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CN-122011004-A - Preparation method of trimethylsilane

CN122011004ACN 122011004 ACN122011004 ACN 122011004ACN-122011004-A

Abstract

The invention relates to a preparation method of trimethylsilane, and relates to the technical field of chemical industry. The preparation method specifically comprises the following steps of S1, carrying out dehydration pretreatment on a reaction solvent tetrahydrofuran, S2, respectively preparing a reducing agent solution, a catalyst suspension and a trimethylchlorosilane solution by using the tetrahydrofuran after the dehydration pretreatment, S3, synthesizing the trimethylsilane, namely, dropwise adding the reducing agent solution and the catalyst suspension into the trimethylchlorosilane solution to construct a liquid-solid reaction system, regulating the pressure of the reaction system to a micro-positive pressure state, stirring the whole process, carrying out hydrogenation reduction reaction for 1-3h at the temperature of 20-40 ℃, S4, collecting the gas generated in the reaction process, and purifying to obtain the trimethylsilane. The method can effectively reduce the use proportion of the common catalyst, and has the advantages of long reaction time, high yield and cost reduction.

Inventors

  • YAO BINGJIE
  • SHEN YONGMING
  • HE SHUO
  • WANG WEI
  • ZHAO XING
  • ZHU JIANGTAO
  • Hua Yingxi
  • ZHANG XUAN

Assignees

  • 中船(邯郸)派瑞特种气体股份有限公司

Dates

Publication Date
20260512
Application Date
20260123

Claims (10)

  1. 1. The preparation method of the trimethylsilane is characterized by comprising the following steps of: S1, carrying out dehydration pretreatment on a reaction solvent tetrahydrofuran; S2, respectively preparing a reducing agent solution, a catalyst suspension and a trimethylchlorosilane solution by using tetrahydrofuran after dehydration pretreatment; s3, synthesizing trimethylsilane, namely dropwise adding a reducing agent solution and a catalyst suspension into a trimethylchlorosilane solution to construct a liquid-solid reaction system, regulating the pressure of the reaction system to be in a micro-positive pressure state, stirring the whole process at 20-40 ℃, and carrying out hydrogenation reduction reaction for 1-3h; S4, collecting products, namely collecting generated gas in the reaction process.
  2. 2. The preparation method of the trimethylsilane according to claim 1, wherein the specific steps of the step S1 are that a water removing agent is added into tetrahydrofuran, stirred for 6-8 hours, filtered, and the pretreated tetrahydrofuran is obtained, and the water content is less than or equal to 100ppm; The water scavenger is one or more of anhydrous calcium chloride, molecular sieve and anhydrous magnesium chloride which are mixed in any proportion; The mass percentage of the water scavenger is 1-5%.
  3. 3. The preparation method of the trimethylsilane according to claim 1, wherein the preparation process of the reducing agent solution in the step S2 is characterized in that under the protection of nitrogen, the reducing agent is weighed and added into a reaction bottle, tetrahydrofuran after dehydration pretreatment is added, and the mixture is stirred until the tetrahydrofuran is completely dissolved, wherein the mass percentage of the reducing agent in the reducing agent solution is 5-15%; The reducing agent is one or more of lithium aluminum hydride, sodium borohydride and lithium hydride.
  4. 4. The preparation method of the trimethylsilane according to claim 1, wherein the preparation process of the catalyst suspension in the step S2 is that the transition metal catalyst is weighed, tetrahydrofuran after dehydration pretreatment is added, and the mixture is stirred to form a suspension; the transition metal catalyst is one or a combination of more of Pt, ni and Cu catalysts; The mass percentage of the transition metal catalyst in the catalyst suspension is 5-15%.
  5. 5. The preparation method of trimethylsilane according to claim 1, wherein the preparation process of the trimethylchlorosilane solution in the step S2 is characterized in that trimethylchlorosilane is weighed and completely dissolved in tetrahydrofuran after water removal pretreatment, and the volume ratio of the tetrahydrofuran after water removal pretreatment to the trimethylchlorosilane is 1:1-1.3:1.
  6. 6. The method for preparing trimethylsilane according to claim 4, wherein the transition metal catalyst in the step S3 is used in an amount of 0.5% -3% by mole of trimethylchlorosilane, and the molar ratio of trimethylchlorosilane to reducing agent is 1 (0.3-0.8).
  7. 7. The method for preparing trimethylsilane according to claim 1, wherein the drop acceleration of the reducing agent solution in the step S3 is 3d/S to 1d/5S, and the drop acceleration of the catalyst suspension is 1d/S to 10d/S.
  8. 8. The process for preparing trimethylsilane according to claim 7, wherein the drop velocity of the reducing agent solution in the step S3 is 3d/S and the drop velocity of the catalyst suspension is 1d/S.
  9. 9. The process for preparing trimethylsilane according to claim 1, wherein the stirring speed in the step S3 is 100-200r/min.
  10. 10. The preparation method of trimethylsilane according to claim 1, wherein the pressure of the micro positive pressure state in the step S3 is 0.01-0.05MPa, and the trimethylsilane is obtained after the gas generated in the step S4 is collected and purified.

