Preparation method of electronic-grade boron trichloride

Abstract

The invention discloses a preparation method of electronic-grade boron trichloride, wherein the preparation method comprises the steps: chlorine and hydrogen are introduced into a photocatalytic reactor from the bottom, phosgene in a reaction product of a fluidized bed reactor is decomposed into carbon monoxide and chlorine under illumination, the chlorine and hydrogen are subjected to a reactionunder ultraviolet irradiation to generate hydrogen chloride, and the hydrogen chloride is extracted from the top of the photocatalytic reactor; hydrogen chloride is subjected to heat exchange and vaporization treatment and then subjected to a reaction with boron powder in the fluidized bed reactor, and a reaction product is extracted from the top of the fluidized bed reactor, then enters a light component removal tower reboiler for heat exchange and next enters a photocatalytic reactor; a boron trichloride crude product extracted from the bottom of the photocatalytic reactor enters the light component removal tower, a product extracted from the top of the light component removal tower enters a heavy component removal tower reboiler for heat exchange, and then enters a fractional condenserfor condensation and cooling, and a liquid phase finally flows back to the light component removal tower; a material of the tower kettle of the light component removal tower enters a heavy component removal tower, and a 6N boron trichloride product is extracted after the tower top of the heavy component removal tower is condensed by a condenser. The method is simple, reliable, low in energy consumption, easy to implement and convenient for industrial production.

Description

technical field

[0001] The invention relates to the field of boron trichloride preparation, in particular to a method for preparing electronic-grade boron trichloride. Background technique

[0002] Boron trichloride is a colorless fuming liquid or gas. It decomposes into hydrogen chloride and boric acid when it meets water, and releases a lot of heat. It generates smoke due to hydrolysis in humid air. Boron trichloride has a strong reaction ability and can form various compounds. Bit compounds are often used as organic synthesis catalysts, and are widely used as etchant in the semiconductor integrated circuit manufacturing industry. With the rapid development of the semiconductor industry, the precision of integrated circuits is getting higher and higher. Therefore, boron trichloride, as an auxiliary raw material in the manufacturing process of integrated circuits, has higher and higher purity requirements.

[0003] CN201810492240.6 proposes a method and device for preparin...

Examples

Embodiment 1

[0036] Boron powder and hydrogen chloride after heat exchange react in the ebullating bed reactor R101. The temperature of the ebullating bed reactor R101 is 300°C and the pressure is 1MPa. After heat exchange, it enters the photocatalytic reactor R102. Chlorine gas is charged from the bottom of the photocatalytic reactor. The molar ratio of boron powder and chlorine gas is 1:1.5. At the same time, an appropriate amount of hydrogen gas is charged to ensure that all the chlorine gas reacts to form hydrogen chloride. The temperature of the photocatalytic reactor R102 is 30°C and the pressure is 0.4MPa. The gas phase from the top of the photocatalytic reactor R102 enters the HCl cold trap E101, and the crude boron trichloride from the bottom of the photocatalytic reactor enters the light removal tower T101. Uncondensed light impurities are extracted from the top of the HCl cold trap E101, hydrogen chloride is extracted from the lower part and enters the vaporizer F101, gas phase ...

Embodiment 2

[0041]Boron powder and hydrogen chloride after heat exchange react in the ebullating bed reactor R101. The temperature of the ebullating bed reactor R101 is 500°C and the pressure is 3MPa. After heat exchange, it enters the photocatalytic reactor R102. Chlorine gas is charged from the bottom of the photocatalytic reactor. The molar ratio of boron powder and chlorine gas is 1:2. At the same time, an appropriate amount of hydrogen gas is charged to ensure that all the chlorine gas reacts to generate hydrogen chloride. The temperature of the photocatalytic reactor R102 is 50°C and the pressure is 0.8MPa. The gas phase from the top of the photocatalytic reactor R102 enters the HCl cold trap E101, and the crude boron trichloride from the bottom of the photocatalytic reactor enters the light removal tower T101. Uncondensed light impurities are extracted from the top of the HCl cold trap E101, hydrogen chloride is extracted from the lower part and enters the vaporizer F101, gas phase...

