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Carburizing chlorination process for extracting and separating cerium and non-Ce rare earth from rare-earth ore

A technology of rare earth compounds and rare earths, which is applied in the field of carbochlorination to extract and separate cerium and non-cerium rare earths from rare earth minerals. Problems such as inability to be effectively separated out, to achieve the effect of being beneficial to operation, realizing large-scale industrial production, and being easy to large-scale industrial production

Inactive Publication Date: 2005-05-04
NORTHEASTERN UNIV LIAONING
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to create a carbon-added chlorination process to extract and separate cerium and non-cerium rare earth element compounds from rare earth minerals, and to overcome the inability to connect the extraction and separation processes of the above two background technologies, and the alkaline earth in the minerals The problem that metals and radioactive elements cannot be effectively separated will affect the production of subsequent processes and the use of products

Method used

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  • Carburizing chlorination process for extracting and separating cerium and non-Ce rare earth from rare-earth ore

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Bastnaesite - monazite mixed concentrate, main chemical composition (%): REO (65.2), TFe (1.7), CaO (3.3), BaO (1.1), ThO 2 (0.2), Nb 2 o 5 (0.1), F(5.4), P(3.1), S(0.4), SiO 2 (0.6), the atomic ratio of cerium and non-cerium rare earth elements in the rare earth elements is 1.0.

[0023] After mixing 10 grams of concentrate with a particle size of 19 microns and 1.0 grams of activated carbon, react with chlorine and silicon tetrachloride at 550 ° C for 2 hours at an input rate of 0.15 grams and 1.5 milligrams per minute, respectively, fluorine, sulfur, phosphorus , iron and niobium are discharged in the form of gas or low-boiling volatiles.

[0024] The solid product was dissolved in water and then filtered, and sulfuric acid and barium chloride were added to the filtrate to co-precipitate and radium was filtered off. After the solution was evaporated to dryness, it was reacted with industrial oxygen at 700°C for half an hour. After condensation, it was dissolved in...

Embodiment 2

[0027] Bastnaesite concentrate, main chemical composition (%): REO(64.3), TFe(0.3), CaO(0.4), BaO(0.2), Al 2 o 3 (0.2), ThO 2 (0.3), F(10), SiO 2 (0.9); the atomic ratio of cerium and non-cerium elements in rare earth elements is 0.85.

[0028] This is an example of high fluorine content in the raw material, therefore, the gas flow with high silicon tetrachloride content is used when the concentrate is chlorinated. After mixing 10 grams of concentrated ore with a particle size of 22 microns and 1.0 gram of activated carbon, at 550 ° C, react with chlorine gas and silicon tetrachloride with input speeds of 0.15 grams and 2.5 milligrams per minute respectively for 2 hours. Exhaust as gas or low-boiling volatiles.

[0029] After replacing the collector, the chlorinated product is heated up to 800°C in a chlorine atmosphere, and at this temperature, the input rate is 0.1 grams of aluminum chloride per minute to react for half an hour, thorium and aluminum are transported in th...

Embodiment 3

[0034] Bastnaesite medium ore, main chemical composition (%): REO (16.8), TFe (2.6), MgO (1.7), CaO (6.4), BaO (11.2), Al 2 o 3 (10.7), PbO(0.6), ThO 2 (0.2), F(2.8), P(0.4), SiO 2 (41.6) The atomic ratio of cerium and non-cerium elements in the rare earth elements is the same as in Example 2.

[0035] This is an example where the rare earth content in the raw material is low and the content of elements such as silicon and alkaline earth metals is high.

[0036] For medium ore with a particle size of 35 microns, after dolomite and other carbonate minerals are dissolved out with dilute acid, 10 grams of dry mineral powder and 1.5 grams of activated carbon are mixed, and at 550 ° C, the input speed is 0.15 grams per minute. React with 1.5 mg of chlorine and silicon tetrachloride for 2 hours, filter the reaction product after soaking in water, and filter out a large amount of unreacted substances. Add sulfuric acid to the aqueous solution to remove radium.

[0037] After the...

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Abstract

The present invention is a carbochlorination process for extracting rare earth elements from rare earth minerals and effectively separating various rare earth elements; it consists of four technical operations, and realizes the chemical metallurgical purpose of extracting and separating rare earth elements; these four The technical operations are: 1. Low-temperature carbon chlorination and adding defluorinating agent, selective chlorination and effective separation of fluorine, phosphorus, iron and other non-rare earth elements from minerals; 2. High-temperature chlorination-- Chemical vapor transport and water dissolution are two different methods to separate radioactive elements in rare earth minerals, and then the alkaline earth metal elements in minerals are separated by oxygen-rich humid air oxidation and water dissolution; 3. Separation of cerium and cerium by dilute acid leaching Non-cerium rare earth elements; 4. Separation of non-cerium rare earth elements by chemical vapor transport method. The invention is suitable for extracting and separating rare earth elements from various fluorine-containing or non-fluorine-containing rare earth ores and rare earth industrial waste, can comprehensively utilize the valuable components and prevent radioactive pollution.

Description

Technical field [0001] Extraction and separation of rare earth elements in chemical metallurgy. Background technique [0002] High temperature plus carbochlorination (1000-1200°C) to treat bastnaesite concentrate was once proposed by German Goldschmidt company and applied to industrial production. The method has the advantages of simple and mature procedure, less consumption of chemical raw materials, etc., and is applicable to various rare earth concentrates. There is only one kind of product, that is, anhydrous mixed rare earth chloride, which can be directly sent to the molten salt electrolysis process to produce mixed rare earth metals. The main disadvantages of this method are: ① the produced product contains a large amount of fluorine and alkaline earth metal elements, the presence of a large amount of fluorine reduces the yield of rare earth chloride, and it is not easy to connect with the subsequent rare earth separation process; a large amount of alkaline earth met...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B59/00
Inventor 王之昌张丽清
Owner NORTHEASTERN UNIV LIAONING
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