CN111593212A - Method for recovering rare earth from rare earth secondary resource - Google Patents
Method for recovering rare earth from rare earth secondary resource Download PDFInfo
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- CN111593212A CN111593212A CN202010432708.XA CN202010432708A CN111593212A CN 111593212 A CN111593212 A CN 111593212A CN 202010432708 A CN202010432708 A CN 202010432708A CN 111593212 A CN111593212 A CN 111593212A
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- rare earth
- acid decomposition
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B59/00—Obtaining rare earth metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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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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- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Environmental & Geological Engineering (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
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- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention provides a method for recovering rare earth from rare earth secondary resources, which comprises the following steps: putting the waste water sediment into a container filled with a sodium hydroxide solution, reacting the waste water sediment with the sodium hydroxide, and separating to obtain a solid product after the reaction is finished; putting the solid product into an acid decomposition tank filled with acid decomposition slag to carry out acid decomposition reaction and then leaching to obtain rare earth feed liquid; the rare earth liquid is introduced into the rare earth separation process, the sodium hydroxide solution is used for carrying out alkali conversion on the waste water sediment, then the waste water sediment is leached by hydrochloric acid through the acid decomposition tank and the acid decomposition residue ingredient, and the rare earth liquid with high rare earth content is finally obtained and can be returned to the rare earth separation production process for recycling.
Description
Technical Field
One or more embodiments of the present disclosure relate to the field of rare earth secondary resource utilization technologies, and in particular, to a method for recovering rare earth from rare earth secondary resources.
Background
China is a big rare earth smelting country, and resource distribution shows the characteristic of 'light south-heavy north', namely, ion type rare earth ore with high content of medium-heavy rare earth is taken as the main part in south, and rare earth ore with high content of light rare earth in north is taken as the main part in north. Usually, the price of the medium-heavy rare earth is far higher than that of the light rare earth, so the smelting value of the south ionic rare earth ore is high, and the ion rare earth ore is generally regarded by the industry.
South ionic rare earth ore is usually prepared into single rare earth or mixed rare earth oxide products by adopting the process flows of acid decomposition, solvent extraction separation, precipitation and calcination. On one hand, in the acid decomposition process of the rare earth ore, in order to reduce the use amount of acid and the leaching rate of impurity elements, the ore is often leached in a hydrochloric acid preferential dissolution mode, but in the production process, the pH value of a pickle liquor system is continuously increased along with the continuous consumption of hydrochloric acid, and rare earth ions entering the pickle liquor are easy to precipitate and enter acid decomposition residues, so that the rare earth content in the acid decomposition residues is high; on the other hand, the rare earth smelting wastewater has complex components, often generates rare earth oxalate or rare earth carbonate particles, and is usually led into a pool to stand to obtain rare earth sediments. No matter acid decomposition slag or waste water sediment, the rare earth content is higher, is the important rare earth secondary resource that produces in the production process of rare earth smelting enterprise, if do not carry out recycle, will cause the waste of resource, to sum up, this application now provides a method of retrieving the tombarthite from the tombarthite secondary resource and solves above-mentioned problem that appears.
Disclosure of Invention
In view of the above, an object of one or more embodiments of the present disclosure is to provide a method for recovering rare earth from a rare earth secondary resource, so as to solve the problems set forth in the background art.
In view of the above, one or more embodiments of the present specification provide a method for recovering rare earth from a rare earth secondary resource, including the steps of:
S1putting the waste water sediment into a container filled with a sodium hydroxide solution, reacting the waste water sediment with the sodium hydroxide, and separating to obtain a solid product after the reaction is finished;
S2will S1Putting the solid product obtained in the step (1) into an acid decomposition tank filled with acid decomposition slag to carry out acid decomposition reaction and then leaching to obtain rare earth feed liquid;
S3will S2Introducing the rare earth feed liquid obtained in the step (b) into a rare earth separation process.