Embodiment 3

[0046] Boron powder and hydrogen chloride after heat exchange react in the ebullating bed reactor R101. The temperature of the ebullating bed reactor R101 is 500°C and the pressure is 5MPa. After heat exchange, it enters the photocatalytic reactor R102. Chlorine gas is charged from the bottom of the photocatalytic reactor. The molar ratio of boron powder and chlorine gas is 1:3. At the same time, an appropriate amount of hydrogen gas is charged to ensure that all the chlorine gas reacts to form hydrogen chloride. The temperature of the photocatalytic reactor R102 is 60°C and the pressure is 1MPa. The gas phase from the top of the photocatalytic reactor R102 enters the HCl cold trap E101, and the crude boron trichloride from the bottom of the photocatalytic reactor enters the light removal tower T101. Uncondensed light impurities are extracted from the top of the HCl cold trap E101, hydrogen chloride is extracted from the lower part and enters the vaporizer F101, gas phase hydr...

technical field

[0001] The invention relates to the field of boron trichloride preparation, in particular to a method for preparing electronic-grade boron trichloride. Background technique

[0002] Boron trichloride is a colorless fuming liquid or gas. It decomposes into hydrogen chloride and boric acid when it meets water, and releases a lot of heat. It generates smoke due to hydrolysis in humid air. Boron trichloride has a strong reaction ability and can form various compounds. Bit compounds are often used as organic synthesis catalysts, and are widely used as etchant in the semiconductor integrated circuit manufacturing industry. With the rapid development of the semiconductor industry, the precision of integrated circuits is getting higher and higher. Therefore, boron trichloride, as an auxiliary raw material in the manufacturing process of integrated circuits, has higher and higher purity requirements.

[0003] CN201810492240.6 proposes a method and device for preparin...

Examples

Embodiment 1

[0036] Boron powder and hydrogen chloride after heat exchange react in the ebullating bed reactor R101. The temperature of the ebullating bed reactor R101 is 300°C and the pressure is 1MPa. After heat exchange, it enters the photocatalytic reactor R102. Chlorine gas is charged from the bottom of the photocatalytic reactor. The molar ratio of boron powder and chlorine gas is 1:1.5. At the same time, an appropriate amount of hydrogen gas is charged to ensure that all the chlorine gas reacts to form hydrogen chloride. The temperature of the photocatalytic reactor R102 is 30°C and the pressure is 0.4MPa. The gas phase from the top of the photocatalytic reactor R102 enters the HCl cold trap E101, and the crude boron trichloride from the bottom of the photocatalytic reactor enters the light removal tower T101. Uncondensed light impurities are extracted from the top of the HCl cold trap E101, hydrogen chloride is extracted from the lower part and enters the vaporizer F101, gas phase ...

Embodiment 2

[0041]Boron powder and hydrogen chloride after heat exchange react in the ebullating bed reactor R101. The temperature of the ebullating bed reactor R101 is 500°C and the pressure is 3MPa. After heat exchange, it enters the photocatalytic reactor R102. Chlorine gas is charged from the bottom of the photocatalytic reactor. The molar ratio of boron powder and chlorine gas is 1:2. At the same time, an appropriate amount of hydrogen gas is charged to ensure that all the chlorine gas reacts to generate hydrogen chloride. The temperature of the photocatalytic reactor R102 is 50°C and the pressure is 0.8MPa. The gas phase from the top of the photocatalytic reactor R102 enters the HCl cold trap E101, and the crude boron trichloride from the bottom of the photocatalytic reactor enters the light removal tower T101. Uncondensed light impurities are extracted from the top of the HCl cold trap E101, hydrogen chloride is extracted from the lower part and enters the vaporizer F101, gas phase...

Embodiment 3

[0046] Boron powder and hydrogen chloride after heat exchange react in the ebullating bed reactor R101. The temperature of the ebullating bed reactor R101 is 500°C and the pressure is 5MPa. After heat exchange, it enters the photocatalytic reactor R102. Chlorine gas is charged from the bottom of the photocatalytic reactor. The molar ratio of boron powder and chlorine gas is 1:3. At the same time, an appropriate amount of hydrogen gas is charged to ensure that all the chlorine gas reacts to form hydrogen chloride. The temperature of the photocatalytic reactor R102 is 60°C and the pressure is 1MPa. The gas phase from the top of the photocatalytic reactor R102 enters the HCl cold trap E101, and the crude boron trichloride from the bottom of the photocatalytic reactor enters the light removal tower T101. Uncondensed light impurities are extracted from the top of the HCl cold trap E101, hydrogen chloride is extracted from the lower part and enters the vaporizer F101, gas phase hydr...

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