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Preparation technology of zirconium tetrachloride and zirconium dioxide

A technology of zirconium tetrachloride and preparation process, applied in zirconium oxide, zirconium halide and other directions, can solve the problems of low automation level, low efficiency, large waste acid discharge and so on

Active Publication Date: 2019-07-26
XINJIANG JINGSHUO NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Alkali fusion process also has obvious shortcomings. The prominent problem is that the discharge of waste acid, waste alkali and waste residue is large, causing serious environmental pollution. In addition, there are still problems such as discontinuous production process, low efficiency, large energy consumption, and automation. Problems such as low level

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  • Preparation technology of zirconium tetrachloride and zirconium dioxide

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Experimental program
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Effect test

Embodiment 1

[0036] The present embodiment provides a kind of preparation technology of zirconium tetrachloride, comprises the following steps:

[0037] 1) Add zircon sand, carbon reducing agent, and chlorine gas into the first-stage fluidized chlorination furnace, heat, and a first-order chlorination reaction occurs to generate zirconium tetrachloride, silicon tetrachloride, carbon monoxide, and carbon dioxide to obtain the first gas mixture ; The first gas mixture includes zirconium tetrachloride, silicon tetrachloride, carbon monoxide, carbon dioxide.

[0038] 2) Separate carbon monoxide from the first gas mixture, pass carbon monoxide into the secondary boiling chlorination furnace, add zircon sand and chlorine gas into the secondary boiling chlorination furnace, heat, and the secondary chlorination reaction occurs to form zirconium tetrachloride, silicon tetrachloride, and carbon dioxide to obtain a second gas mixture. The second gas mixture includes zirconium tetrachloride, silicon ...

Embodiment 2

[0042] Such as figure 1 Shown, present embodiment provides a kind of preparation technology of zirconium tetrachloride, comprises the following steps:

[0043] 1) Add zircon sand, carbon reducing agent, additives, and chlorine gas into the first-stage fluidized chlorination furnace. The mass ratio of zircon sand to additive is 6:1, and the mass ratio of zircon sand to carbon reducing agent is 8:1. , the feed rate of solid material is 10kg / h, and the feed rate of chlorine gas is 25kg / h into the first-stage boiling chlorination furnace. When heated to 1200°C, a first-order chlorination reaction occurs to generate zirconium tetrachloride, tetrachloride silicon dioxide, carbon monoxide, and carbon dioxide to obtain a first gas mixture. The first gas mixture includes 10%-25% by volume of zirconium tetrachloride, 10%-35% of silicon tetrachloride, 10%-50% of carbon monoxide, 10%-20% of carbon dioxide, and a small amount of chlorinated Aluminum, titanium chloride and other impuritie...

Embodiment 3

[0066] This embodiment provides a kind of preparation technology of zirconium tetrachloride, and the difference with the preparation technology of zirconium dioxide in embodiment 2 is:

[0067] In step 1), the mass ratio of zircon sand to additive is 7:1, the mass ratio of zircon sand to carbon reducing agent is 7:1, and the feed rate of solid material added to the first-stage fluidized chlorination furnace is 100kg / h, the feed rate of chlorine gas is 22kg / h, heated to 1250°C, the additives are silicon carbide and ferrosilicon (mass ratio is 1:1), and the carbon reducing agent is petroleum coke;

[0068] The mass ratio of zircon sand and additive in step 2) is 7:1, and the feeding rate of adding solid material in the secondary boiling chlorination furnace is 10kg / h, and the chlorine gas feeding rate is 20kg / h, and the feeding rate of carbon monoxide The rate is 12kg / h, heated to 1250°C, and the additives are silicon carbide and ferrosilicon (mass ratio 1:1).

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Abstract

The invention discloses preparation processes of zirconium tetrachloride and zirconium dioxide. The preparation process of zirconium tetrachloride comprises the following steps that 1, zircon sand, acarbon reducing agent and chlorine are added into a primary fluidizing chlorination furnace, heating is performed, primary chlorination reaction is performed to generate zirconium tetrachloride, silicon tetrachloride, carbon monoxide and carbon dioxide, and a first gas mixture is obtained; 2, the carbon monoxide is separated from the first gas mixture and is introduced into a secondary fluidizingchlorination furnace, the zircon sand and the chlorine are added into the secondary fluidizing chlorination furnace, heating is performed, secondary chlorination reaction is performed to generate zirconium tetrachloride, silicon tetrachloride and carbon dioxide, and a second gas mixture is obtained. The primary chlorination reaction and secondary chlorination reaction in the process can promote reaction of CO serving as a reducing agent, the CO having reducing potential and produced by the primary chlorination reaction can be fully and effectively utilized by coupling the primary chlorinationreaction and the secondary chlorination reaction, the input of reaction raw materials in the whole process is reduced, accordingly the production cost is reduced, and discharge of greenhouse gas is decreased.

Description

technical field [0001] The invention belongs to the technical field of zirconium tetrachloride production, and in particular relates to a preparation process of zirconium tetrachloride and zirconium dioxide. Background technique [0002] At present, the industrial production of zirconia mainly adopts electric fusion method and alkali fusion method. The production process of producing zirconia by electric melting method is to pass zircon sand and petroleum coke through high-temperature electric arc, zirconium silicate begins to decompose at 1540 ° C, and the decomposition amount increases with the increase of temperature, forming zirconia and dioxide At the same time, carbon captures an oxygen in silicon dioxide to generate carbon monoxide and silicon monoxide gas, and silicon monoxide gas is oxidized into silicon dioxide during the escape process. Electrofusion production has the advantages of short process route, stable quality, and low cost. The main disadvantage is that ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G25/04C01G25/02
CPCC01G25/02C01G25/04
Inventor 银波黄彬范协诚孙永仕刘兴平何隆武珠峰
Owner XINJIANG JINGSHUO NEW MATERIALS CO LTD
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