Preferably, said step S1The concentration of the sodium hydroxide solution in the solution is 10 to 30 percent.
Preferably, said step S1The liquid-solid ratio of the sodium hydroxide solution to the wastewater sediment is 4: 1-1: 1.
preferably, said step S1The reaction temperature in (1) is 60-90 ℃.
Preferably, said step S1The reaction time in (1) is 0.5-2 h.
Preferably, said step S1The waste water sediment in the process is sediment in a rare earth separation waste water pool.
Preferably, said step S2The liquid-solid ratio of the solution in the acid decomposition tank to the mixture of the acid decomposition slag and the solid product is 2: 1-4: 1.
preferably, said step S2The temperature of the acid decomposition reaction in (1) was 50 ℃ at room temperature.
Preferably, said step S2The concentration of hydrochloric acid in the medium acid decomposition tank is 4-8 mol/L.
Preferably, said step S2The acid decomposition slag in the method is obtained by decomposing oxide rare earth ore or carbonate rare earth ore of south ionic rare earth ore by adopting a hydrochloric acid optimum dissolution method.
From the above, the method provided by the invention has the advantages that the sodium hydroxide solution is used for carrying out alkali conversion on the wastewater sediments, then the hydrochloric acid leaching is carried out on the wastewater sediments and the acid decomposition residue ingredient through the acid decomposition tank, and finally the rare earth feed liquid with high rare earth content is obtained and can be returned to the rare earth separation production flow for recycling.
Detailed Description
To make the objects, technical solutions and advantages of the present disclosure more apparent, the present disclosure is further described in detail below with reference to specific embodiments.
It is to be noted that unless otherwise defined, technical or scientific terms used in one or more embodiments of the present specification should have the ordinary meaning as understood by those of ordinary skill in the art to which this disclosure belongs. The use of "first," "second," and similar terms in one or more embodiments of the specification is not intended to indicate any order, quantity, or importance, but rather is used to distinguish one element from another. The word "comprising" or "comprises", and the like, means that the element or item listed before the word covers the element or item listed after the word and its equivalents, but does not exclude other elements or items. The terms "connected" or "coupled" and the like are not restricted to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "upper", "lower", "left", "right", and the like are used merely to indicate relative positional relationships, and when the absolute position of the object being described is changed, the relative positional relationships may also be changed accordingly.
Example one
A method for recovering rare earth from rare earth secondary resources comprises the following steps:
S1depositing the waste waterPutting the waste water into a container filled with a sodium hydroxide solution to react the waste water sediment with the sodium hydroxide, and separating to obtain a solid product after the reaction is finished;
S2will S1Putting the solid product obtained in the step (1) into an acid decomposition tank filled with acid decomposition slag to carry out acid decomposition reaction and then leaching to obtain rare earth feed liquid;
S3will S2Introducing the rare earth feed liquid obtained in the step (b) into a rare earth separation process.
As a modification of the above, the step S1The concentration of the sodium hydroxide solution in the solution is 10 to 30 percent.
As a modification of the above, the step S1The liquid-solid ratio of the sodium hydroxide solution to the wastewater sediment is 4: 1-1: 1.
as a modification of the above, the step S1The reaction temperature in (1) is 60-90 ℃.
As a modification of the above, the step S1The reaction time in (1) is 0.5-2 h.
As a modification of the above, the step S1The waste water sediment in the process is sediment in a rare earth separation waste water pool.
As a modification of the above, the step S2The liquid-solid ratio of acid decomposition slag to solid product is 2: 1-4: 1.
as a modification of the above, the step S2The temperature of the acid decomposition reaction in (1) was 50 ℃ at room temperature.
As a modification of the above, the step S2The concentration of hydrochloric acid in the medium acid decomposition tank is 4-8 mol/L.
As a modification of the above, the step S2The acid decomposition slag in the method is obtained by decomposing oxide rare earth ore or carbonate rare earth ore of south ionic rare earth ore by adopting a hydrochloric acid optimum dissolution method.
