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Method for preparing zirconium tetrachloride by zircon sand boiling chlorination method and zirconium tetrachloride

A technology of boiling chlorination and zirconium tetrachloride, applied in zirconium halide and other directions, can solve the problems of high production cost, high price of fused zirconia and high technical difficulty

Active Publication Date: 2020-11-13
LIAONING HUAXIANG NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the zircon sand carbonization and chlorination method has been eliminated due to reasons such as high production cost and backward technology; the electric fusion desilication zirconia chlorination method uses desilication zirconia fine powder and carbon reducing agent to mix boiling chlorine Zirconium tetrachloride is prepared by chemical reaction, which has the advantage that the reaction can be carried out at a lower temperature, and the equipment requirements are not too strict, but the price of raw material fused zirconia is relatively high. This method is currently the most mature and widely used production process; The zircon sand boiling chlorination method uses zircon sand as raw material, and chlorine gas is introduced into the fluidized bed reactor to generate silicon tetrachloride and zirconium tetrachloride. This method uses cheap zircon sand as raw material and has a market The valuable silicon tetrachloride greatly reduces the production cost of zirconium tetrachloride, which has a great cost advantage, but the boiling chlorination of zircon sand needs to be reacted at a higher temperature, which requires strict equipment and materials. high technical difficulty

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Grind the zircon sand to 400 mesh, and the carbon reducing agent to 400 mesh, and then mix the zircon powder, desiliconized zirconium, carbon reducing agent, binder and foaming agent according to the ratio of 1:0.1:0.31: 0.052: 0.009% by mass for batching, mixing in the mixer, adding to the kneading granulator for granulation, sieving and selecting materials with a particle size of 50-100 mesh, drying in a dryer at 105°C, and making granules The material is ready for use, and the sieve and under-sieve materials are returned to the granulator for re-granulation treatment; the dried granulated material is put into the boiling chlorination furnace for boiling chlorination reaction, and the reaction chamber of the boiling chlorination furnace adopts a bottom-up The diameter is gradually reduced in the form of a cone, lined with a graphite surface, the reaction chamber is designed to be 4.95 meters high, the upper end diameter is 0.72 meters, and the lower end diameter is 1.2...

Embodiment 2

[0057] The zircon sand is ground to below 325 mesh, the carbon reducing agent is ground to below 450 mesh, and the zircon powder, desiliconized zirconium, carbon reducing agent, binder and foaming agent are mixed according to the ratio of 1:0.05:0.26:0.034:0.015 The mass percentage is used for batching, mixed evenly in the mixer, then added to the kneading and granulating machine for granulation, and the particle size is 30-80 mesh after sieving, and the material is dried at 120 °C in the dryer to make a product with a certain strength. The granules are set aside, and the sieve and sieve materials are returned for re-granulation treatment; the above dried and granulated materials are put into the boiling chlorination furnace for boiling chlorination reaction, and the reaction chamber of the boiling chlorination furnace adopts a gradually increasing diameter from bottom to top. The reduced conical form is lined with a graphite surface. The reaction chamber is designed to be 5.82...

Embodiment 3

[0060] The zircon sand is ground to below 500 mesh, the carbon reducing agent is ground to below 450 mesh, and the zircon powder, carbon reducing agent, binder and foaming agent are mixed according to the mass percentage of 1:0.35:0.063:0.023, After mixing evenly in the mixer, add it to the kneading and granulating machine for granulation. After sieving, the material with a particle size of 30-100 meshes is sent to the dryer and dried at 135 ° C to make a granulated material with a certain strength for later use. and the sieve material are returned for re-granulation treatment; the above dried and granulated materials are put into the boiling chlorination furnace for boiling chlorination reaction. Lined with graphite curved surface, the reaction chamber is designed to be 7.15 meters in height, 0.95 meters in diameter at the upper end, and 1.58 meters in diameter at the lower end. It is heated by an induction coil, and the coil height is 3.35 meters. The temperature in the heat...

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Abstract

The invention relates to a method for preparing zirconium tetrachloride by using a zircon sand boiling chlorination method, and prepared zirconium tetrachloride. The method comprises: (1) mixing various raw materials, and granulating; (2) placing the granulating material obtained in the step (1) in a boiling chlorination furnace reaction chamber, and carrying out a boiling chlorination reaction to obtain a reaction product, wherein the boiling chlorination furnace reaction chamber has a cone cylinder structure having gradually decreased diameter from bottom to top, and in the boiling chlorination reaction, chlorine gas is introduced from a bottom wind distribution plate, the granulating material is fed into the top portion of the boiling chlorination furnace reaction chamber in a screw feeding manner, and the material in the boiling chlorination furnace reaction chamber is controlled to remain in a boiling reaction state; and (3) separating the reaction product to obtain zirconium tetrachloride. According to the present invention, the method has advantages of high product purity, low chlorine gas consumption, less slag in the reaction process, good reaction stability and reduced overall process difficulty.

Description

technical field [0001] The invention relates to inorganic materials, in particular to a method for preparing zirconium tetrachloride by using a zircon sand boiling chlorination method and the prepared zirconium tetrachloride. Background technique [0002] Zirconium tetrachloride prepared by the chlorination method is an important intermediate product in the production of zirconium oxychloride and zirconium sponge. The existing industrial technologies for preparing zirconium tetrachloride mainly include carbonation and chlorination of zircon sand, chlorination of fused desiliconized zirconium dioxide and boiling chlorination of zircon sand. Among them, the zircon sand carbonization and chlorination method has been eliminated due to reasons such as high production cost and backward technology; the electric fusion desilication zirconia chlorination method uses desilication zirconia fine powder and carbon reducing agent to mix boiling chlorine Zirconium tetrachloride is prepare...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G25/04
CPCC01G25/04C01P2006/80
Inventor 石政君包晓刚李小毅叶旦旺胡天喜
Owner LIAONING HUAXIANG NEW MATERIAL CO LTD
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