in filtrate, stir, placement is spent the night, collect the precipitation of bottom, be the rhenium product.
Above-mentioned a kind of from rhenium-containing material slag the method for extraction separation rhenium: described sour solvent is nitric acid and the 5% sulfuric acid mixed solution of 1:1-3 by volume.
The invention has the beneficial effects as follows: the present invention adopts sodium hydroxide as the precipitation agent of rhenium-containing material slag, and the rhenium rate of loss is below 5%.Adopt the present invention to reclaim the easy method of having founded that develops for the rhenium of China rare metal manufacturing enterprise.The present invention is raw material with rhenium-containing material slag, by method of the present invention, has realized the quick recovery of rhenium, realizes the rate of recovery of rhenium greater than 90%, economic benefit, social benefit and obvious environment benefit.
Embodiment
Embodiment 1A kind of from rhenium-containing material slag the method for extraction separation rhenium
The rhenium-containing material slag that the roasting brightness concentrated molybdenum ore that provides with certain A of company produces is raw material, in rhenium-containing material slag, and rhenium-containing 0.065%, the contaminating metal ion amounts to 43.5%.
The sour solvent (nitric acid and 5% sulfuric acid is the mixed solution of 1:1 by volume) that adds 10 times of volumes in the rhenium-containing material slag, after waiting to expect the most of dissolving of slag, feed liquid was heated 60 minutes down in 60 ℃, the sodium hydroxide that adds feed liquid weight 10% then, to be cooled to room temperature, filter, remove precipitation, the filtrate heating evaporation is removed most of moisture content after, the precipitation agent aniline blue black that adds filtrate weight 5% again in the residual filtrate, mechanical stirring 30 minutes is filtered, and feeds hydrogen sulfide in filtrate, vigorous stirring 60 minutes, placement is spent the night, and collects the precipitation of bottom, is the rhenium-containing product.
With content and the foreign matter content of ICP mensuration rhenium, the result contains a small amount of sodium, potassium for the rate of recovery of rhenium is 85% in the rhenium product, the salt of ammonium, and the metal in the material slag is removed substantially.
Embodiment 2A kind of from rhenium-containing material slag the method for extraction separation rhenium
The rhenium-containing material slag that produces with certain B of company roasting brightness concentrated molybdenum ore is raw material, in rhenium-containing material slag, and rhenium-containing 0.014%, nickeliferous 6.5%, iron content 72.4% contains zinc 18.9%.
The sour solvent (nitric acid and 5% sulfuric acid is the mixed solution of 1:2 by volume) that adds 10 times of volumes in the rhenium-containing material slag, after waiting to expect the most of dissolving of slag, feed liquid was heated 90 minutes down in 70 ℃, the sodium hydroxide that adds feed liquid weight 5% then, to be cooled to room temperature, filter, remove precipitation, the filtrate heating evaporation is removed most of moisture content after, the precipitation agent aniline blue black that adds filtrate weight 4% again in the residual filtrate, mechanical stirring 30 minutes is filtered, and feeds hydrogen sulfide in filtrate, vigorous stirring 60 minutes, placement is spent the night, and collects the precipitation of bottom, is the rhenium product.
With content and the foreign matter content of ICP mensuration rhenium, the result contains a small amount of sodium, potassium for the rate of recovery of rhenium is 88% in the rhenium product, the salt of ammonium, and the metal in the material slag is removed substantially.
Embodiment 3A kind of from rhenium-containing material slag the method for extraction separation rhenium
The rhenium-containing material slag that provides with certain C of company is raw material, and in rhenium-containing material slag, rhenium-containing 0.033% contains molybdenum 0.04%, iron content 45.5%.
The sour solvent (nitric acid and 5% sulfuric acid is the mixed solution of 1:3 by volume) that adds 10 times of volumes in the rhenium-containing material slag, after waiting to expect the most of dissolving of slag, feed liquid was heated 60 minutes down in 80 ℃, the sodium hydroxide that adds feed liquid weight 1% then, to be cooled to room temperature, filter, remove precipitation, the filtrate heating evaporation is removed most of moisture content after, the precipitation agent aniline blue black that adds filtrate weight 2% again in the residual filtrate, mechanical stirring 30 minutes is filtered, and feeds hydrogen sulfide in filtrate, vigorous stirring 60 minutes, placement is spent the night, and collects the precipitation of bottom, is the rhenium product.
With content and the foreign matter content of ICP mensuration rhenium, the result contains a small amount of sodium, potassium for the rate of recovery of rhenium is 89% in the rhenium product, the salt of ammonium, and the metal in the material slag is removed substantially.
Embodiment 4A kind of from rhenium-containing material slag the method for extraction separation rhenium
The rhenium-containing material slag that provides with certain D of company is raw material, in rhenium-containing material slag, and rhenium-containing 0.011%, iron content 9.8%, platiniferous 2.1% contains aluminium 85.4%.
