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Method for preparing zirconium tetrachloride through fluidizing chlorination of zircon sand with silicon tetrachloride as byproduct

A technology of by-product silicon tetrachloride and zirconium tetrachloride, which is applied in the direction of chemical instruments and methods, zirconium halides, silicon halide compounds, etc., can solve problems such as waste of resources, explosion, and increased consumption of raw materials, so as to improve production capacity, The effect of saving fossil resources and improving the conversion rate

Active Publication Date: 2016-05-11
山东广通新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Not only is it a waste of resources, but also there are safety hazards such as CO combustion, explosion, and poisoning
[0015] 3. CO produced by CO combustion enthalpy 2 , CO 2 It is the main greenhouse gas, which will intensify the greenhouse effect of the atmosphere, lead to global warming, and cause natural disasters, which seriously threaten the survival and development of human beings.
[0016] 4. In the prior art, Cl 2 As the main raw material of the chlorination reaction, due to the lack of recovery and recycling, the consumption of raw materials increases and the production cost of products increases.
[0017] 5. In the prior art, Cl 2 As the main raw material for the chlorination reaction, since there is no recovery and recycling, zircon sand and Cl 2 The molar ratio of zircon sand can only be maintained at about 1:6, which limits the reaction speed of zircon sand chlorination reaction
Affected the improvement of the production capacity of the device

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0071] The method for preparing zirconium tetrachloride by-product silicon tetrachloride by boiling chlorination of a kind of zircon sand of the present invention comprises the following steps:

[0072] ①. Chlorination of zircon sand

[0073] First, crush the quartz sand into a fine powder of 300-350 mesh, mix it with 150-180 mesh petroleum coke and catalyst boron oxide according to the ratio of 100:20-23:0.4-0.5, and add it to the boiling chlorination furnace for chlorination reaction , the molar ratio of zircon sand to chlorine gas is 1:8, the reaction temperature is 950-1100°C, and the controlled chlorine flow rate is 1.0-1.5m3 / h;

[0074] ②. Separation and collection of zirconium tetrachloride

[0075] The gas product from step ① is cooled by a multi-stage condenser, the temperature of the cooled material reaches 210-230°C, and enters the cyclone gas-solid separator for gas-solid separation. When the outlet temperature is controlled at 100-110°C, tetrachloride is separate...

Embodiment 2

[0088] The method for preparing zirconium tetrachloride by-product silicon tetrachloride by boiling chlorination of a kind of zircon sand of the present invention comprises the following steps:

[0089] ①. Chlorination of zircon sand

[0090] First, crush the quartz sand into a fine powder of 300-350 mesh, mix it with 150-180 mesh petroleum coke and catalyst boron oxide according to the ratio of 100:20-23:0.4-0.5, and add it to the boiling chlorination furnace for chlorination reaction , the molar ratio of zircon sand to chlorine gas is 1:9, the reaction temperature is 950-1100°C, and the controlled chlorine flow rate is 1.0-1.5m3 / h;

[0091] ②. Separation and collection of zirconium tetrachloride

[0092]The gas product from step ① is cooled by a multi-stage condenser, the temperature of the cooled material reaches 210-230°C, and enters the cyclone gas-solid separator for gas-solid separation. When the outlet temperature is controlled at 100-110°C, tetrachloride is separated...

Embodiment 3

[0105] The method for preparing zirconium tetrachloride by-product silicon tetrachloride by boiling chlorination of a kind of zircon sand of the present invention comprises the following steps:

[0106] ①. Chlorination of zircon sand

[0107] First, crush the quartz sand into a fine powder of 300-350 mesh, mix it with 150-180 mesh petroleum coke and catalyst boron oxide according to the ratio of 100:20-23:0.4-0.5, and add it to the boiling chlorination furnace for chlorination reaction , the molar ratio of zircon sand to chlorine gas is 1:10, the reaction temperature is 950-1100°C, and the chlorine flow rate is controlled to be 1.0-1.5m3 / h;

[0108] ②. Separation and collection of zirconium tetrachloride

[0109] The gas product from step ① is cooled by a multi-stage condenser, the temperature of the cooled material reaches 210-230°C, and enters the cyclone gas-solid separator for gas-solid separation. When the outlet temperature is controlled at 100-110°C, tetrachloride is s...

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Abstract

The invention relates to a method for preparing zirconium tetrachloride through fluidizing chlorination of zircon sand with silicon tetrachloride as a byproduct. The method is a preparation method of zirconium halide. A system for realizing the method comprises a zircon sand fluidizing chlorination system, a zirconium tetrachloride condensation and collection system and a silicon tetrachloride rectification system, and also comprises a tail gas recycling system; the tail gas recycling system comprises a tail gas storage device, a chlorine separation and recovery device and a CO recovery and storage device; chlorine in separated and collected tail gas is used as a raw material of a zircon sand fluidizing chlorination reaction, and can be recycled; and the chlorine separated tail gas is used as a raw material of an industrial production apparatus for carrying out a CO participated synthesis reaction. The method for preparing zirconium tetrachloride through fluidizing chlorination of zircon sand with silicon tetrachloride as a byproduct, provided by the invention, has the advantages of effective utilization of Cl2 and CO resources, reduction of discharge of the greenhouse gas CO2, reduction of the product production cost of a zircon sand fluidizing chlorination apparatus, and improvement of the productivity of the apparatus.

Description

technical field [0001] The invention relates to a method for preparing zirconium tetrachloride by-product silicon tetrachloride by boiling chlorination of zircon sand. A process for the preparation of zirconium halides. Background technique [0002] Zircon sand is zircon (ZrSiO) obtained by processing and beneficiating zircon minerals. 4 ) concentrate, its theoretical composition is: ZrO 2 Content is 67.21%, SiO 2 The content is 32.79%. Zircon sand is the main raw material for the production of metal zirconium and its chemical products. For the preparation of silicon tetrachloride, zirconium oxychloride and zirconium dioxide. [0003] Zirconium tetrachloride ZrCl 4 , is the main raw material for preparing other zirconium products, such as zirconium sponge, zirconium oxychloride, etc. It is also a catalyst for organic synthesis. [0004] At present, the main source of silicon tetrachloride is the by-products of the organic silicon industry and polysilicon industry. Du...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/04C01B33/107C01B31/18C01B32/40
CPCC01B33/10721C01G25/04
Inventor 郝本清毕明亮
Owner 山东广通新材料有限公司
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