Operation method and device for continuous refining of titanium tetrachloride crude

An operation method, the technology of titanium tetrachloride, applied in the direction of titanium halide, etc., can solve the problems of high labor intensity, high energy consumption, unstable product quality, etc., and achieve the effect of improving product quality and increasing throughput

Inactive Publication Date: 2011-03-16
TIANJIN UNIV
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Problems solved by technology

Chinese patent "coarse titanium tetrachloride refining device (patent publication number CN101786657A)" has announced a kind of crude titanium tetrachloride refining device, also mainly is processed for vanadium impurity, but this device does not propose specific refining effect, other published The literature also mainly describes the process of how to remove vanadium impurities in crude titanium tetrachloride
[0005] The present invention a

Method used

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  • Operation method and device for continuous refining of titanium tetrachloride crude
  • Operation method and device for continuous refining of titanium tetrachloride crude

Examples

Experimental program
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Effect test

Embodiment 1

[0016] The raw material composition of titanium tetrachloride crude product is as follows: TiCl 4 ≥99.9; VOCl 3 ≤0.06; FeCl 3 ≤0.003; SiCl 4 ≤0.02, other heavy components ≤0.007%, liquid-solid ratio<0.5%.

[0017] Crude titanium tetrachloride 1 continuously enters the evaporating kettle 2 with stirring, and is fed into the heat conduction oil 12 of the system, so that the temperature in the evaporating kettle is controlled at 145°C, the stirring motor rotates at 10 rpm, and the crude titanium tetrachloride 1 Evaporation is carried out in the agitated evaporation tank 2, and the generated steam 3 enters the rectification column system 4. The steam 5 at the top of the rectification column is condensed into a liquid phase by the cooling medium water 9 entering the system in the condenser 6, and the temperature of the condensed liquid phase is 40°C. A part of the liquid phase is extracted as a refined titanium tetrachloride product 8 and leaves the system , the other part retu...

Embodiment 2

[0019] All the other conditions were the same as in Example 1, and the temperature in the stirring evaporator 2 was controlled at 150°C.

Embodiment 3

[0021] The rest of the conditions are the same as in Example 1, and the temperature in the stirring evaporator 2 is controlled at 160°C.

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Abstract

The invention relates to an operation method for continuous refining of a titanium tetrachloride crude and an operation device for continuous refining of the titanium tetrachloride crude. A multi-stage distillation process of an evaporator with stirring is adopted in the method. Materials are fed to the evaporator with stirring and heated for evaporation. The rotation speed of a stirring motor is 1-200 rpm. The temperature in the evaporator is controlled between 145 DEG C and 160 DEG C by heating. The titanium tetrachloride crude is evaporated in the evaporator. The produced vapor phase is condensed to be a liquid phase by a cooling medium. The condensed liquid phase has a temperature of between 40 DEG C and 145 DEG C. A part of the liquid phase is extracted as a refined titanium tetrachloride product and departed from a system. A part of the liquid phase flows back to the system, and is contacted with the vapor phase generated by the evaporator on a mass and heat transfer element in a multi-stage manner. The titanium tetrachloride is refined through a mass and heat transfer process. The content of the titanium tetrachloride is greater than 99.9%; the content of AlCl3 is not greater than 0.003%; the content of SiCl4 is not greater than 0.01%; the content of VoCl3 is not greater than 0.0025%; the content of FeCl3 is not greater than 0.002%; and the colorimetric degree of K2Cr3O7 is smaller than 5 mg/l. The method is a continuous process, solves problems of low production capability of a single batch or semi-batch refining device and non-acceptable product.

Description

technical field [0001] The invention relates to an operation method for continuously refining crude titanium tetrachloride, in particular to an operation method device for refining crude titanium tetrachloride by adopting a continuous multi-stage distillation refining process. Background technique [0002] Titanium tetrachloride (TiCl 4 ) is an essential intermediate product for the production of titanium sponge and titanium dioxide chloride. At present, all kinds of TiCL in the world 4 The total production capacity is about 6.5 million tons / year. Sponge titanium is a silver-white metal, which is the raw material for making titanium metal. Titanium has excellent properties and is widely used in aerospace, defense industry, petroleum industry, navigation equipment, electronic materials and other industries. With the continuous growth of my country's economy, the consumption of titanium has grown rapidly. Although my country's sponge titanium industry has made great progre...

Claims

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Application Information

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IPC IPC(8): C01G23/02
Inventor 刘艳丽华超黄国强
Owner TIANJIN UNIV
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