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Improved preparation method of zirconium tetrachloride and zirconium tetrachloride

A technology of zirconium tetrachloride and silicon tetrachloride, applied in the direction of zirconium halide, etc., can solve the problem of difficult removal of metal impurities, achieve the effect of reducing the difficulty of separation and purification, improving purity and quality, and improving purity

Inactive Publication Date: 2018-11-13
XINTE ENERGY +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The technical problem to be solved by the present invention is to provide a kind of preparation method of improved zirconium tetrachloride and zirconium tetrachloride, solve the removal of metal impurities in the zirconium tetrachloride product that generates difficult question

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  • Improved preparation method of zirconium tetrachloride and zirconium tetrachloride
  • Improved preparation method of zirconium tetrachloride and zirconium tetrachloride
  • Improved preparation method of zirconium tetrachloride and zirconium tetrachloride

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Embodiment 1

[0044] The present embodiment provides a kind of preparation method of improved zirconium tetrachloride, comprises the following steps:

[0045]1) The zircon sand contains metal oxide impurities, and the metal oxide impurities in the zircon sand are removed to obtain purified zircon sand;

[0046] 2) Heating the purified zircon sand with a carbonaceous reducing agent and chlorine gas to react to generate a mixed gas of zirconium tetrachloride, silicon tetrachloride, carbon monoxide and carbon dioxide. Separate the mixed gas to obtain zirconium tetrachloride.

[0047] The improved zirconium tetrachloride preparation method in this example first removes the metal oxide impurities in the zircon sand, and then reacts with carbonaceous reducing agent and chlorine gas, which greatly reduces the obtained zirconium tetrachloride product. The content of the chloride of metal impurity in the middle, has avoided the chloride of metal impurity mixed in the zirconium tetrachloride product...

Embodiment 2

[0049] Such as figure 1 As shown, the present embodiment provides a kind of device for preparing zirconium tetrachloride, comprising:

[0050] Impurity removal reactor 1, zircon sand and reaction gas are mixed in the impurity removal reactor 1, the reaction gas is chlorine and hydrogen chloride, the impurity removal reactor 1 is heated, and the metal oxide impurities in the zircon sand react with the reaction gas to form a gaseous state The metal chloride, obtains purified zircon sand, first syngas, the first syngas comprises gaseous metal chloride;

[0051] The outside of the impurity removal reactor 1 is made of 800H alloy steel (nickel-based alloy), and the inner lining is zirconia and silicon nitride ceramic anticorrosion layer. The outside is equipped with an induction heater and a temperature controller. The internal temperature and the current of inductive heating are controlled in a cascade loop, which is used to control the temperature of the impurity removal reactor...

Embodiment 3

[0082] This embodiment provides a kind of preparation method of the improved zirconium tetrachloride using the device in embodiment 2, and the difference of the preparation method of the improved zirconium tetrachloride in embodiment 2 is:

[0083] The molar ratio of chlorine and hydrogen chloride in the reaction gas in step 2) is 4:1, and the impurity removal reactor is heated to 400°C for 5 hours,

[0084] In step 4), the mass ratio of zircon sand to carbonaceous reducing agent is 4.5:1, the chlorination reactor is heated to 1200° C., and the pressure is 50KPa. The carbonaceous reducing agent is petroleum coke.

[0085] In step 5), the liquid silicon tetrachloride is passed into the first washing tower from the top to wash the second synthesis gas and lower the temperature to 200°C.

[0086] In step 6), the liquid silicon tetrachloride is passed into the second washing tower from the top to wash the third synthesis gas and lower the temperature to 40°C.

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Abstract

The invention discloses an improved preparation method of zirconium tetrachloride and the zirconium tetrachloride. The preparation method comprises the following steps: 1), removing metal oxide impurities from zircon sand to obtain purified zircon sand; 2), heating the purified zircon sand together with a carbonaceous reducing agent and chlorine gas, reacting to produce zirconium tetrachloride, silicon tetrachloride, carbon monoxide and carbon dioxide and separating the zirconium tetrachloride. According to the preparation method, the metal oxide impurities in the zircon sand are removed firstand then the purified zircon sand reacts with the carbonaceous reducing agent and the chlorine gas, so that the content of chloride of the metal impurities in an obtained zirconium tetrachloride product is greatly reduced and the chloride of the metal impurities is avoided from entering the produced zirconium tetrachloride product, and thus the purity of the zirconium tetrachloride product is improved, the step of removing the chloride of the metal impurities is omitted, the separating and purifying difficulty of a back-end separation system is reduced, the purity and the quality of the zirconium tetrachloride product are improved, and the quality of a back-end product is improved.

Description

technical field [0001] The invention belongs to the technical field of zirconium tetrachloride preparation, and in particular relates to an improved preparation method of zirconium tetrachloride and zirconium tetrachloride. Background technique [0002] Zirconia (ZrO 2 ) is an important ceramic material with superior functions such as high temperature resistance, wear resistance and corrosion resistance. In addition to being used in refractory materials and ceramic pigments, it has become the main raw material for electronic ceramics, functional ceramics and artificial gemstones. The application of science and technology is becoming more and more extensive. [0003] At present, the production methods of zirconia used in industry mainly include electric fusion method, alkali fusion method and chlorination method. The process flow of the electric fusion method is simple, but the quality of the zirconia produced is low; the quality of the product prepared by the alkali fusion...

Claims

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Application Information

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IPC IPC(8): C01G25/04
CPCC01G25/04
Inventor 武珠峰范协诚银波黄彬刘兴平孙永仕何隆
Owner XINTE ENERGY
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