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Method for preparing small-granularity cerium terbium lanthanum phosphate rare earth product with high luminous efficiency

A technology of lanthanum cerium terbium phosphate and high luminous efficiency, which is applied in the field of high luminous efficiency, rare earth phosphate-lanthanum cerium terbium phosphate, and can solve the problem of hard lumps formed by particles that are difficult to sieve, different particle size distribution and crystal morphology, precipitation performance and Poor filtering performance and other problems, to achieve the effect of low production conditions, low price, and good anti-attenuation characteristics

Active Publication Date: 2014-12-03
YIXING XINWEI LEESHING RARE EARTH
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Problems solved by technology

[0005] At present, the common problem in domestic wet synthesis is that the synthesized lanthanum cerium terbium phosphate is often in a gel state, with poor precipitation and filtration properties, especially after high-temperature calcination, it is easy to sinter, and the particles form hard lumps that are difficult to sieve. Compared with foreign products, there is still a gap, and there are also differences in particle size distribution and crystal morphology.

Method used

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  • Method for preparing small-granularity cerium terbium lanthanum phosphate rare earth product with high luminous efficiency

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preparation example Construction

[0014] A method for preparing a rare earth product of lanthanum cerium terbium phosphate with high luminous efficiency and small particle size, comprising the following steps:

[0015] (1) Prepare raw materials: select more than 99.99% LaCl3, CeCl3, TbCl3 as raw materials, and accurately weigh the corresponding raw materials according to the molar ratio required by the following chemical composition formula LaxCeyTb1-x-yPO4; the general chemical composition formula is LaxCeyTb1-x-yPO4 , the value range of x and y is: X is between 0.4 and 0.6, x + y > 0.8, the composition ratio of lanthanum, cerium and terbium is formulated to a concentration of 0.2-0.5 mol / l and a rare earth with an acidity of 0.1-0.2 mol / l Chloride salt or rare earth nitrate solution.

[0016] (2) Precipitation: use 0.5-1.0 mol / l phosphate-containing precipitant solution, add the above-mentioned feed liquid to the bottom liquid at 0.1-1.0 liter / min, and use the phosphate in the precipitant to react with rare ...

Embodiment 1

[0023] Embodiment 1: Mix evenly with the lanthanum chloride, cerium chloride and terbium chloride solution of the required ratio, adjust the concentration of the gained lanthanum chloride cerium terbium solution to 0.2~0.5mol / l, get a certain amount of diammonium hydrogen phosphate and dissolve to obtain A precipitant with a concentration of 0.5-1.0mol / l is added to the reactor with a bottom solution at a temperature of 25°C and an acidity of 0.1N, and at a stirring speed of 200 rpm, inject lanthanum cerium terbium chloride solution and dihydrogen phosphate Ammonium precipitant, the precipitation is carried out in four stages by the automatic feeding control system. At the beginning of the nucleation control stage, the flow rate of the feed liquid is controlled at 0.1 liters / minute, the flow rate of the precipitant is 1.0 liters / minute, and the precipitation time is 30 seconds after the nucleation In the transition control stage, the flow rate of the feed liquid is controlled a...

Embodiment 2

[0024]Embodiment 2: Mix evenly with the lanthanum chloride, cerium chloride and terbium chloride solution of the required ratio, adjust the concentration of the gained lanthanum chloride cerium terbium solution to 0.2~0.5mol / l, get a certain amount of diammonium hydrogen phosphate and dissolve to obtain A precipitant with a concentration of 0.5-1.0mol / l is added to the reactor with a bottom solution at a temperature of 25°C and an acidity of 0.1N, and at a stirring speed of 200 rpm, inject lanthanum cerium terbium chloride solution and dihydrogen phosphate Ammonium precipitant, the precipitation is carried out in four stages by the automatic feeding control system. At the beginning of the nucleation control stage, the flow rate of the feed liquid is controlled at 0.2 liters / minute, the flow rate of the precipitant is 1 liter / minute, and the precipitation time is 30 seconds after the nucleation In the transition control stage, the flow rate of the feed liquid is controlled at 0....

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Abstract

The invention relates to a method for preparing a small-granularity cerium terbium lanthanum phosphate rare earth product with high luminous efficiency. The method comprises the following steps of preparing a 0.2-0.5 mol / l rare earth chloride or nitrate solution and a 0.5-1.0 mol / l precipitant containing phosphate radical; adding the raw materials into a reactor containing a base solution of which the temperature is 30-50 DEG C and the acidity is 0.1-0.5N and reacting; after the precipitation is carried out, aging, washing with water, carrying out vacuum dehydration and microwave drying, sieving and firing to obtain the cerium terbium lanthanum phosphate product. According to the invention, the raw materials are subjected to precipitation, feeding and mixing by virtue of a precision control system, the control process is divided into four stages, the precipitation process is effectively controlled in the four stages, the morphology and performance of a precipitate particle are improved, the product obtained by vacuum filtration, microwave drying and other methods has excellent quality in the aspects of impurities, granularity, the crystal morphology and the like, the method meets the industrial needs and is suitable for being popularized and the preparation is simple.

Description

technical field [0001] The invention relates to a rare earth phosphate-lanthanum cerium terbium phosphate, in particular to a rare earth phosphate-lanthanum cerium terbium phosphate with high luminous efficiency and small particle size and a preparation method thereof. The invention belongs to the field of luminescent lighting and the field of material science and technology. Background technique [0002] The three primary color phosphors currently commercially mainly include lanthanum cerium terbium green powder and magnesium cerium terbium aluminate green powder. Magnesium cerium terbium aluminate occupies the low-end market due to its low price, simple process, and relatively low production condition requirements. ; and lanthanum cerium terbium phosphate (LaPO4: Ce, Tb) is a very important class of high-efficiency green luminescent materials in the trichromatic phosphor. Grasp the high-end market with the advantages of high stability, good anti-attenuation characteristic...

Claims

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Application Information

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IPC IPC(8): C09K11/81
Inventor 李文捷徐建文许鹏盛红赵红星陈家运
Owner YIXING XINWEI LEESHING RARE EARTH
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