The sour solvent (nitric acid and 5% sulfuric acid is the mixed solution of 1:1 by volume) that adds 10 times of volumes in the rhenium-containing material slag, after waiting to expect the most of dissolving of slag, feed liquid was heated 90 minutes down in 75 ℃, the sodium hydroxide that adds feed liquid weight 10% then, to be cooled to room temperature, filter, remove precipitation, the filtrate heating evaporation is removed most of moisture content after, the precipitation agent aniline blue black that adds filtrate weight 1% again in the residual filtrate, mechanical stirring 30 minutes is filtered, and feeds hydrogen sulfide in filtrate, vigorous stirring 60 minutes, placement is spent the night, and collects the precipitation of bottom, is the rhenium product.
With content and the foreign matter content of ICP mensuration rhenium, the result contains a small amount of sodium, potassium for the rate of recovery of rhenium is 82% in the rhenium product, the salt of ammonium, and the metal in the material slag is removed substantially.
Embodiment 5A kind of from rhenium-containing material slag the method for extraction separation rhenium
The rhenium-containing material slag that provides with certain E of company is raw material, in rhenium-containing material slag, and rhenium-containing 0.11%, platiniferous 0.51%, siliceous 39.5%L contains aluminium 58.5%.
The sour solvent (nitric acid and 5% sulfuric acid is the mixed solution of 1:1 by volume) that adds 10 times of volumes in the rhenium-containing material slag, after waiting to expect the most of dissolving of slag, feed liquid was heated 60 minutes down in 70 ℃, the sodium hydroxide that adds feed liquid weight 8% then, to be cooled to room temperature, filter, remove precipitation, the filtrate heating evaporation is removed most of moisture content after, the precipitation agent aniline blue black that adds filtrate weight 2% again in the residual filtrate, mechanical stirring 30 minutes is filtered, and feeds hydrogen sulfide in filtrate, vigorous stirring 60 minutes, placement is spent the night, and collects the precipitation of bottom, is the rhenium product.
With content and the foreign matter content of ICP mensuration rhenium, the result contains a small amount of sodium, potassium for the rate of recovery of rhenium is 85% in the rhenium product, the salt of ammonium, and the metal in the material slag is removed substantially.
Claims (2)
1. the method for an extraction separation rhenium from rhenium-containing material slag, it is characterized in that method is as follows: the sour solvent that adds 10 times of volumes in the rhenium-containing material slag, after the dissolving, feed liquid was heated 60-90 minute down in 60-80 ℃, the sodium hydroxide that adds feed liquid weight 1%-10% then, after being cooled to room temperature, filter, the filtrate heating evaporation is removed most of moisture content after, the precipitation agent aniline blue black that adds filtrate weight 1%-5% in the residual filtrate, stirred 30 minutes, and filtered, in filtrate, feed hydrogen sulfide, stir, placement is spent the night, and collects the precipitation of bottom, is the rhenium-containing product.
According to claim 1 described a kind of from rhenium-containing material slag the method for extraction separation rhenium, it is characterized in that: described sour solvent is that nitric acid and mass percentage concentration are the 5% sulfuric acid mixed solution of 1:1-3 by volume.
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CN105983707B (en) * | 2015-01-27 | 2019-02-15 | 昆明冶金高等专科学校 | A method of high-purity rhenium powder is prepared from rhenium-containing high arsenic-and copper-bearing sulfide |
CN106676267A (en) * | 2017-03-28 | 2017-05-17 | 青岛阿库卡稀有金属有限公司 | Method for removing anions from rhenium-contained feed liquid |
CN109355509B (en) * | 2018-12-03 | 2020-03-24 | 攀枝花环业冶金渣开发有限责任公司 | Method for selecting rhenium from high-titanium type blast furnace slag |
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JPS60131829A (en) * | 1983-12-16 | 1985-07-13 | Nippon Mining Co Ltd | Method for recovering rhenium |
JPS60131828A (en) * | 1983-12-16 | 1985-07-13 | Nippon Mining Co Ltd | Method for recovering rhenium from waste acid |
JPH07286221A (en) * | 1994-04-15 | 1995-10-31 | Sumitomo Metal Mining Co Ltd | Method for recovering rhenium from nonferrous metal refining process |
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CN1342779A (en) * | 2000-12-29 | 2002-04-03 | 张方宇 | Process for recovering metals Pt, Re and Al from waste reforming catalyst |
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Effective date of registration: 20190507 Address after: 412000 No. 3 Dong Jiaduo High-tech Park Aviation Road, Lusong District, Zhuzhou City, Hunan Province Patentee after: Re in New Material Co. Ltd. Address before: 266113 500 metres west of the Exit Processing Zone Management Committee Building, Chengyang District, Qingdao City, Shandong Province Patentee before: Qingdao Akuka Rare Metal Co.,Ltd. |