Method for preparing titanium tetrafluoride

A technology of titanium tetrafluoride and fluorine gas, applied in the direction of titanium halide, etc., can solve the problems of difficult separation and purification, serious equipment corrosion, environmental pollution, etc., and achieve the effects of stable product quality, low environmental pollution, and simple equipment

Active Publication Date: 2014-04-16
RES INST OF PHYSICAL & CHEM ENG OF NUCLEAR IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The disadvantage of the above method is that the crude titanium tetrafluoride contains a large amount of hydrogen chloride and unreacted hydrogen fluoride, which are corrosive and toxic substances, which seriously corrode the equipment, are difficult to separate and purify, and cause serious environmental pollution after leakage.

Method used

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  • Method for preparing titanium tetrafluoride
  • Method for preparing titanium tetrafluoride

Examples

Experimental program
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Effect test

Embodiment 1

[0043] First, clean and dry the reactor 3, add 2 kg of titanium metal with a purity of 98.5% into the reactor 3, close the reactor 3, and evacuate it to -0.10MPa (gauge pressure), and after the leak test of the reactor 3 is qualified, remove it Preheat to 100°C.

[0044] Secondly, slowly open the fluorine gas inlet valve 2 in front of the reactor 3, and feed fluorine gas with a purity of 96% into the reactor 3, so that the fluorine gas and metal titanium are contacted in the reactor 3 to undergo a synthesis reaction to generate gaseous tetrafluoride. For the crude titanium product, the reaction process pressure is -0.05MPa, and the temperature in the reactor 3 is 200°C.

[0045] Again, the gaseous titanium tetrafluoride from the reactor 3 enters the purifier 4, the temperature inside the purifier 4 is 150° C., and the gauge pressure inside the purifier 4 is -0.10 MPa.

[0046] Finally, 4.0 kg of crude gaseous titanium tetrafluoride was collected in the purifier 4. The te...

Embodiment 2

[0048] First, the reactor 3 is cleaned and dried, 2 kg of titanium metal with a purity of 98.5% is added to the reactor 3, the reactor 3 is sealed, and the gauge pressure is evacuated to -0.09MPa. Heat to 150°C.

[0049] Secondly, slowly open the fluorine gas inlet valve 3 in front of the reactor 3, and feed fluorine gas with a purity of 96% into the reactor 3, so that the fluorine gas and metal titanium are contacted in the reactor 3 to undergo a synthesis reaction to generate gaseous tetrafluoride. Titanium crude product, the reaction process pressure is 0MPa, and the temperature of reactor 3 is 310°C.

[0050] Again, the titanium tetrafluoride coming out of the reactor 3 enters the purifier 4, the temperature inside the purifier 4 is 200°C, and the internal surface pressure of the purifier 4 is -0.05MPa.

[0051] Finally, 4.7 kg of crude gaseous titanium tetrafluoride was collected in purifier 4. Cool the temperature in the purifier to normal temperature, condense the gas...

Embodiment 3

[0053] First, the reactor 3 is cleaned and dried, 2 kg of titanium metal with a purity of 98.5% is added to the reactor 3, the reactor 3 is sealed, and the gauge pressure is evacuated to -0.08MPa. Heat to 200°C.

[0054] Secondly, slowly open the fluorine gas inlet valve 2 in front of the reactor 3, and feed fluorine gas with a purity of 96% into the reactor 3, so that the fluorine gas and metal titanium are contacted in the reactor 3 to undergo a synthesis reaction to generate titanium tetrafluoride For the crude product, the gauge pressure during the reaction was 0.05MPa, and the temperature in the reactor 3 was 500°C.

[0055] Again, the gaseous titanium tetrafluoride from the reactor 3 enters the purifier 4, the temperature inside the purifier 4 is 280° C., and the gauge pressure inside the purifier 4 is 0 MPa.

[0056] Finally, 4.5 kg of crude gaseous titanium tetrafluoride was collected in the purifier 4. Cool the temperature in the purifier to normal temperature, cond...

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Abstract

The invention discloses a method for preparing titanium tetrafluoride, which comprises the following steps of: (i) pretreating a reactor, adding metal titanium into the reactor, vacuumizing until the surface pressure is -0.10MPa to -0.08MPa and preheating the metal titanium to 100-200 DEG C; (ii) carrying out synthetic reaction on fluoride and the metal titanium to generate a gas state titanium tetrafluoride crude product, and controlling the surface pressure in the reactor to be -0.05 to 0.05MPa and the temperature to be 200-500 DEG C; (iii) collecting the titanium tetrafluoride, putting the gas state titanium tetrafluoride crude product into a purifier, and controlling the temperature in the purifier to be 150-280 DEG C and the surface pressure in the purifier to be -0.10 to 0 MPa; (iv) purifying the titanium tetrafluoride, vacuumizing non-condensable gas impurities by a tail gas treater, putting the purified gas state titanium tetrafluoride into a product storage tank, and cooling to the room temperature to obtain the titanium tetrafluoride solid powder product. The method is simple in technology, simple and convenient in operation, easy in control of reaction temperature, safe in running, low in environmental pollution and stable in product quality, and the purity of the product reaches up to more than 98%.

Description

technical field [0001] The invention belongs to a method for preparing titanium tetrafluoride, in particular to a method for preparing titanium tetrafluoride by using fluorine gas and metallic titanium as raw materials. Background technique [0002] Titanium tetrafluoride is used as an etchant in the microelectronics industry and as a catalyst in the petrochemical industry. Titanium tetrafluoride is a hygroscopic white powder with a molecular weight of 123.861, a sublimation point of 284°C and a relative density of 2.798. [0003] The commonly used method for preparing titanium tetrafluoride is as follows: [0004] Titanium tetrachloride (TiCl 4 ) reacts with hydrogen fluoride (HF) to produce titanium tetrafluoride (TiF 4 ), the reaction formula is: [0005] [0006] The process of the method: use titanium tetrachloride and hydrogen fluoride as raw materials to prepare titanium tetrafluoride, put 50% titanium tetrachloride into a reactor made of platinum or copper acc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/02
Inventor 王筠陈光华崔学文李于教
Owner RES INST OF PHYSICAL & CHEM ENG OF NUCLEAR IND
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