Method for preparing superfine high-purity cerium oxide by using rear earth ore sulfuric acid calcination products

A technology of sulfuric acid roasting and cerium oxide, which is applied in the fields of rare earth metal compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of difficult to meet the requirements of product use, low separation rate and efficiency, uneven particle size distribution, etc. , to achieve the effect of saving fractionation, extraction and separation operating unit devices, increasing extraction rate, and fast extraction rate

Inactive Publication Date: 2007-08-29
常州市西南化工研究所 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the method of leaching and separating rare earth sulfuric acid roasting products to produce high-purity rare earth oxides mainly has the following defects: low rare earth leaching efficiency, long leaching time, low recovery rate, large energy consumption, separation rate and separation The efficiency is low, and there are still problems such as unstable product quality, large amount of "three wastes" treatment, and "poisoning" of the extraction agent.
It is generally difficult to obtain cerium oxide Ce 2 o 3 The content is as high as 99.99% purity, especially the particle size of the product is large, and the particle size distribution is uneven, it is difficult to meet the requirements of the product used in the high-tech field

Method used

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  • Method for preparing superfine high-purity cerium oxide by using rear earth ore sulfuric acid calcination products
  • Method for preparing superfine high-purity cerium oxide by using rear earth ore sulfuric acid calcination products

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Main equipment: extraction kettle with probe-type ultrasonic generator, crystallization kettle with probe-type ultrasonic generator, fixed-bed electrochemical reactor.

[0028] Main raw materials: rare earth mineral sulfuric acid roasting product, P204 extractant, kerosene, NH 4 HCO 3 , NH 3 .

[0029] As shown in Fig. 1 and Fig. 2, a kind of method for preparing superfine high-purity cerium oxide by roasting product of sulfuric acid of rare earth mine is to be raw material by roasting product of sulfuric acid of rare earth mine, and described method step is as follows:

[0030] (1) Ultrasonic leaching-extraction: In the extraction kettle with a probe-type ultrasonic generating device, add the roasted product of rare earth ore sulfuric acid, leaching solution, and extraction solution. The proportion of the three materials is 1000g: 2L: 1L, and the operation The condition is that the ultrasonic frequency is 19kHz, and the ultrasonic action intensity is 0.2W / cm 2 , th...

Embodiment 2

[0041] Main equipment: extraction tank with vibrator-type ultrasonic generator, crystallization tank with vibrator-type ultrasonic generator, fluidized bed electrochemical reactor.

[0042] Main raw materials: rare earth mineral sulfuric acid roasting product, P204 extractant, sulfonated kerosene, (NH 4 ) 2 CO 3 , NH 3 .

[0043]As shown in Fig. 1 and Fig. 3, a kind of method for preparing superfine high-purity cerium oxide by roasting product of sulfuric acid of rare earth mine is to be raw material by roasting product of sulfuric acid of rare earth mine, and described method step is as follows:

[0044] (1) Ultrasonic leaching-extraction: In the extraction tank with a vibrator-type ultrasonic generator, add the roasted product of rare earth ore sulfuric acid, leaching solution, and extraction solution. The ratio of the three materials is 1000g: 25L: 10L, and the operation The condition is that the ultrasonic frequency is 80kHz, and the ultrasonic action intensity is 20.0...

Embodiment 3

[0055] Main equipment: extraction tube with vibrating plate ultrasonic generator, crystallization tube with vibrating plate ultrasonic generator, fixed bed electrochemical reactor.

[0056] Main raw materials: rare earth mineral sulfuric acid roasting product, P204 extractant, kerosene, NH 4 HCO 3 , NH 3 .

[0057] As shown in Fig. 1 and Fig. 5, a kind of method for preparing superfine high-purity cerium oxide by roasting product of sulfuric acid of rare earth mine is to be raw material by roasting product of sulfuric acid of rare earth mine, and described method step is as follows:

[0058] (1) Ultrasonic leaching-extraction: In the extraction tube with a vibrating plate type ultrasonic generating device, add the roasted product of rare earth ore sulfuric acid, leaching solution, and extraction solution. The proportion of the three materials is 1000g: 15L: 5L, and the operation The condition is that the ultrasonic frequency is 25kHz, and the ultrasonic action intensity is ...

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Abstract

The invention relates to a method to make high purity cerium oxide that includes the following steps: taking ultrasonic leaching and extraction to gain rare earth sulfate enriched liquid; taking solid-liquid separation; taking neutralization deposition, taking solid-liquid separation, taking electrochemistry oxide to gain quadravalence cerous sulfate material liquid, taking ultrasonic fractional extraction, taking electrochemistry reducing to gain trivalence cerous sulfate, taking ultrasonic crystallization deposition to gain cerous sulfate crystal deposition, taking solid-liquid separation, drying and burning to gain the superfine high purity cerium oxide product of content over 99.99%, and the particle diameter is 0.01-10.0um. The advantages of the invention are that it improves leaching and extracting speed, improves yield, and purity, lowers cost and is environment protection.

Description

technical field [0001] The invention relates to a method for separating and preparing high-purity cerium oxides, in particular to a method for preparing ultrafine high-purity cerium oxides from sulfuric acid roasting products of rare earth ores, belonging to the field of hydrometallurgy. Background technique [0002] Ultra-fine high-purity cerium oxide Ce 2 o 3 The product refers to a cerium oxide product with a cerium oxide content ≥ 99.99% and a particle size ≤ 10.0 μm. The sulfuric acid roasting product of rare earth ore is a product obtained by mixing rare earth concentrate (bastnaesite or a mixed ore of bastnaesite and monazite) with concentrated sulfuric acid and then roasting. Its main components are soluble sulfuric acid of rare earth and thorium and other elements. Salt also includes insoluble sulfur-concentrated calcium transformed from fluorite, volatile gas hydrogen fluoride or silicon fluoride, and sulfates formed from the decomposition and transformation of i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00C22B3/00
CPCY02P10/20
Inventor 许文林王雅琼魏晓廷朱金玉魏巍张月
Owner 常州市西南化工研究所
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