CN115747533A - Method for recovering scandium from scandium-containing salt slag - Google Patents

Method for recovering scandium from scandium-containing salt slag Download PDF

Info

Publication number
CN115747533A
CN115747533A CN202211431628.8A CN202211431628A CN115747533A CN 115747533 A CN115747533 A CN 115747533A CN 202211431628 A CN202211431628 A CN 202211431628A CN 115747533 A CN115747533 A CN 115747533A
Authority
CN
China
Prior art keywords
scandium
filter cake
slag
salt
sodium hydroxide
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202211431628.8A
Other languages
Chinese (zh)
Inventor
罗智坚
邱叶红
殷亮
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
First Rare Materials Co Ltd
Original Assignee
First Rare Materials Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by First Rare Materials Co Ltd filed Critical First Rare Materials Co Ltd
Priority to CN202211431628.8A priority Critical patent/CN115747533A/en
Publication of CN115747533A publication Critical patent/CN115747533A/en
Pending legal-status Critical Current

Links

Classifications

    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Landscapes

  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention provides a method for recycling scandium from scandium-containing salt slag, which comprises the following steps: crushing and levigating scandium salt-containing slag; adding sodium hydroxide into the scandium salt-containing slag, reacting, and filtering to obtain a scandium-rich filter cake and a filtrate containing aluminum and fluorine; adding tap water into the scandium-rich filter cake, stirring, performing suction filtration to obtain a washed filter cake, and drying the filter cake; step four, adding sodium hydroxide into the filter cake, fully mixing and roasting; step five, adding tap water into the roasted substance, stirring and filtering to obtain a filter cake; adding aluminum sulfate octadecahydrate powder into the filter cake, mixing uniformly, adding sulfuric acid, reacting until the solution is clear, and performing suction filtration; and seventhly, adding sodium sulfate into the filtrate, and performing suction filtration to obtain the sodium-scandium double salt. The method disclosed by the invention can avoid the generation of hydrogen fluoride gas, and can enrich scandium in advance before alkali melting, thereby reducing the consumption of sodium hydroxide and reducing the production cost.

