Method for synthesizing hexamethyldisilazane

A technology of hexamethyldisilazane and hexamethyldisiloxane, which is applied in the field of hexamethyldisilazane synthesis, can solve the problems of reduced yield of the target product, low product purity and yield, and achieve The effect of short reaction time, low rectification energy consumption and high yield

Active Publication Date: 2012-11-07
鲁南新时代生物技术有限公司
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  • Abstract
  • Description
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  • Application Information

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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
Chinese patent CN101613363A and CN101704835A all produce hexamethyldisilazane by this method, and the reported product purity and yield are all lower

Method used

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  • Method for synthesizing hexamethyldisilazane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Add 630ml of trimethylchlorosilane, 250ml of hexamethyldisiloxane, 500ml of benzene, and 500ml of xylene into a reaction kettle equipped with a stirrer, thermometer, and pressure gauge, and stir evenly. Ammonia gas is introduced to carry out the ammoniation reaction, and the change of the state of the material in the flask is carefully observed during the process of passing ammonia gas. Strictly control the feeding rate of ammonia gas, and the reaction rate should not be too fast, so as to prevent the salt particles from wrapping trimethylchlorosilane. Control the reaction temperature to ≤80°C and the reaction pressure to ≤0.2Mpa. After the ammoniation reaction is finished, the material is cooled to 35° C., and 800 ml of water is added for the first water washing. After washing, let it stand for 5 minutes, and separate the phases to remove the lower layer of NH 4 Cl aqueous solution. Add 400 ml of 30% potassium hydroxide solution to wash the organic phase, let stand ...

Embodiment 2

[0016] Add 630ml of trimethylchlorosilane, 250ml of hexamethyldisiloxane, and 1000ml of xylene into a reaction kettle equipped with a stirrer, thermometer, and pressure gauge, and stir evenly. Ammonia gas is introduced to carry out the ammoniation reaction, and the change of the state of the material in the flask is carefully observed during the process of passing ammonia gas. Strictly control the feeding rate of ammonia gas, and the reaction rate should not be too fast, so as to prevent the salt particles from wrapping trimethylchlorosilane. Control the reaction temperature to ≤80°C and the reaction pressure to ≤0.2Mpa. After the ammoniation reaction is finished, the material is cooled to 35° C., and 800 ml of water is added for the first water washing. After washing, let it stand for 5 minutes, and separate the phases to remove the lower layer of NH 4 Cl aqueous solution. Add 400 ml of 10% sodium hydroxide solution to wash the organic phase, let stand for 5 minutes after ...

Embodiment 3、4、5

[0018] Similar to Example 2, adopting different mixed solvents to react, the experimental results are as follows:

[0019]

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Abstract

The invention relates to a method for synthesizing hexamethyldisilazane. The hexamethyldisilazane is synthesized by a mixed solvent method through one-step ammoniation reaction, the hydrolysis side reaction of the hexamethyldisilazane can be inhibited by adding hexamethyldisiloxane into a reaction system, and reaction yield is improved. By the method, the yield is high, reaction time is short, energy consumption during rectification is low, the production cost of the hexamethyldisilazane is reduced, and the large advantage of industrialization is achieved.

Description

technical field [0001] The invention relates to a method for synthesizing hexamethyldisilazane. 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 in an inert organic solvent. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/10
Inventor 赵志全孙颖夏燕
Owner 鲁南新时代生物技术有限公司
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