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Production method of ultra granule yttria

A production method and technology of yttrium oxide, applied in chemical instruments and methods, inorganic chemistry, rare earth metal compounds, etc., can solve the problems of rough surface, high equipment requirements, large particle size, etc., achieve simple production process, improve luminous brightness, The effect of smooth and bright surface

Inactive Publication Date: 2007-09-19
广东省富远稀土有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The physical methods mainly include: 1. Physical crushing method, through mechanical crushing, electric spark explosion, ultrasonic fragmentation, etc. to obtain superfine yttrium oxide, which is characterized by simple operation and low cost, but the product has low purity and uneven particle size distribution. The surface is rough, especially after being crushed, the physical properties of the grains deteriorate and the performance index decreases
2. The mechanical wet ball milling method, under the condition of adding water, ball-mills large particles of yttrium oxide, dehydrates, dries, and roasts. It is characterized by simple operation, but the product has low purity, uneven particle size distribution, and complicated procedures. High equipment requirements and large investment
The chemical methods mainly include: 1. Microemulsion method. Two kinds of immiscible solvents form an emulsion under the action of a surfactant, and form nuclei in microbubbles, coalesce, agglomerate, and heat treat to obtain ultrafine particles. It is characterized by good monodispersity and interfacial properties of particles, and uniform particle size distribution, but its solvent cost is high, the process is complicated, and it is not easy to control
2. Precipitation method, control certain conditions, add precipitant to yttrium solution and react, then filter and burn the precipitate to obtain superfine yttrium oxide, which is characterized by simple operation, low production cost, low equipment requirements, and low investment Small, but the particle size is large and difficult to control, and the particle size distribution is not ideal

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] Get 1000L yttrium chloride solution and use pure water to adjust the concentration to 40g / L, adjust the pH value to 2 with pure ammonia water, and the temperature is 15°C; get 80Kg high-purity oxalic acid, and prepare 1000L of 8% oxalic acid solution with a concentration of 15°C; % volume, that is, 40L of yttrium chloride solution is added to the precipitation reaction pot, the precipitation reaction pot is started to stir, and 1L of polybutanol solution is added. Polybutanol can effectively inhibit the growth of grains and agglomeration adsorption, so that the precipitation system becomes uniform. And do not introduce impurity and influence performance to product; Yttrium chloride solution adds 1 minute earlier than oxalic acid solution, and precipitation time is 10 minutes, calculates that yttrium chloride solution adding speed is 50.53L / min, and concentration 8% oxalic acid solution adding speed is 100L / min, control the yttrium chloride solution and the oxalic acid so...

Embodiment 2

[0012] Take 500L of yttrium chloride solution and adjust the concentration to 100g / L with pure water, adjust the pH value to 2 with pure ammonia water, and the temperature is 25°C; take 110kg of high-purity oxalic acid, and prepare 1100L of oxalic acid solution with a concentration of 10%, and the temperature is 25°C; % volume, that is, 30L of yttrium chloride solution is added to the precipitation reaction tank, the precipitation reaction tank is started to stir, and 1.5L of polybutanol solution is added; the yttrium chloride solution is added 2 minutes earlier than the oxalic acid solution, and the precipitation time is 20 minutes. The adding speed of the yttrium chloride solution is 26.11L / min, and the adding speed of the 10% oxalic acid solution is 55L / min, and the yttrium chloride solution and the oxalic acid solution are simultaneously added to the precipitate at the calculated adding speed by the pump, valve and rotameter. In the reaction tank, after adding the oxalic ac...

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Abstract

The present invention provides a preparation method of superfine yttrium oxide. The yttrium oxide solution and oxalic acid solution are subjected to homogeneous precipitation in a co-precipitation manner with an error of 4~6% and a reaction time of 10~20 minutes; wherein the yttrium oxide solution has a concentration of 40~100 g / l, a pH value of 2 and a temperature of 15~25 DEG C; the oxalic acid solution has a concentration of 8~10% and a temperature of 15~25 DEG C. Then, polybutanol serving as dispersant is added into the homogeneous precipitation solution, wherein the dosage of polybutano is 0.1~0.3% by volume of the total amount of the precipitation solution, and the obtained precipitation solution is filtered for 10~20 minutes to separate the mother liquor and the precipitate, then the precipitate is scrubbed for 3~5 times, filtered, and roasted at 850~900 DEG C for 3~3.5 hours, thereby, the superfine yttrium oxide (D50 less than 1 um)is obtained. The present invention has the advantages of simple manufacturing technique, high product quality, excellent size distribution, uniform particle displayed under ultramicroscope, smooth and shining surface, no hardened layer, excellent physical property; besides, when the superfine yttrium oxide is used for fluorescent powder, the light colour is good, the light wane and the color temperature are excellent.

Description

technical field [0001] The invention belongs to the field of new materials and relates to a production method of ultrafine yttrium oxide. Background technique [0002] The particle size and other physical properties of yttrium oxide directly affect the quality and application of downstream products. Ultrafine yttrium oxide has attracted much attention because of its excellent performance in the fields of light, electricity, and physical and chemical reactions. At present, the production of superfine particle center particle size D 50 = 0.1 ~ 1μm yttrium oxide methods, mainly physical and chemical methods. The physical methods mainly include: 1. Physical crushing method, through mechanical crushing, electric spark explosion, ultrasonic fragmentation, etc. to obtain superfine yttrium oxide, which is characterized by simple operation and low cost, but the product has low purity and uneven particle size distribution. The surface is rough, especially after crushing, the physica...

Claims

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Application Information

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IPC IPC(8): C01F17/00
Inventor 杨金华韩旗英韩新福韩德义凌诚
Owner 广东省富远稀土有限公司