Description

Method for recovering scandium from scandium-containing salt slag
Technical Field
The invention relates to the technical field of rare earth metal hydrometallurgy, in particular to a method for recycling scandium from scandium-containing salt slag.
Background
Scandium is widely applied to high-end technical fields such as aluminum-scandium alloy, novel electric light source materials, laser materials, electronic materials, catalysis industry, superconducting materials, optical materials, ceramics and the like due to excellent physical and chemical properties of scandium. Scandium is high in the crust, but independent scandium deposits are few, mainly in the form of associated ores, but in these ores scandium content is low. During the process of preparing the aluminum-scandium alloy by molten salt electrolysis, scandium-containing molten salt electrolysis waste residues are generated, wherein a scandium-containing raw material (0.76%) is included, so that the scandium recovery from the scandium-containing salt residues is of great significance.
Disclosure of Invention
In view of the problems in the prior art, it is an object of the present disclosure to provide a method for recovering scandium from a scandium-containing salt slag.
In order to achieve the above object, the present disclosure provides a method for recovering scandium from a scandium-containing salt slag, which includes the following steps: step one, crushing and grinding scandium salt-containing slag; adding sodium hydroxide into the scandium salt-containing slag, reacting, and filtering to obtain a scandium-rich filter cake and a filtrate containing aluminum and fluorine; adding tap water into the scandium-rich filter cake, stirring, removing alkali liquor and soluble impurities remaining on the surface of the scandium-rich filter cake, performing suction filtration to obtain a washed filter cake, and drying the filter cake; step four, adding sodium hydroxide into the filter cake, fully mixing and roasting; adding tap water into the roasted substance, stirring until the slag agglomeration disappears, and performing suction filtration to obtain a filter cake; adding aluminum sulfate octadecahydrate powder into the filter cake, uniformly mixing, adding sulfuric acid, reacting until the solution is clear, and performing suction filtration; and seventhly, adding sodium sulfate into the filtrate, stirring until the solution becomes white and turbid, and performing suction filtration to obtain the sodium-scandium double salt.
In some embodiments, in step one, the scandium-containing salt slag is crushed and ground to 200 mesh.
In some embodiments, in the second step, the liquid-solid ratio of the scandium-containing salt slag to the sodium hydroxide is 1:8-12.
In some embodiments, in step two, the concentration of sodium hydroxide is 1 to 3mol/L.
In some embodiments, in the second step, the reaction temperature is 80-90 ℃, and the stirring reaction is carried out for 2 hours.
In some embodiments, in step three, the liquid-to-solid ratio of the scandium-rich filter cake to tap water is 1: 10.
In some embodiments, in step three, stirring is performed at room temperature for 0.5-1h.
In some embodiments, in step three, the drying temperature is 80-100 ℃.
In some embodiments, in step four, the liquid-to-solid ratio of the filter cake to sodium hydroxide is 1: 0.8-2.
In some embodiments, in the fourth step, the roasting temperature is 360-600 ℃ and the roasting time is 2-4h.
In some embodiments, in step five, the liquid-to-solid ratio of calcined material to tap water is 1:5-10.
In some embodiments, in step six, the mass ratio of filter cake to aluminum sulfate octadecahydrate is 18-30: 1.
In some embodiments, in step six, the liquid-to-solid ratio of the filter cake to dilute sulfuric acid is 1: 3 to 8.
In some embodiments, in step six, the concentration of sulfuric acid is 32%.
In some embodiments, in step seven, the concentration of sodium sulfate is 250-350g/L.
The beneficial effects of this disclosure are as follows:
the method disclosed by the invention can avoid the generation of hydrogen fluoride gas, the scandium is enriched in advance before alkali melting, the consumption of sodium hydroxide is reduced, the production cost is reduced, the scandium is preliminarily purified by using sodium sulfate after being leached by sulfuric acid, the use of an extracting agent is avoided, and the generation of organic wastewater is reduced.
Detailed Description
The method for recovering scandium from the scandium-containing salt slag according to the present disclosure is explained in detail below.
The application discloses a method for recycling scandium from scandium-containing salt slag, which comprises the following steps: crushing and levigating scandium salt-containing slag; adding sodium hydroxide into the scandium salt-containing slag, reacting, and filtering to obtain a scandium-rich filter cake and a filtrate containing aluminum and fluorine; adding tap water into the scandium-enriched filter cake, stirring, removing alkali liquor and soluble impurities remained on the surface of the scandium-enriched filter cake, performing suction filtration to obtain a washed filter cake, and drying the filter cake; step four, adding sodium hydroxide into the filter cake, fully mixing and roasting; adding tap water into the roasted substance, stirring until the slag agglomeration disappears, and performing suction filtration to obtain a filter cake; step six, adding the aluminum sulfate octadecahydrate powder into the filter cake, uniformly mixing, adding sulfuric acid, reacting until the solution is clear, and performing suction filtration; and seventhly, adding sodium sulfate into the filtrate, stirring until the solution becomes white and turbid, and performing suction filtration to obtain the sodium-scandium double salt.
The method enriches scandium in the salt residue by low-concentration alkaline leaching and water washing under the condition of not leaching scandium; then the sodium hydroxide is used for alkali melting, water washing and acid leaching, wherein the water washing liquid after the alkali melting can be used for alkali leaching, and aluminum in the alkali leaching liquid is [ Al (OH) 4 ] - The form exists, and in the subsequent wastewater treatment stage, the pH value is adjusted, so that the fluoride ions in the leachate can be adsorbed and settled, and the concentration of the fluoride ions in the filtrate is reduced.
In some embodiments, in step one, the scandium salt-containing slag is ground to 200 mesh.
In some embodiments, in the second step, the liquid-solid ratio of the scandium-containing salt slag to the sodium hydroxide is 1:8-12. By low-concentration alkaline leaching, scandium is effectively prevented from being leached while scandium is enriched and defluorinated.
