Method for preparing rare-earth phosphorate

A rare-earth phosphate and rare-earth carbonate technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of high reaction conditions and equipment requirements, difficulty in large-scale application, etc., and achieve easy filtration and washing, simple process, and easy operation simple effect

Inactive Publication Date: 2017-01-11
淄博包钢灵芝稀土高科技股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The subsequent dehydration and drying of these particles cannot be handled by simple dehydration and drying equipment, so these production processes have high requirements on reaction conditions and equipment, and are difficult to be used in large-scale production.

Method used

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  • Method for preparing rare-earth phosphorate
  • Method for preparing rare-earth phosphorate
  • Method for preparing rare-earth phosphorate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Get the high-purity lanthanum carbonate produced by Zibo Baotou Steel Ganoderma Lucidum Rare Earth Reprocessing Workshop, and follow the steps below:

[0032] (1) Add 2000mL of pure water into a 5000mL beaker, start stirring, and add 500 grams of high-purity lanthanum carbonate to obtain a suspension of lanthanum carbonate.

[0033] (2) Slowly add 28% phosphoric acid into the suspension of lanthanum carbonate at room temperature under continuous stirring until the pH value is 1.5.

[0034] (3) Stir continuously for 30 minutes, the detected pH value is still 1.5, and the reaction reaches the end point.

[0035] (4) Suction filter the precipitate, wash 5 times with pure water, and obtain the lanthanum phosphate product.

[0036] The prepared lanthanum phosphate product was dried in a 90-degree oven, and the particle size was detected. The test results are shown in Table 1, and the particle size distribution curve is shown in figure 1 .

Embodiment 2

[0038] Get the lanthanum, cerium and terbium carbonate produced by Zibo Baotou Steel Ganoderma lucidum rare earth research and development center, and follow the steps below:

[0039] (1) Add 1000mL of pure water into a 5000mL beaker, start stirring, and add 100 grams of lanthanum cerium carbonate to obtain a suspension of lanthanum cerium terbium carbonate.

[0040] (2) Slowly add 42% phosphoric acid to the suspension of lanthanum, cerium and terbium carbonate at room temperature under continuous stirring until the pH value is 1.0.

[0041] (3) Continue to stir for 10 minutes, and detect that the pH value is 1.5, and the reaction reaches the end point.

[0042] (4) Suction filter the precipitate, wash with pure water 6 times to obtain the lanthanum cerium terbium phosphate product.

[0043] Dry the prepared lanthanum cerium terbium phosphate in a 90-degree oven to detect the particle size. The test results are shown in Table 1, and the particle size distribution curve is sho...

Embodiment 3

[0045] Get the neodymium carbonate produced by Zibo Baotou Steel Ganoderma lucidum rare earth post-processing workshop, and follow the steps below:

[0046] (1) Add 2000L of pure water to a 5000L reactor, start stirring, add 500 kg of neodymium carbonate to obtain a suspension of neodymium carbonate.

[0047] (2) Slowly add 20% ammonium dihydrogen phosphate to the neodymium carbonate suspension under constant stirring at room temperature until the pH value is 4.5.

[0048] (3) Stirring was continued for 10 minutes, the detected pH value rose to 5.5, and 40% phosphoric acid was added to make the pH value 4.5. Stirring was continued for 30 minutes, the detected pH value was still 4.5, and the reaction reached the end point.

[0049] (4) Centrifuge and dehydrate the precipitate, rinse it with pure water for 15 minutes, and obtain the neodymium phosphate product.

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Abstract

The invention belongs to the technical field of rare earth chemical engineering and particularly relates to a method for preparing rare-earth phosphorate. The method for preparing rare-earth phosphorate comprises the following steps that firstly, a rare-earth carbonate or rare-earth oxide suspension with the concentration of 10-1000 g/L is prepared; secondly, a precipitator is added into the suspension under continuous stirring at the room temperature until the pH value is smaller than or equal to 5; thirdly, stirring continues for 5-30 min, the reaction endpoint is reached when it is observed that the pH does not rise any more, if in the stirring process, the pH rises to 2 or above, the precipitator is supplemented until the pH is smaller than or equal to 5, and stirring and observation are carried out until the reaction endpoint is reached; fourthly, precipitation, dehydration and washing are carried out, and rare-earth phosphorate is obtained. According to the method, rare-earth phosphorate obtained through precipitation is large in particle size and easy to filter and wash with water; compared with preparation with a hydrothermal reaction and a solid-phase reaction, the method is relatively easy to implement, and certain industrial popularization meaning is achieved.

Description

technical field [0001] The invention belongs to the technical field of rare earth chemical industry, and in particular relates to a method for preparing rare earth phosphate. Background technique [0002] Rare earth phosphate mainly includes lanthanum phosphate, neodymium phosphate, lanthanum cerium terbium phosphate, and mixed rare earth phosphate, which are important raw materials for the preparation of rare earth fluorescent materials, rare earth lasers and other products. Since rare earth phosphates are easy to form fine colloidal particles during the preparation process, in order to obtain the precipitation of their crystalline particles, they are often prepared by hydrothermal reaction or solid phase reaction in production or experiments, and the obtained rare earth phosphates are generally nano-sized or sub-micron-sized particles. The subsequent dehydration and drying of these particles cannot be handled by simple dehydration and drying equipment, so these production ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37
CPCC01B25/37C01P2004/61C01P2006/60
Inventor 李炳伟牟元璋董云彭欢饶向东龚丽华
Owner 淄博包钢灵芝稀土高科技股份有限公司
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