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Preparation method of pollucite sub-microspheres with kilogram yield grade

A cesium garnet, sub-micron technology, applied in the direction of aluminum silicate, silicate, etc., can solve the problems of quartz with many impurities and not suitable for preparation, and achieve the effects of simple preparation process, environmental protection and low energy consumption

Active Publication Date: 2017-11-17
SOUTHWEAT UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN105905920 A discloses "a method for generating cesium zeolite using soil as a raw material". The cesium zeolite is generated using soil as a raw material. In the reaction kettle, react at a hydrothermal temperature of 100°C to 240°C for 2h to 48h, and after drying, the reaction product cesium zeolite is obtained. The soil used is natural clay material, and the clay mineral provides the seed crystal effect, but the natural soil is used as the The raw materials inevitably lead to more quartz impurities in the synthesized cesium zeolite, which is not suitable for the preparation of regular cesium garnet powder materials

Method used

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  • Preparation method of pollucite sub-microspheres with kilogram yield grade
  • Preparation method of pollucite sub-microspheres with kilogram yield grade
  • Preparation method of pollucite sub-microspheres with kilogram yield grade

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Experimental program
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Effect test

Embodiment 1

[0027] A preparation method of kilogram output level cesium garnet submicron spheres, the steps are: according to the molar ratio Cs:Al:Si=1:1:2, carry out batching, weigh amorphous silica, amorphous alumina, metakaolin , cesium hydroxide monohydrate, and added to (can be 20L, the same below) in the autoclaved reaction kettle with a built-in stirrer (or stirring blade, the same below); according to the solid raw material amorphous silica, amorphous oxidation The total weight of aluminum, metakaolin and cesium hydroxide monohydrate: deionized water is the weight ratio of 1:18 to take deionized water, join in the autoclave reactor and become liquid-solid mixture (the liquid level after adding deionized water reaches About 2 / 3 of the volume of the autoclaved reactor), close the autoclaved reactor; set the stirring speed at 60-100 rpm; crystallize in a hydrothermal environment with a temperature of 140 ° C and a pressure of 0.3-0.8 MPa for 10 hours and then cool Take it out, wash ...

Embodiment 2

[0029]A preparation method of kilogram output level cesium garnet submicron spheres, the steps are: according to the molar ratio Cs:Al:Si=1:1:2, carry out batching, weigh amorphous silica, amorphous alumina, metakaolin , cesium hydroxide monohydrate, and added to (20L) built-in autoclaved reactor with stirring blade; according to the total weight of solid raw material amorphous silica, amorphous alumina, metakaolin and cesium hydroxide monohydrate: The weight ratio of deionized water is 1:18. Take deionized water and add it to the autoclaved reactor to form a liquid-solid mixture (the liquid level after adding deionized water reaches about 2 / 3 of the volume of the autoclaved reactor), close Autoclave reaction kettle; set the stirring speed at 60-100 rpm; crystallize in a hydrothermal environment with a temperature of 160°C and a pressure of 0.3-0.8 MPa for 11 hours, then take it out after cooling, wash and dry to obtain cesium garnet submicron spheres.

Embodiment 3

[0031] A preparation method of kilogram output level cesium garnet submicron spheres, the steps are: according to the molar ratio Cs:Al:Si=1:1:2, carry out batching, weigh amorphous silica, amorphous alumina, metakaolin , cesium hydroxide monohydrate, and added to (20L) autoclaved reaction kettle with built-in stirring blade; according to the total weight of solid raw material amorphous silica, amorphous alumina, metakaolin and cesium hydroxide monohydrate: to The weight ratio of ionized water is 1:18. Take deionized water and add it to the autoclaved reactor to form a liquid-solid mixture (the liquid level after adding deionized water reaches about 2 / 3 of the volume of the autoclaved reactor), close the steamer Press the reaction kettle; set the stirring speed at 60-100 rpm; crystallize in a hydrothermal environment with a temperature of 180°C and a pressure of 0.3-0.8 MPa for 13 hours, then take it out after cooling, wash with water, and dry to obtain cesium garnet submicron ...

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Abstract

The invention discloses a preparation method of pollucite sub-microspheres with kilogram yield grade. The preparation method is characterized by comprising the following steps: firstly, taking solid raw materials such as amorphous silica, amorphous alumina, metakaolin and cesium hydroxide monohydrate, and adding the solid materials into a autoclaved reaction kettle; secondly, taking deionized water according to the weight ratio of the solid materials to the deionized water being 1 to (15 to 20) and then adding the deionized water into the autoclaved reaction kettle; thirdly, reacting for 4 to 20 hours under the conditions that the temperature is 140 to 200 DEG C, the pressure is 0.3 to 0.8MPa and the stirring speed is 60 to 100r / min, then cooling and filtering; washing solids with water and then drying to obtain the pollucite sub-microspheres. According to the preparation method disclosed by the invention, synthesis and preparation of the pollucite sub-microspheres with the kilogram grade under mild conditions are realized; the preparation method is suitable for industrial scale production. The prepared pollucite sub-microspheres can be used for preparing a ceramic container for storing a cesium radioactive source core material or radioactive wastes, and also can be used for high-temperature-resisting ceramics in the field of aerospace.

Description

technical field [0001] The invention belongs to inorganic chemistry and relates to a method for preparing a kilogram output level cesium garnet submicron sphere. The cesium garnet submicron spheres prepared by the invention can be used to prepare cesium radioactive source core materials or ceramic containers for radioactive waste storage, and can also be used for high-temperature-resistant ceramics in the aerospace field, and have wide application prospects in the field of national defense and military industry. Background technique [0002] Cesium garnet is also known as cesium zeolite, and its theoretical chemical structure is CsAlSi 2 o 6 , is the main natural mineral form of cesium (Cs) that exists stably, and its crystal structure is composed of (Al,Si)O 4 The framework of the tetrahedral network structure is composed of Cs ions distributed in parallel channels in the <111> direction, which can theoretically accommodate more than 40wt% of Cs. Cesium garnet has ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/26
CPCC01B33/26C01P2002/72C01P2004/03C01P2004/32C01P2004/62
Inventor 李军侯莉卢忠远牛云辉
Owner SOUTHWEAT UNIV OF SCI & TECH
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