In some embodiments, in step two, the concentration of sodium hydroxide is 1 to 3mol/L.
In some embodiments, in the second step, the reaction temperature is 80-90 ℃, and the stirring reaction is carried out for 2 hours.
In some embodiments, in step three, the liquid-to-solid ratio of the scandium-rich filter cake to tap water is 1: 10.
In some embodiments, in step three, stirring is carried out at room temperature for 0.5-1h.
In some embodiments, in step three, the oven temperature is 80-100 ℃.
In some embodiments, in step four, the liquid-to-solid ratio of the filter cake to sodium hydroxide is 1: 0.8-2. Sodium hydroxide is adopted for alkali melting, and scandium fluoride can be converted into scandium oxide before the decomposition temperature of scandium fluoride, so that the generation of hydrogen fluoride is avoided.
In some embodiments, in the fourth step, the roasting temperature is 360-600 ℃ and the roasting time is 2-4h.
In some embodiments, in step five, the liquid-to-solid ratio of the calcined material to tap water is 1:5 to 10. Through two steps of alkaline leaching and alkaline melting water washing, nearly 99% of fluoride ions are removed, and aluminum salt is added during acid leaching to avoid hydrogen fluoride escaping in the reaction process, so that the requirement on production equipment is lowered, and the harm to the body of production personnel is reduced.
In some embodiments, in step six, the mass ratio of filter cake to aluminum sulfate octadecahydrate is 18-30: 1. The aluminum sulfate octadecahydrate can provide aluminum ions, partial fluoride ions can not be washed away after alkali is melted and washed, and the aluminum ions are utilized to complex the fluoride ions in order to prevent the fluoride ions and the sulfuric acid from generating hydrogen fluoride during acid leaching.
In some embodiments, in step six, the liquid-to-solid ratio of the filter cake to dilute sulfuric acid is 1: 3 to 8.
In some embodiments, in step six, the concentration of sulfuric acid is 32%.
In some embodiments, in step seven, the concentration of sodium sulfate is 250-350g/L.
[ test ]
Example 1
Step one, crushing and grinding 20g of scandium salt-containing slag to 200 meshes;
adding 2mol/L sodium hydroxide solution into the scandium-containing salt slag according to the solid-to-liquid ratio of 1: 10, controlling the reaction temperature to be 80-90 ℃, stirring for 2 hours at the rotating speed of 360r, filtering after reaction to obtain a scandium-rich filter cake and a filtrate containing aluminum and fluorine, wherein the content of scandium in the filtrate is lower than 2ppm;
adding tap water into the scandium-rich filter cake according to the solid-to-liquid ratio of 1: 10, stirring for 0.5h at room temperature, removing alkali liquor and soluble impurities remaining on the surface of the scandium-rich filter cake, performing suction filtration to obtain a washed filter cake, and drying the filter cake at the drying temperature of 80-90 ℃;
adding sodium hydroxide into the filter cake, wherein the liquid-solid ratio of the filter cake to the sodium hydroxide is 1: 0.8, fully mixing, roasting, uniformly stirring, and roasting at 600 ℃ for 4 hours;
adding tap water into the roasted substance according to the solid-liquid ratio of 1: 10, stirring for 30min until the slag agglomeration disappears, and performing suction filtration to obtain a filter cake, wherein the scandium content in the filtrate is lower than 40ppm;
step six, adding the aluminum sulfate octadecahydrate powder into the filter cake according to the mass ratio of the filter cake to the aluminum sulfate octadecahydrate being 24: 1, uniformly mixing, adding 32% sulfuric acid into the filter cake according to the solid-to-liquid ratio being 1:8, stirring for 1 hour at room temperature until the solution is clear, and filtering;
and seventhly, adding sodium sulfate into the filtrate to 300g/L, stirring for 6 hours at room temperature until a large number of white insoluble particles appear in the solution and are not increased, and performing suction filtration to obtain the sodium-scandium double salt, wherein the scandium content in the filtrate is 231ppm.
The leaching rate of scandium is 99.1%, and the recovery rate of scandium in the sodium-scandium double salt is 97.3%.
Example 2
Crushing and grinding 50g of scandium salt-containing slag to 200 meshes;
adding 2mol/L sodium hydroxide solution into the scandium-containing salt slag according to the solid-to-liquid ratio of 1:8, controlling the reaction temperature to be 80-90 ℃, stirring for 1h at the rotating speed of 360r, filtering after reaction to obtain a scandium-rich filter cake and a filtrate containing aluminum and fluorine, wherein the content of scandium in the filtrate is lower than 2ppm;
adding tap water into the scandium-enriched filter cake according to the solid-to-liquid ratio of 1: 10, stirring for 0.5h at room temperature, removing alkali liquor and soluble impurities remained on the surface of the scandium-enriched filter cake, performing suction filtration to obtain a washed filter cake, and drying the filter cake at the drying temperature of 80-90 ℃;
step four, adding sodium hydroxide into the filter cake, wherein the liquid-solid ratio of the filter cake to the sodium hydroxide is 1:1, fully mixing, roasting, uniformly stirring, and roasting at 480 ℃ for 2 hours;
adding tap water into the roasted substance according to the solid-liquid ratio of 1: 10, stirring for 15min until the slag agglomeration disappears, and performing suction filtration to obtain a filter cake, wherein the scandium content in the filtrate is lower than 80ppm;
step six, adding the aluminum sulfate octadecahydrate powder into the filter cake according to the mass ratio of the filter cake to the aluminum sulfate octadecahydrate being 18: 1, uniformly mixing, adding 32% sulfuric acid into the filter cake according to the solid-to-liquid ratio being 1:5, stirring for 1 hour at room temperature until the solution is clear, and filtering;
and seventhly, adding sodium sulfate into the filtrate to 300g/L, stirring for 6 hours at room temperature until a large number of white insoluble particles appear in the solution and are not increased any more, and performing suction filtration to obtain the sodium-scandium double salt, wherein the scandium content in the filtrate is 114ppm.
The leaching rate of scandium is 97.1%, and the recovery rate of scandium in the sodium-scandium double salt is 98.2%.
The above-disclosed features are not intended to limit the scope of practice of the present disclosure, and therefore, all equivalent variations that are described in the claims of the present disclosure are intended to be included within the scope of the claims of the present disclosure.

