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 separation 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: 2009-06-17
常州市西南化工研究所 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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

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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: sulfuric acid roasted products of rare earth ore, P204 extractant, kerosene, NH 4 HCO 3 , NH 3 .

[0029] Such as figure 1 with figure 2 As shown, a method for preparing ultrafine high-purity cerium oxide from a sulfuric acid roasted product of a rare earth ore uses the sulfuric acid roasted product of a rare earth ore as a raw material, and the method steps are as follows:

[0030] (1) Ultrasonic leaching-extraction: In an extraction kettle with a probe-type ultrasonic generator, add rare earth ore sulfuric acid roasted product, leaching solution, and extracting solution. The ratio of the three materials is 1000g: 2L: 1L. Operation The condition is that the ultrasonic frequency is 19kHz, the ultrasonic intensity is 0.2W / cm 2 , The operating temperature is 5℃, ultrasonic leachin...

Embodiment 2

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

[0042] Main raw materials: sulfuric acid roasted products of rare earth ore, P204 extractant, sulfonated kerosene, (NH 4 ) 2CO 3 , NH 3 .

[0043] Such as figure 1 with image 3 As shown, a method for preparing ultrafine high-purity cerium oxide from a sulfuric acid roasted product of a rare earth ore uses the sulfuric acid roasted product of a rare earth ore as a raw material, and the method steps are as follows:

[0044] (1) Ultrasonic leaching-extraction: In an extraction tank with a vibrator-type ultrasonic generator, add the sulfuric acid roasted product, leaching liquid, and extracting liquid of rare earth ore. The ratio of the three materials is 1000g:25L:10L, and the operation The conditions are 80kHz ultrasonic frequency and 20.0W / cm ultrasonic intensity 2 , The operating temperature is 60 ℃, ultrason...

Embodiment 3

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

[0056] Main raw materials: sulfuric acid roasted products of rare earth ore, P204 extractant, kerosene, NH 4 HCO 3 , NH 3 .

[0057] Such as figure 1 with Figure 5 As shown, a method for preparing ultrafine high-purity cerium oxide from a sulfuric acid roasted product of a rare earth ore uses the sulfuric acid roasted product of a rare earth ore as a raw material, and the method steps are as follows:

[0058] (1) Ultrasonic leaching-extraction: In the extraction tube with a vibrating plate ultrasonic generator, add the sulfuric acid roasted product, leaching liquid, and extracting liquid of rare earth ore. The ratio of the three materials is 1000g:15L:5L, operation The condition is that the ultrasonic frequency is 25kHz, the ultrasonic intensity is 2.0W / cm 2 , The operating temperature is 40 ℃, ultrasonic le...

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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 oxide, in particular to a method for preparing ultra-fine high-purity cerium oxide from sulfuric acid roasted products of rare earth ore, and belongs to the field of hydrometallurgy. Background technique [0002] Ultrafine high purity cerium oxide Ce 2 O 3 The product refers to the cerium oxide product with cerium oxide content ≥99.99% and particle size ≤10.0μm. Rare earth ore sulfuric acid roasting product is a product obtained by mixing rare earth concentrate (bastnasite or a mixed ore of bastnasite lanthanum and monazite) with concentrated sulfuric acid and roasting. Its main component is soluble sulfuric acid of rare earth and thorium. Salts also include the insoluble concentrated calcium sulfur and the volatile gas hydrogen fluoride or silicon fluoride converted from fluorite, as well as sulfates converted from the decomposition and conversion of minerals such as iron and...

Claims

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Application Information

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Patent Type & Authority Patents(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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