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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- rhenium
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- containing material
- material slag
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- 229910052702 rhenium Inorganic materials 0.000 title claims abstract description 95
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 239000002893 slag Substances 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 39
- 239000000706 filtrate Substances 0.000 claims abstract description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 239000000047 product Substances 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001704 evaporation Methods 0.000 claims abstract description 8
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims abstract description 8
- 238000001556 precipitation Methods 0.000 claims description 20
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- 238000000605 extraction Methods 0.000 claims description 14
- 238000000926 separation method Methods 0.000 claims description 13
- HKJKONMZMPUGHJ-UHFFFAOYSA-N 4-amino-5-hydroxy-3-[(4-nitrophenyl)diazenyl]-6-phenyldiazenylnaphthalene-2,7-disulfonic acid Chemical compound OS(=O)(=O)C1=CC2=CC(S(O)(=O)=O)=C(N=NC=3C=CC=CC=3)C(O)=C2C(N)=C1N=NC1=CC=C([N+]([O-])=O)C=C1 HKJKONMZMPUGHJ-UHFFFAOYSA-N 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 230000008020 evaporation Effects 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 238000011084 recovery Methods 0.000 abstract description 9
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract 2
- FWLHAQYOFMQTHQ-UHFFFAOYSA-N 2-N-[8-[[8-(4-aminoanilino)-10-phenylphenazin-10-ium-2-yl]amino]-10-phenylphenazin-10-ium-2-yl]-8-N,10-diphenylphenazin-10-ium-2,8-diamine hydroxy-oxido-dioxochromium Chemical compound O[Cr]([O-])(=O)=O.O[Cr]([O-])(=O)=O.O[Cr]([O-])(=O)=O.Nc1ccc(Nc2ccc3nc4ccc(Nc5ccc6nc7ccc(Nc8ccc9nc%10ccc(Nc%11ccccc%11)cc%10[n+](-c%10ccccc%10)c9c8)cc7[n+](-c7ccccc7)c6c5)cc4[n+](-c4ccccc4)c3c2)cc1 FWLHAQYOFMQTHQ-UHFFFAOYSA-N 0.000 abstract 1
- 239000002253 acid Substances 0.000 abstract 1
- 230000032683 aging Effects 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 229920000767 polyaniline Polymers 0.000 abstract 1
- 239000002244 precipitate Substances 0.000 abstract 1
- 230000001376 precipitating effect Effects 0.000 abstract 1
- XOSXWYQMOYSSKB-LDKJGXKFSA-L water blue Chemical compound CC1=CC(/C(\C(C=C2)=CC=C2NC(C=C2)=CC=C2S([O-])(=O)=O)=C(\C=C2)/C=C/C\2=N\C(C=C2)=CC=C2S([O-])(=O)=O)=CC(S(O)(=O)=O)=C1N.[Na+].[Na+] XOSXWYQMOYSSKB-LDKJGXKFSA-L 0.000 abstract 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 13
- 229910052750 molybdenum Inorganic materials 0.000 description 13
- 239000011733 molybdenum Substances 0.000 description 13
- 239000002994 raw material Substances 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 239000002699 waste material Substances 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 5
- 238000010907 mechanical stirring Methods 0.000 description 5
- 229910052700 potassium Inorganic materials 0.000 description 5
- 239000011591 potassium Substances 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 229910052708 sodium Inorganic materials 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- 229910052500 inorganic mineral Inorganic materials 0.000 description 4
- 239000011707 mineral Substances 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- QPHSHUVNLKVKTL-UHFFFAOYSA-N [Re].[Cu]=S Chemical compound [Re].[Cu]=S QPHSHUVNLKVKTL-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 229910001729 niobium mineral Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229910052569 sulfide mineral Inorganic materials 0.000 description 1
- 230000031068 symbiosis, encompassing mutualism through parasitism Effects 0.000 description 1
Classifications
-
- 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
Landscapes
- Manufacture And Refinement Of Metals (AREA)
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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| CN2012102167518A CN102703737B (en) | 2012-06-28 | 2012-06-28 | Method for extracting and separating rhenium from rhenium-containing slag |
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| CN2012102167518A CN102703737B (en) | 2012-06-28 | 2012-06-28 | Method for extracting and separating rhenium from rhenium-containing slag |
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| CN102703737B true CN102703737B (en) | 2013-08-07 |
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| CN105983707B (en) * | 2015-01-27 | 2019-02-15 | 昆明冶金高等专科学校 | A method for preparing high-purity rhenium powder from rhenium-containing high-arsenic copper 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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