Claims (8)

1. A method for recovering scandium from scandium-containing salt slag comprises the following steps:
step one, crushing and grinding scandium salt-containing slag;
adding sodium hydroxide into the scandium salt-containing slag, reacting, and filtering to obtain a scandium-rich filter cake and a filtrate containing aluminum and fluorine;
adding tap water into the scandium-rich filter cake, stirring, removing alkali liquor and soluble impurities remaining on the surface of the scandium-rich filter cake, performing suction filtration to obtain a washed filter cake, and drying the filter cake;
step four, adding sodium hydroxide into the filter cake, fully mixing and roasting;
adding tap water into the roasted substance, stirring until the slag agglomeration disappears, and performing suction filtration to obtain a filter cake;
step six, adding the aluminum sulfate octadecahydrate powder into the filter cake, uniformly mixing, adding sulfuric acid, reacting until the solution is clear, and performing suction filtration;
and seventhly, adding sodium sulfate into the filtrate, stirring until the solution becomes white and turbid, and performing suction filtration to obtain the sodium-scandium double salt.
2. The method for recovering scandium from the scandium-containing salt slag according to claim 1, wherein,
in the first step, the scandium salt-containing slag is crushed and ground to 200 meshes.
3. The method for recovering scandium from the scandium-containing salt slag according to claim 1, wherein,
in the second step, the liquid-solid ratio of the scandium-containing salt slag to the sodium hydroxide is 1: 8-12;
in the second step, the concentration of the sodium hydroxide is 1-3mol/L;
in the second step, the reaction temperature is 80-90 ℃, and the stirring reaction is carried out for 2 hours.
4. The method for recovering scandium from the scandium-containing salt slag according to claim 1, wherein,
in the third step, the liquid-solid ratio of the scandium-rich filter cake to the tap water is 1: 10;
stirring at room temperature for 0.5-1h in step three;
in the third step, the drying temperature is 80-100 ℃.
5. The method for recovering scandium from the scandium-containing salt slag according to claim 1, wherein,
in the fourth step, the liquid-solid ratio of the filter cake to the sodium hydroxide is 1: 0.8-2;
in the fourth step, the roasting temperature is 360-600 ℃, and the roasting time is 2-4h.
6. The method for recovering scandium from the scandium-containing salt slag according to claim 1, wherein,
in the fifth step, the liquid-solid ratio of the roasted substance to tap water is 1:5-10.
7. The method for recovering scandium from the scandium-containing salt slag according to claim 1, wherein,
in the sixth step, the mass ratio of the filter cake to the aluminum sulfate octadecahydrate is 18-30: 1;
in the sixth step, the liquid-solid ratio of the filter cake to the dilute sulfuric acid is 1: 3-8;
in step six, the concentration of sulfuric acid is 32%.
8. The method for recovering scandium from the scandium-containing salt slag according to claim 1, wherein,
in the seventh step, the concentration of the sodium sulfate is 250-350g/L.
CN202211431628.8A 2022-11-15 2022-11-15 Method for recovering scandium from scandium-containing salt slag Pending CN115747533A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202211431628.8A CN115747533A (en) 2022-11-15 2022-11-15 Method for recovering scandium from scandium-containing salt slag

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202211431628.8A CN115747533A (en) 2022-11-15 2022-11-15 Method for recovering scandium from scandium-containing salt slag

Publications (1)

Publication Number Publication Date
CN115747533A true CN115747533A (en) 2023-03-07

Family

ID=85371589

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202211431628.8A Pending CN115747533A (en) 2022-11-15 2022-11-15 Method for recovering scandium from scandium-containing salt slag

Country Status (1)

Country Link
CN (1) CN115747533A (en)

