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Low-price titanium dichloride slurry and preparation method thereof

A technology of low-valent titanium chloride and titanium tetrachloride, which is applied in the direction of titanium trichloride, aluminum chloride, titanium halide, etc., can solve the problems of unstable quality of low-valent titanium slurry, difficult control of heating reaction, and high quality requirements. Advanced problems, to achieve excellent physical and chemical properties, easy to operate, and good product reproducibility

Inactive Publication Date: 2015-01-28
PANZHIHUA STEEL ENTERPRISES XINYU CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the industry generally adopts the addition of AlCl 3 Catalyst, after heating up to 120°C, react to prepare 3TiCl 3 .AlCl 3 The method of complex material slurry, this method is to AlCl 3 The quality requirements are high, the reaction needs to be heated in the early stage and the reaction is difficult to control, the quality of the low-priced titanium slurry is unstable, the effect of vanadium removal is poor, and explosions have occurred during the production process, etc.

Method used

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preparation example Construction

[0018] A preparation method for low-valent titanium chloride slurry, comprising the following steps:

[0019] a. First, add titanium tetrachloride and aluminum powder into the mixing tank and stir to obtain a suspension; since the volume of the mixing tank is small in industrial operation, the concentration of aluminum powder in the suspension is first controlled to 35-50 %;

[0020] b. Add the suspension to the low-valent titanium chloride preparation reactor, and then add titanium tetrachloride to adjust the concentration of aluminum powder in the suspension to 12-17%;

[0021] c. Introduce chlorine gas, control the pressure at 90-150kPa, and the flow rate of chlorine gas is 8-10m 3 / h;

[0022] d. When the temperature in the reactor reaches 120°C, stop feeding chlorine gas; continue to stir for 20 to 30 minutes to obtain qualified low-valent titanium chloride slurry; both steps a and b are carried out under the protection of inert gas, and the inertness is controlled. Th...

Embodiment 1

[0031] First pump the prepared aluminum powder suspension with a concentration of 40% into the low-priced titanium preparation reactor with a diameter of 1000mm and a height of 1000mm. The liquid level in the reactor reaches 230mm, and the liquid in the reactor is replenished with refined titanium tetrachloride. The position reaches 800mm, the concentration of aluminum powder in the detection reactor is 13%, and the nitrogen pressure and flow are controlled at 100-200kPa, 3.5-4.0m 3 / h, feed nitrogen into the reactor and start stirring on the reactor, after stirring for 5 minutes, feed the pressure 120±10kPa into the reactor, flow rate 8m 3 Chlorine gas per hour, when the temperature in the reactor reaches 120°C, close the chlorine gas inlet valve, stop feeding chlorine gas to the reactor, continue to stir after 30min, sample analysis and obtain the concentration of titanium trichloride in the low-valent titanium chloride is 9.1%, the concentration of aluminum trichloride is 3...

Embodiment 2

[0033] First pump the prepared aluminum powder suspension with a concentration of 40% into the low-priced titanium preparation reactor with a diameter of 1000mm and a height of 1000mm, so that the liquid level in the reactor reaches 290mm, and replenish the reactor with refined titanium tetrachloride. The liquid level reaches 800mm, the aluminum powder concentration in the detection reactor is 15%, and the nitrogen pressure and flow are controlled at 100-200kPa, 3.5-4.0m 3 / h, feed nitrogen into the reactor and start stirring on the reactor. After stirring for 5 minutes, open the chlorine gas valve to feed chlorine gas with a pressure of 120±10kPa and a flow rate of 9m3 / h into the reactor until the temperature in the reactor reaches 120°C When the chlorine gas inlet valve is closed, the chlorine gas supply to the reactor is stopped. After continuing to stir for 25 minutes, the concentration of titanium trichloride in the subvalent titanium chloride was 11.3% through sampling a...

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Abstract

The invention provides a preparation method of low-price titanium dichloride slurry and belongs to the field of titanium tetrachloride refining, solving the technical problem that the preparation method of the low-price titanium dichloride slurry is provided. The preparation method comprises the following steps: a, adding aluminum powder to titanium tetrachloride and stirring to obtain a suspension, and controlling the mass concentration of the aluminum powder in the suspension to 12-17%; b, introducing chlorine to a reactor and stopping introduction of nitrogen when the temperature in the reactor reaches 120 DEG C, and further stirring to obtain the qualified low-price titanium dichloride slurry, wherein the step a and the step b both are performed under inert gas protection. The low-price titanium dichloride slurry prepared by use of the method is high in activity, good in vanadium removal, and safe and reliable in process. Compared with a traditional low-price titanium dichloride preparation method, the preparation method of the low-price titanium dichloride slurry is simple in equipment, easy to operate, stable in product quality and low in energy consumption.

Description

technical field [0001] The invention belongs to the field of refining titanium tetrachloride, and in particular relates to a low-valent titanium chloride slurry and a preparation method thereof. The low-valent titanium chloride slurry can be used for vanadium removal of crude titanium tetrachloride. Background technique [0002] Coarse TiCl produced by chlorination of titanium-rich materials (including high-titanium slag, artificial rutile, and natural rutile) 4 Contains chloride impurity components of elements such as iron, aluminum, silicon, vanadium, etc., these impurities will seriously affect the quality of Haijin titanium products prepared by reduction and distillation in the next step. Therefore, the crude TiCl must be 4 Carry out refining and purification to provide qualified raw materials for the production of Haijin Titanium. Crude TiCl 4 The principle of refining is: remove high-boiling impurities by distillation, and remove low-boiling impurities by rectificat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/02
CPCC01F7/56C01G23/026
Inventor 石玉英陈映志周云英赵迪锋罗明松焦国宣
Owner PANZHIHUA STEEL ENTERPRISES XINYU CHEM