Preparation method of large-particle neodymium oxalate

A neodymium oxalate and large particle technology is applied in the field of preparation of large particle neodymium oxalate, which can solve the problems of insufficient particle size of oxides, a large amount of ammonia nitrogen waste water, increase production cost, etc., achieve easy industrial production, reduce production cost, realize The effect of recycling

Inactive Publication Date: 2015-05-27
JIANGXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] It can be seen that some patents use ammonium bicarbonate as a precipitant, which makes it difficult to filter rare earth precipitates, and the particle size of the prepared oxides cannot meet the current industrial needs
Some preparation methods also need to add ammonium chloride, resulting in a large amount of ammonia nitrogen wastewater, polluting the environment and increasing production costs
There is no document or patent report on the method of preparing large-grain neodymium oxalate by using a trace amount of organic phase neodymium chloride strip raffinate as raw material, oxalic acid as precipitant, and adding neodymium oxalate seed crystals

Method used

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  • Preparation method of large-particle neodymium oxalate
  • Preparation method of large-particle neodymium oxalate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1: Take 0.1L of neodymium chloride stripping raffinate with a concentration of 0.2 mol / L, heat it to 35°C, and stir at a speed of 400 r / min. -1 and 1035±25cm -1 The absorption peak (the organic phase composition of the following examples is the same), add 3% neodymium oxalate crystal seeds to the feed liquid, the seed crystal center particle size D 50 oxalic acid solution was added dropwise at a rate of 5ml / min to obtain a precipitate of neodymium oxalate, which was aged for 24 hours, filtered, washed, and dried at 80°C to obtain a central particle size D 50 Neodymium oxalate particles with a particle size of 78.63 μm and a normal distribution.

Embodiment 2

[0029] Embodiment 2: Take 0.5L of neodymium chloride stripping raffinate that concentration is 0.12 mol / L, adjust temperature to 15 DEG C, stirring speed is 300 r / min, add 6% neodymium oxalate seed crystal to feed liquid, crystal Kind of central particle size D 50 oxalic acid solution was added dropwise at a rate of 10ml / min to obtain a precipitate of neodymium oxalate, which was aged for 8 hours, filtered, washed, and dried at 100°C to obtain a central particle size D 50 Neodymium oxalate particles with a particle size of 134.65 μm and a normal distribution.

Embodiment 3

[0030] Example 3: Take 0.1L of neodymium chloride stripping raffinate with a concentration of 0.08 mol / L, heat it to 75°C, and stir at a speed of 200 r / min, add 12% neodymium oxalate seed crystals to the feed liquid, and the seed crystals Center particle size D 50 oxalic acid solution was added dropwise at a rate of 8ml / min to obtain a precipitate of neodymium oxalate, which was aged for 32 hours, filtered, washed, and dried at 90°C to obtain a central particle size D 50 Neodymium oxalate particles with normal particle size distribution of 94.65 μm.

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Abstract

The invention relates to a preparation method of large-particle neodymium oxalate, belonging to the process of powdery materials. The preparation method comprises the following steps: adding an oxalic acid solution serving as a precipitator into neodymium chloride reverse extraction raffinate containing a trace organic phase, adding seed crystals to generate a neodymium oxalate precipitate, aging, washing, filtering and drying to finally obtain neodymium oxalate particles with a central particle size D50 of 55-200mu m, wherein the particle sizes of the neodymium oxalate particles are in normal distribution. The preparation method disclosed by the invention is simple in process and can be put into industrial production easily; the obtained neodymium oxalate can be further used for preparing neodymium oxide with a central particle size D50 of 25-95mu m and uniform particle distribution.

Description

technical field [0001] The invention belongs to the preparation process of powder materials, in particular to a preparation method of large-grain neodymium oxalate whose particle size is normally distributed. Background technique [0002] Neodymium oxide is widely used in the fields of glass, ceramics and magnetic materials, and is an important raw material for the manufacture of metallic neodymium and strong magnetic NdFeB. With the continuous development of science and technology, rare earth oxides with large particle size and uniform particle distribution have attracted more and more attention, and have good market prospects. For example, in the preparation of neodymium metal, in order to reduce the fine particle dust in the workshop and increase the electrolysis yield, it is generally required that the particle size of neodymium oxide reaches 50 μm and the particle distribution is uniform. In the glass industry, in order to increase the refractive index, reduce scatteri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/41C07C51/43C07C55/07
CPCC07C51/412C07C51/43C07C55/07
Inventor 叶信宇杨明焦芸芬杨幼明王瑞祥杨斌
Owner JIANGXI UNIV OF SCI & TECH
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