Method for preparing ultrapure zirconium oxychloride and byproduct silicon tetrachloride through zircon sand boiling chlorination

A technology of ultra-pure zirconium oxychloride and by-product silicon tetrachloride, which is applied in the preparation of carbon-based compounds, chlorine/hydrogen chloride purification, chemical instruments and methods, etc., can solve problems such as waste of resources, increased consumption of raw materials, explosions, etc. Achieve the effect of improving the production capacity of the device, reducing production costs and saving fossil resources

Active Publication Date: 2016-04-20
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
[0016] 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.
[0017] 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.
[0018] 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

[0074] A method for preparing ultrapure zirconium oxychloride by-product silicon tetrachloride by boiling chlorination of zircon sand of the present invention comprises the following steps:

[0075] ①. Chlorination of zircon sand

[0076] First, crush the quartz sand to 300-350 mesh fine powder, 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 chlorine flow rate is controlled to be 1.0-1.5m 3 / h;

[0077] ②. Separation and collection of zirconium tetrachloride

[0078] 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 2

[0093] A method for preparing ultrapure zirconium oxychloride by-product silicon tetrachloride by boiling chlorination of zircon sand of the present invention comprises the following steps:

[0094] ①. Chlorination of zircon sand

[0095] First, crush the quartz sand to 300-350 mesh fine powder, 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 chlorine flow rate is controlled to be 1.0-1.5m 3 / h;

[0096] ②. Separation and collection of zirconium tetrachloride

[0097] 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

[0112] A method for preparing ultrapure zirconium oxychloride by-product silicon tetrachloride by boiling chlorination of zircon sand of the present invention comprises the following steps:

[0113] ①. Chlorination of zircon sand

[0114] First, crush the quartz sand to 300-350 mesh fine powder, 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 1.0-1.5m 3 / h;

[0115] ②. Separation and collection of zirconium tetrachloride

[0116] 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...

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Abstract

The invention provides a method for preparing ultrapure zirconium oxychloride and a byproduct silicon tetrachloride through zircon sand boiling chlorination, belonging to preparation methods of halides of zirconium. A device comprises a zircon sand boiling chlorination system, a zirconium tetrachloride condensing and collecting system, a silicon tetrachloride rectifying system and a system for preparing high-purity zirconium oxychloride through silicon tetrachloride hydrolysis. The device is characterized by also comprising a tail gas recovery system, wherein the tail gas recovery system comprises a tail gas storage device, a chlorine separation and recovery device and a CO recovery and storage device. The method is characterized by firstly separating and collecting chlorine in the tail gas, using chlorine as the raw material of zircon sand boiling chlorination reaction and recycling chlorine; and utilizing the tail gas after chlorine is separated as the raw material of an industrial production device involved synthetic reaction in which CO participates. The method for preparing ultrapure zirconium oxychloride and the byproduct silicon tetrachloride through zircon sand boiling chlorination can achieve the effects of effectively utilizing Cl2 and CO resources, reducing emission of the greenhouse gas CO2, reducing the product production cost of a zircon sand boiling chlorination device and improving the production capacity of the device.

Description

technical field [0001] The invention relates to a method for preparing ultra-pure zirconium oxychloride 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 oxychloride (ZrOCl 2 ·8H 2 O) is an important zirconium chemical, and is the basic raw material for the preparation of metal zirconium, zirconium dioxide, many zirconium salts and other zirconium compounds. It can be used as paint drying agent, rubber additive, refractory material, ceramic pigment, lubricant; it is wi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/00C01B31/18C01B33/107C01B7/07C01B3/12C07C29/151C07C31/04C07C45/50C07C47/02C07C51/12C07C53/08C08G67/02C01B32/40
CPCC01B3/12C01B7/0743C01B33/10721C01B2203/068C01G25/00C07C29/151C07C45/505C07C51/12C08G67/02C07C31/04C07C47/02C07C53/08Y02P30/00
Inventor 郝本清毕明亮
Owner 山东广通新材料有限公司
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