Example two
Taking 1.5kg of wastewater sediment, wherein the content of REO is 18.97 wt%, putting 1.5kg of wastewater sediment into a container containing 20% sodium hydroxide solution, and the liquid-solid ratio is 2: 1, reacting for 1h in an environment with the temperature of 70 ℃ to obtain a solid product, mixing the obtained solid product with acid decomposition slag, putting the mixture into an acid decomposition tank containing hydrochloric acid with the concentration of 6mol/L, wherein the liquid-solid ratio is 3: 1, leaching reaction at 50 ℃, and filtering to obtain rare earth feed liquid with the concentration of 28.98g/L, wherein the leaching rate of rare earth is 99.15%.
EXAMPLE III
Taking 4.5kg of wastewater sediment, wherein the REO content is 16.87 wt%, putting the 4.5kg of wastewater sediment into a container containing 15% sodium hydroxide solution, and the liquid-solid ratio is 3: 1, reacting for 0.8h in an environment with the temperature of 65 ℃ to obtain a solid product, mixing the obtained solid product with acid decomposition slag, putting the mixture into an acid decomposition tank containing hydrochloric acid with the concentration of 5.5mol/L, wherein the liquid-solid ratio is 2.5: 1, leaching reaction at 50 ℃, and filtering to obtain rare earth feed liquid with the concentration of 32.04g/L, wherein the leaching rate of rare earth is 99.08%.
Example four
Taking 8.5kg of wastewater sediment, wherein the content of REO is 30.08 wt%, putting 8.5kg of wastewater sediment into a container containing 25% sodium hydroxide solution, and the liquid-solid ratio is 3: 1, reacting for 1.5 hours in an environment with the temperature of 75 ℃ to obtain a solid product, mixing the obtained solid product with acid decomposition slag, putting the mixture into an acid decomposition tank containing hydrochloric acid with the concentration of 7.5mol/L, wherein the liquid-solid ratio is 3.5: 1, leaching reaction at 50 ℃, and filtering to obtain rare earth feed liquid with the concentration of 29.54g/L, wherein the leaching rate of the rare earth is 99.43%.
And finally, recovering the obtained rare earth feed liquid to a main process of rare earth separation for recovering the rare earth.
It is intended that the one or more embodiments of the present specification embrace all such alternatives, modifications and variations as fall within the broad scope of the appended claims. Therefore, any omissions, modifications, substitutions, improvements, and the like that may be made without departing from the spirit and principles of one or more embodiments of the present disclosure are intended to be included within the scope of the present disclosure.
Claims (10)
1. A method for recovering rare earth from rare earth secondary resources is characterized by comprising the following steps:
S1putting the waste water sediment into a container filled with a sodium hydroxide solution, reacting the waste water sediment with the sodium hydroxide, and separating to obtain a solid product after the reaction is finished;
S2will S1Putting the solid product obtained in the step (1) into an acid decomposition tank filled with acid decomposition slag to carry out acid decomposition reaction and then leaching to obtain rare earth feed liquid;
S3will S2Introducing the rare earth feed liquid obtained in the step (b) into a rare earth separation process.
2. The method for recovering rare earth from rare earth secondary resources according to claim 1, wherein the step S1The concentration of the sodium hydroxide solution in the solution is 10 to 30 percent.
3. The method for recovering rare earth from rare earth secondary resources according to claim 1, wherein the step S1The liquid-solid ratio of the sodium hydroxide solution to the wastewater sediment is 4: 1-1: 1.
4. the method for recovering rare earth from rare earth secondary resources according to claim 1, wherein the step S1The reaction temperature in (1) is 60-90 ℃.
5. The method for recovering rare earth from rare earth secondary resources according to claim 1, wherein the step S1The reaction time in (1) is 0.5-2 h.
6. The method for recovering rare earth from rare earth secondary resources according to claim 1, wherein the step S1The waste water sediment in the process is sediment in a rare earth separation waste water pool.
7. The method for recovering rare earth from rare earth secondary resources according to claim 1, wherein the step S2The liquid-solid ratio of the solution in the acid decomposition tank to the mixture of the acid decomposition slag and the solid product is 2: 1-4: 1.
8. the method for recovering rare earth from rare earth secondary resources according to claim 1, wherein the step S2The temperature of the acid decomposition reaction in (1) was 50 ℃ at room temperature.
9. The method for recovering rare earth from rare earth secondary resources according to claim 1, wherein the step S2The concentration of hydrochloric acid in the medium acid decomposition tank is 4-8 mol/L.
10. The method for recovering rare earth from rare earth secondary resources according to claim 1, wherein the step S2The acid decomposition slag in the method is obtained by decomposing oxide rare earth ore or carbonate rare earth ore of south ionic rare earth ore by adopting a hydrochloric acid optimum dissolution method.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010432708.XA CN111593212A (en) | 2020-05-20 | 2020-05-20 | Method for recovering rare earth from rare earth secondary resource |
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| CN202010432708.XA CN111593212A (en) | 2020-05-20 | 2020-05-20 | Method for recovering rare earth from rare earth secondary resource |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114934201A (en) * | 2022-06-20 | 2022-08-23 | 淄博灵芝化工有限公司 | Method for recovering rare earth from rare earth tempering slag |
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| CN101880782A (en) * | 2010-01-06 | 2010-11-10 | 马克印 | Process for rare-earth smelting resource reclamation and cyclic production |
| EP2444507A1 (en) * | 2010-10-20 | 2012-04-25 | Montanuniversität Leoben | Recovery of rare earth metals from waste material by leaching in non-oxidizing acid and by precipitating using sulphates |
| CN104928504A (en) * | 2014-03-17 | 2015-09-23 | 有研稀土新材料股份有限公司 | Recycling method of rare earth in aluminum silicon waste |
| CN105803187A (en) * | 2016-05-19 | 2016-07-27 | 东北大学 | Microwave-assisted decomposition method for Baotou mixed rare earth concentrates |
| CN107099670A (en) * | 2017-05-11 | 2017-08-29 | 青岛惠城环保科技股份有限公司 | A kind of preparation method of rare earth chloride |
| US11028461B2 (en) * | 2017-05-11 | 2021-06-08 | Worcester Polytechnic Institute | Bauxite residue recycling |
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2020
- 2020-05-20 CN CN202010432708.XA patent/CN111593212A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880782A (en) * | 2010-01-06 | 2010-11-10 | 马克印 | Process for rare-earth smelting resource reclamation and cyclic production |
| EP2444507A1 (en) * | 2010-10-20 | 2012-04-25 | Montanuniversität Leoben | Recovery of rare earth metals from waste material by leaching in non-oxidizing acid and by precipitating using sulphates |
| CN104928504A (en) * | 2014-03-17 | 2015-09-23 | 有研稀土新材料股份有限公司 | Recycling method of rare earth in aluminum silicon waste |
| CN105803187A (en) * | 2016-05-19 | 2016-07-27 | 东北大学 | Microwave-assisted decomposition method for Baotou mixed rare earth concentrates |
| CN107099670A (en) * | 2017-05-11 | 2017-08-29 | 青岛惠城环保科技股份有限公司 | A kind of preparation method of rare earth chloride |
| US11028461B2 (en) * | 2017-05-11 | 2021-06-08 | Worcester Polytechnic Institute | Bauxite residue recycling |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114934201A (en) * | 2022-06-20 | 2022-08-23 | 淄博灵芝化工有限公司 | Method for recovering rare earth from rare earth tempering slag |
| CN114934201B (en) * | 2022-06-20 | 2024-05-17 | 淄博灵芝化工有限公司 | Method for recovering rare earth from rare earth callback slag |
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