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Novel technology for producing hexamethyl disilazane from trimethyl chlorosilane

A technology of hexamethyldisilazane and trimethylchlorosilane, which is applied in the new process field of producing hexamethyldisilazane from trimethylchlorosilane, can solve the problems such as the reduction of the yield of the target product, and achieve The effect of product reduction, simple process and improved product quality

Active Publication Date: 2017-06-23
浙江硕而博化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the washing process, HMDS is prone to hydrolysis reaction to generate hexamethyldisiloxane and trimethylsilanol, resulting in a decrease in the yield of the target product

Method used

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  • Novel technology for producing hexamethyl disilazane from trimethyl chlorosilane
  • Novel technology for producing hexamethyl disilazane from trimethyl chlorosilane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Add 200kg trimethylchlorosilane into the reaction kettle, stir, and the stirring time is 15min. After the stirring is completed, add ice brine to the jacket outside the reaction kettle for cooling and cooling until the temperature in the reaction kettle drops to 60°C. The slurry discharge pump makes the trimethylchlorosilane flow into the mother liquor buffer tank through the first filter, and then returns to the reactor. At the same time, feed ammonia gas into the reactor, the feed rate of ammonia gas is 0.5L / min, the molar mass ratio of ammonia gas to trimethylchlorosilane is 3.0:2, the reaction temperature is 40°C, and the reaction time is 0.5h , the trimethylchlorosilane in the reactor reacts with ammonia to generate a mixed slurry of liquid hexamethyldisilazane and solid ammonium chloride, and the mixed slurry flows into the mother liquor buffer tank through the first filter, so that the solid Ammonium chloride is deposited on the screen of the first filter.

[00...

Embodiment 2

[0040] Add 250kg of trimethylchlorosilane into the reaction kettle and stir for 18 minutes. After the stirring is completed, add ice salt water to the jacket outside the reaction kettle for cooling and cooling until the temperature in the reaction kettle drops to 70°C. The slurry discharge pump makes the trimethylchlorosilane flow into the mother liquor buffer tank through the first filter, and then returns to the reactor. At the same time, feed ammonia gas into the reactor, the feed rate of ammonia gas is 0.8L / min, the molar mass ratio of ammonia gas to trimethylchlorosilane is 3.1:2, the reaction temperature is 45°C, and the reaction time is 0.8h , the trimethylchlorosilane in the reactor reacts with ammonia to generate a mixed slurry of liquid hexamethyldisilazane and solid ammonium chloride, and the mixed slurry flows into the mother liquor buffer tank through the first filter, so that the solid Ammonium chloride is deposited on the screen of the first filter.

[0041] Wh...

Embodiment 3

[0045] Add 320kg trimethylchlorosilane into the reaction kettle, stir, and the stirring time is 20min. After the stirring is completed, add ice salt water to the jacket outside the reaction kettle for cooling and cooling until the temperature in the reaction kettle drops to 73°C. The slurry discharge pump makes the trimethylchlorosilane flow into the mother liquor buffer tank through the first filter, and then returns to the reactor. At the same time, feed ammonia gas into the reaction kettle, the feed rate of ammonia gas is 1L / min, the molar mass ratio of ammonia gas to trimethylchlorosilane is 3.3:2, the reaction temperature is 48°C, and the reaction time is 1h, so that The trimethylchlorosilane in the reaction kettle reacts with ammonia gas to generate a mixed slurry of liquid hexamethyldisilazane and solid ammonium chloride, and the mixed slurry flows into the mother liquor buffer tank through the first filter to make the solid chlorination Ammonium is deposited on the scr...

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Abstract

The invention discloses a novel technology for producing hexamethyl disilazane from trimethyl chlorosilane. The novel technology comprises the following steps: (1) adding the trimethyl chlorosilane into a reaction container, then introducing ammonia gas, enabling the mixed materials in the reaction container to flow circularly and depositing generated solid ammonium chloride on a filter screen; (2) flushing the solid ammonium chloride through hot water in an ammonium chloride heating kettle, then enabling the water to flow back to the ammonium chloride heating kettle, and pumping hot water solution in the ammonium chloride heating kettle into a centrifugal machine to perform solid-liquid separation; (3) recycling mother solution when the content of the trimethyl chlorosilane in a mother solution buffer tank is smaller than or equal to 0.5%, and then performing rectification for purification, thus obtaining a product. The novel technology for producing the hexamethyl disilazane from the trimethyl chlorosilane disclosed by the technical scheme of the invention has the advantages of high practicability, low labor intensity, good product quality, high yield, and simpler equipment and operation process; furthermore, a reaction byproduct in reaction is reduced; meanwhile, energy consumption is reduced.

Description

technical field [0001] The invention relates to a new process for producing hexamethyldisilazane from trimethylchlorosilane. Background technique [0002] Hexamethyldisilazane (HMDS) is an important organosilicon compound, which is widely used in organosilicon chemistry and organic synthesis. Hexamethyldisilazane is not only the key raw material for the synthesis of hexamethyldisilazane (BSU), but also a commonly used silylating reagent in organic synthesis, which has important industrial application value. In organosilazane chemistry, it can be used for chlorine exchange with chlorosilane monomers to obtain polysilazanes. This method has a huge advantage in synthesis over direct ammonia. Used as an adhesion aid for photoresists in the semiconductor industry. Hexamethyldisilazane is used in the synthesis of amikacin, penicillin, and cephalosporins in the pharmaceutical industry. [0003] Industrially, HMDS is mostly prepared by reacting trimethylchlorosilane with ammonia ...

Claims

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Application Information

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IPC IPC(8): C07F7/10C07F7/20
CPCC07F7/10C07F7/20
Inventor 丁希望李宏星倪丽娟毛国胜
Owner 浙江硕而博化工有限公司
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