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1133346A (en) * 1995-04-12 1996-10-16 北京有色金属研究总院 Sorting cerium process by extraction from rare-earth sulfate solution containing fluorine
CN102021343A (en) * 2010-10-13 2011-04-20 赣州鑫磊稀土新材料有限公司 Method for separating and recovering scandium oxide from aluminum-scandium alloy smelting waste
CN103215439A (en) * 2013-04-16 2013-07-24 内蒙古科技大学 Method for extracting scandium from scandium enrichment
CN107429320A (en) * 2015-03-24 2017-12-01 住友金属矿山株式会社 Scandium recovery method
CN108026609A (en) * 2016-08-04 2018-05-11 俄铝工程技术中心有限责任公司 The production of the concentrate containing scandium and therefrom further extraction high-purity mangesium oxide scandium
CN110387474A (en) * 2019-08-23 2019-10-29 中国恩菲工程技术有限公司 The processing method of the electrolytic slag generated during aluminum production by fused-salt electrolysis scandium alloy
GB2578655A (en) * 2018-11-01 2020-05-20 Grimley Smith Associates Env Ltd Metals recovery

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1133346A (en) * 1995-04-12 1996-10-16 北京有色金属研究总院 Sorting cerium process by extraction from rare-earth sulfate solution containing fluorine
CN102021343A (en) * 2010-10-13 2011-04-20 赣州鑫磊稀土新材料有限公司 Method for separating and recovering scandium oxide from aluminum-scandium alloy smelting waste
CN103215439A (en) * 2013-04-16 2013-07-24 内蒙古科技大学 Method for extracting scandium from scandium enrichment
CN107429320A (en) * 2015-03-24 2017-12-01 住友金属矿山株式会社 Scandium recovery method
CN108026609A (en) * 2016-08-04 2018-05-11 俄铝工程技术中心有限责任公司 The production of the concentrate containing scandium and therefrom further extraction high-purity mangesium oxide scandium
GB2578655A (en) * 2018-11-01 2020-05-20 Grimley Smith Associates Env Ltd Metals recovery
CN110387474A (en) * 2019-08-23 2019-10-29 中国恩菲工程技术有限公司 The processing method of the electrolytic slag generated during aluminum production by fused-salt electrolysis scandium alloy

Similar Documents

Publication Publication Date Title
CN103397213B (en) Method for decomposing and extracting Baotou rare earth ore through mixed alkali roasting process
CN110835683A (en) Method for selectively extracting lithium from waste lithium ion battery material
CN105274352B (en) A kind of method that copper cobalt manganese is separated in the manganese cobalt calcium zinc mixture from copper carbonate
CN110629045A (en) Method for preparing titanium-rich material for boiling chlorination from high-calcium magnesium and low-grade titanium slag
WO2021134515A1 (en) Battery-level ni-co-mn mixed solution and preparation method for battery-level mn solution
CN111440955A (en) Method for extracting gallium from gallium-containing smelting slag
CN114349079A (en) Recycling treatment method for nickel slag solid waste in nitrogen trifluoride gas electrolysis production
CN111926193B (en) Method for recovering magnesium from ferronickel slag
CN114133014A (en) Process method for recycling nickel-containing waste residue generated by electrolyzing nitrogen trifluoride
KR20090109733A (en) Method for producing high purity cobalt carbonate
CN106904664A (en) Hydroxyl cobaltosic oxide and preparation method thereof
CN108517426B (en) Method for efficiently separating and recycling rare earth in waste CRT fluorescent powder under mild condition
CN109055764B (en) Comprehensive recovery method of high-chlorine low-zinc material
CN115747533A (en) Method for recovering scandium from scandium-containing salt slag
CN115852177A (en) Method for recycling scandium from fused salt chlorination dust collection slag
CN110629043B (en) Bismuth extraction method based on phase transformation of bismuth sulfide ore
US4384940A (en) Chlorine leaching of nickel-cobalt-iron sulphides
CN111438354B (en) Clean production method of high-purity gold powder
CN113981230A (en) Method for leaching nickel cobalt slag
CN110541074B (en) Method for extracting germanium and cobalt from white alloy
CN112126791A (en) Method for recycling high-purity copper from metal waste
CN111807342A (en) Method for purifying and preparing submicron-grade iron phosphate from phosphated slag
CN110627106A (en) Method for producing zinc carbonate by using blast furnace cloth bag ash dechlorination wastewater
CN115566307B (en) Method for recovering high-purity lithium oxalate and high-purity lithium hydroxide from waste lithium battery
CN114318019B (en) Method for separating rare earth and aluminum from ionic rare earth mine leachate

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination