CN111593213A - Method for extracting rare earth from rare earth organic slag - Google Patents
Method for extracting rare earth from rare earth organic slag Download PDFInfo
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- CN111593213A CN111593213A CN202010432709.4A CN202010432709A CN111593213A CN 111593213 A CN111593213 A CN 111593213A CN 202010432709 A CN202010432709 A CN 202010432709A CN 111593213 A CN111593213 A CN 111593213A
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/005—Preliminary treatment of scrap
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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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Abstract
One or more embodiments of the present specification provide a method of extracting rare earth from rare earth organic slag, including the steps of: placing the rare earth organic slag in a container filled with water, and stirring the rare earth organic slag in one direction by using a stirring shovel to obtain slurry; adding flake caustic soda into the container, and stirring the flake caustic soda in one direction by using a stirring shovel to perform alkali conversion on the slurry to obtain alkali-converted slag; washing the alkali-converted slag with water, and then putting the washed alkali brick slag into an acid decomposition tank for leaching to obtain rare earth feed liquid; returning the rare earth feed liquid to the rare earth separation production flow for recycling; according to the invention, the rare earth organic slag is treated through steps of size mixing, alkali conversion, acid dissolution and the like, so that the rare earth feed liquid with high rare earth content is finally obtained, the rare earth feed liquid can be returned to the main process of rare earth separation production for cyclic utilization, the method is simple, practical and effective, and has high recovery rate, and the resource loss is prevented.
Description
Technical Field
One or more embodiments of the present disclosure relate to the technical field of recycling rare earth secondary resources, and in particular, to a method for extracting rare earth from rare earth organic slag.
Background
Rare earth is an important strategic resource. The rare earth resource reserves in China are large, and the rare earth resource reserves are important 'rare earth kingdom' in the world. Rare earth resources are mainly divided into southern ionic ore and northern light rare earth ore in China. Whether the ore is south ore or north ore, the smelting process is the same approximately: the method comprises the steps of pretreating minerals, leaching with inorganic acid to obtain rare earth feed liquid, extracting and separating with a solvent to obtain a single rare earth or an enriched solution, precipitating with oxalic acid or carbonate to obtain rare earth oxalate or rare earth carbonate, and calcining the rare earth oxalate or rare earth carbonate to obtain rare earth oxide. In the whole rare earth smelting process, dissolution and extraction are the most important links.
Due to the large exploitation and utilization of high-quality ore sources, rare earth ore is increasingly complex, the content and total class of impurities are more and more, more or less of the impurities also enter an extraction system, and the forward movement of the impurities in a tank body often causes the phenomenon of 'emulsification' of the tank body. In order to keep the normal work of the tank body, production enterprises often discharge the generated emulsified third phase from the tank body and accumulate the third phase outside, so that a large amount of rare earth organic slag is formed in a long time, the content of rare earth in the rare earth organic slag is high, and the rare earth organic slag is usually 6% -10% of the weight of the rare earth organic slag, and the rare earth organic slag can only be accumulated in an enterprise slag warehouse due to the lack of an effective treatment method. On one hand, the rare earth organic slag contains organic matters and is easy to diffuse into the air to destroy the environment; on the other hand, precious rare earth resources in the slag cannot be recycled, so that the waste of resources is caused, and the sustainable development of the rare earth industry is not facilitated.
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 extracting rare earth from rare earth organic slag, so as to solve the problems in the background art.
In view of the above, one or more embodiments of the present specification provide a method for extracting rare earth from a rare earth organic slag, including the steps of:
s1, placing the rare earth organic slag into a container filled with water, and stirring the rare earth organic slag in one direction by using a stirring shovel to obtain slurry;
s2, adding caustic soda flakes into the container in the step S1, stirring the mixture in one direction by using a stirring shovel, and performing alkali conversion on the slurry obtained in the step S1 to obtain alkali-converted slag;
s3, washing the alkali-converted slag obtained in the step S2 with water, and then putting the washed alkali brick slag into an acid decomposition tank for leaching to obtain rare earth feed liquid;
and S4, returning the rare earth feed liquid obtained in the step S3 to the rare earth separation production flow for recycling.
Preferably, the mass ratio of the rare earth organic slag to the water in the step S1 is 1: 1-1: 2.
Preferably, the mass ratio of the addition amount of caustic soda flakes to the rare earth organic slag in the step S2 is as follows: 0.1 to 0.4.
Preferably, the temperature of the alkali conversion in the step S2 is 70-95 ℃.
Preferably, the time for alkali conversion in the step S2 is 0.5-3 h.
Preferably, the hydrochloric acid concentration in the acid decomposition tank in the step S3 is 4-6 mol/L.
Preferably, the temperature of the reaction between the washed alkaline residue and hydrochloric acid in the acid decomposition tank in step S3 is 60 ℃.
Preferably, the liquid-solid ratio of the hydrochloric acid in the acid decomposition tank to the alkali-converted slag in the step S3 is 2:1 to 5: 1.
Preferably, the concentration of hydrochloric acid remaining after the reaction of the washed alkaline transfer residue and hydrochloric acid in the acid decomposition tank in the step S3 is 0.5 to 1 mol/L.
From the above, the rare earth organic slag is treated through the steps of size mixing, alkali conversion, acid dissolution and the like, so that the rare earth feed liquid with high rare earth content is finally obtained, the rare earth feed liquid can be returned to the main process of rare earth separation production for recycling, the method is simple, practical and effective, the recovery rate is high, and the resource loss is prevented.
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 extracting rare earth from rare earth organic slag comprises the following steps:
s1, placing the rare earth organic slag into a container filled with water, and stirring the rare earth organic slag in one direction by using a stirring shovel to obtain slurry;
s2, adding caustic soda flakes into the container in the step S1, stirring the mixture in one direction by using a stirring shovel, and performing alkali conversion on the slurry obtained in the step S1 to obtain alkali-converted slag;
s3, washing the alkali-converted slag obtained in the step S2 with water, and then putting the washed alkali brick slag into an acid decomposition tank for leaching to obtain rare earth feed liquid;
and S4, returning the rare earth feed liquid obtained in the step S3 to the rare earth separation production flow for recycling.
As an improvement scheme of the scheme, the mass ratio of the rare earth organic slag to the water in the step S1 is 1: 1-1: 2.
As an improvement of the above scheme, the mass ratio of the addition amount of the caustic soda flakes to the rare earth organic slag in the step S2 is as follows: 0.1 to 0.4.
As a modification of the above scheme, the temperature of the alkali conversion in the step S2 is 70-95 ℃.
As a modification of the above scheme, the time for alkali conversion in the step S2 is 0.5-3 h.
As a modification of the above, the hydrochloric acid concentration in the acid decomposition tank in the step S3 is 4-6 mol/L.
As a modification of the above scheme, the temperature of the reaction between the washed alkaline transfer residue and hydrochloric acid in the acid decomposition tank in the step S3 is 60 ℃.
As an improvement of the scheme, the liquid-solid ratio of the hydrochloric acid in the acid decomposition tank to the alkali transfer slag in the step S3 is 2: 1-5: 1.
As a modification of the above scheme, the concentration of hydrochloric acid remaining after the reaction of the alkali-exchanged slag washed with water in the step S3 and hydrochloric acid in the acid decomposition tank is 0.5-1 mol/L.
Example two
Taking 2.0kg of rare earth organic slag, wherein the content of REO is 25.67 wt%, putting 2.0kg of organic slag into a container containing water, the liquid-solid ratio is 1.15, stirring to obtain a slurry, adding caustic soda flakes into the container, the mass ratio of the caustic soda flakes to the rare earth organic slag is 0.2, carrying out alkali conversion on the slurry and the caustic soda flakes for 2 hours at the temperature of 80 ℃ to obtain alkali conversion slag, washing alkali brick slag with boiled water, putting the alkali brick slag into an acid decomposition tank containing hydrochloric acid with the concentration of 5mol/L, keeping the liquid-solid ratio at 3:1, carrying out leaching reaction at the temperature of 60 ℃, carrying out residual acid concentration of 0.7mol/L after reaction, and filtering to obtain rare earth feed liquid with the concentration of 32.08g/L, wherein the rare earth leaching rate is 99.36%.
EXAMPLE III
Taking 5.0kg of rare earth organic slag, wherein the content of REO is 32.38 wt%, putting 5.0kg of organic slag into a container containing water, the liquid-solid ratio is 1.18, stirring to obtain a slurry, adding caustic soda flakes into the container, the mass ratio of the caustic soda flakes to the rare earth organic slag is 0.3, carrying out alkali conversion on the slurry and the caustic soda flakes for 2.5 hours at the temperature of 85 ℃ to obtain alkali conversion slag, washing the alkali brick slag with boiled water, putting the alkali brick slag into an acid decomposition tank with the hydrochloric acid concentration of 5.5mol/L, keeping the liquid-solid ratio at 4:1, carrying out leaching reaction at the temperature of 60 ℃, the residual acid concentration after the reaction is 0.6mol/L, and filtering to obtain rare earth feed liquid with the rare earth concentration of 44.56g/L, wherein the leaching rate of the rare earth is 99.49%.
Example four
Taking 8.0kg of rare earth organic slag, wherein the content of REO is 36.79 wt%, putting 8.0kg of organic slag into a container containing water, the liquid-solid ratio is 1.14, stirring to obtain a slurry, adding caustic soda flakes into the container, the mass ratio of the caustic soda flakes to the rare earth organic slag is 0.2, carrying out alkali conversion on the slurry and the caustic soda flakes for 3 hours at the temperature of 75 ℃ to obtain an alkali conversion slag, washing the alkali brick slag with boiled water, putting the alkali brick slag into an acid decomposition tank containing hydrochloric acid with the concentration of 5.8mol/L, keeping the liquid-solid ratio at 4.5:1, carrying out leaching reaction at the temperature of 60 ℃, the residual acid concentration after the reaction is 0.8mol/L, and filtering to obtain rare earth feed liquid with the concentration of 55.89g/L, wherein the leaching rate of the rare earth is 99.28%.
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 (9)
1. A method for extracting rare earth from rare earth organic slag is characterized by comprising the following steps:
S1placing the rare earth organic slag in a container filled with water, and stirring the rare earth organic slag in one direction by using a stirring shovel to obtain slurry;
S2to step S1Adding flake caustic soda into the container, and stirring in one direction by using a stirring shovel to ensure that the step S1Carrying out alkali conversion on the slurry obtained in the step (1) to obtain alkali-converted slag;
S3for step S2Washing the alkali-converted slag obtained in the step (1), and then putting the washed alkali brick slag into an acid decomposition tank for leaching to obtain rare earth feed liquid;
S4step S3The obtained rare earth feed liquid is returned to the rare earth separation production flow for recycling.
2. The method for extracting rare earth from rare earth organic slag according to claim 1, wherein the step S1The mass ratio of the medium rare earth organic slag to the water is 1: 1-1: 2.
3. The method for extracting rare earth from rare earth organic slag according to claim 1, wherein the step S2The mass ratio of the addition amount of the sodium mesoflake to the rare earth organic slag is as follows: 0.1 to 0.4.
4. The method for extracting rare earth from rare earth organic slag according to claim 1, wherein the step S2The temperature of medium-alkali conversion is 70-95 ℃.
5. The method of claim 1, wherein the rare earth is extracted from the rare earth organic slag,said step S2The time for medium-alkali conversion is 0.5-3 h.
6. The method for extracting rare earth from rare earth organic slag according to claim 1, wherein the step S3The concentration of hydrochloric acid in the medium acid decomposition tank is 4-6 mol/L.
7. The method for extracting rare earth from rare earth organic slag according to claim 1, wherein the step S3The temperature of the reaction between the alkali transfer slag washed by the reclaimed water and hydrochloric acid in the acid decomposition tank is 60 ℃.
8. The method for extracting rare earth from rare earth organic slag according to claim 1, wherein the step S3The liquid-solid ratio of the hydrochloric acid in the medium-acid decomposition tank to the alkali-converted slag is 2: 1-5: 1.
9. The method for extracting rare earth from rare earth organic slag according to claim 1, wherein the step S3The concentration of the residual hydrochloric acid after the alkali transfer slag washed by the water reacts with the hydrochloric acid in the acid decomposition tank is 0.5-1 mol/L.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113061756A (en) * | 2021-03-17 | 2021-07-02 | 赣州齐畅新材料有限公司 | Method for extracting rare earth from rare earth organic slag |
| CN115418504A (en) * | 2022-08-25 | 2022-12-02 | 萍乡鑫森新材料有限责任公司 | Method for extracting rare earth from rare earth organic slag |
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| CN104862505A (en) * | 2015-06-05 | 2015-08-26 | 乐山盛和稀土股份有限公司 | Method for recycling organic phase from rare earth extract dregs |
| 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 |
| CN106636689A (en) * | 2017-01-04 | 2017-05-10 | 江西理工大学 | Method for extracting rare earth from precipitation sludge of rare earth wastewater pool |
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2020
- 2020-05-20 CN CN202010432709.4A patent/CN111593213A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104862505A (en) * | 2015-06-05 | 2015-08-26 | 乐山盛和稀土股份有限公司 | Method for recycling organic phase from rare earth extract dregs |
| CN106636689A (en) * | 2017-01-04 | 2017-05-10 | 江西理工大学 | Method for extracting rare earth from precipitation sludge of rare earth wastewater pool |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113061756A (en) * | 2021-03-17 | 2021-07-02 | 赣州齐畅新材料有限公司 | Method for extracting rare earth from rare earth organic slag |
| CN115418504A (en) * | 2022-08-25 | 2022-12-02 | 萍乡鑫森新材料有限责任公司 | Method for extracting rare earth from rare earth organic slag |
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