Description

Preparation method of trimethylsilane Technical Field The invention relates to the technical field of trimethylsilane synthesis, in particular to a preparation method of trimethylsilane. Background Trimethylsilane (3 MS) is an organosilicon compound with a chemical formula (CH 3)3 SiH) and is colorless and volatile, and has certain toxicity and danger, but has wide application in the fields of semiconductor manufacturing, chemical synthesis, surface treatment, paint ink, medicine and the like. At present, a hydrogenation reduction method is a mainstream technology for preparing trimethylsilane, and the method generates a target product and a hydrogen chloride byproduct by reacting hydrogen atoms in a reducing agent with chlorine atoms in trimethylchlorosilane, and has the advantages of high product purity and good environmental protection. However, the existing hydrogenation reduction method has the defects that firstly, the cost is high due to the large consumption of the reducing agent, for example, the invention patent CN100516074C adopts lithium aluminum hydride as a strong reducing agent, the economic burden is caused by excessive consumption, secondly, the reaction efficiency is low, the time is long, the traditional reaction can be completed within 10-15 hours, the production efficiency is severely restricted, thirdly, the yield is low, the raw material waste is serious, fourthly, the part of the catalytic system adopts expensive catalysts such as iridium-amido complex and the like, the reaction effect can be improved, but the cost is too high, and the industrial popularization is not facilitated. Disclosure of Invention In order to solve the defects in the prior art, the invention provides a preparation method of trimethylsilane, which realizes high-efficiency and low-cost synthesis by combining micro-positive pressure condition regulation and control through the synergistic effect of transition metal catalysis and liquid-solid multiphase reaction. The technical scheme of the invention is as follows: A method for preparing trimethylsilane, comprising the following steps: S1, carrying out dehydration pretreatment on a reaction solvent tetrahydrofuran; S2, respectively preparing a reducing agent solution, a catalyst suspension and a trimethylchlorosilane solution by using tetrahydrofuran after dehydration pretreatment; s3, synthesizing trimethylsilane, namely dropwise adding a reducing agent solution and a catalyst suspension into a trimethylchlorosilane solution to construct a liquid-solid reaction system, regulating the pressure of the reaction system to be in a micro-positive pressure state, stirring the whole process at 20-40 ℃, and carrying out hydrogenation reduction reaction for 1-3h; S4, collecting products, namely collecting generated gas in the reaction process. Preferably, the specific step of the step S1 is that a water removing agent is added into tetrahydrofuran, stirred for 6-8 hours, filtered to obtain pretreated tetrahydrofuran, wherein the water content is less than or equal to 100ppm; The water scavenger is one or more of anhydrous calcium chloride, molecular sieve and anhydrous magnesium chloride which are mixed in any proportion; The mass percentage of the water scavenger is 1-5%, or the solid-liquid mass ratio of the water scavenger to tetrahydrofuran is 1-5:95-99. Preferably, the preparation process of the reducing agent solution in the step S2 comprises the steps of weighing the reducing agent, adding the reducing agent into a reaction bottle under the protection of nitrogen, adding tetrahydrofuran after dehydration pretreatment, and stirring until the tetrahydrofuran is completely dissolved, wherein the mass percentage of the reducing agent in the reducing agent solution is 5-15%; The reducing agent is one or more of lithium aluminum hydride, sodium borohydride and lithium hydride. Preferably, the preparation process of the catalyst suspension in the step S2 comprises the steps of weighing a transition metal catalyst, adding tetrahydrofuran after dehydration pretreatment, and stirring to form a suspension; the transition metal catalyst is one or a combination of more of Pt, ni and Cu catalysts; The mass percentage of the transition metal catalyst in the catalyst suspension is 5-15%. Preferably, the preparation process of the trimethylchlorosilane solution in the step S2 comprises the steps of weighing trimethylchlorosilane, completely dissolving the trimethylchlorosilane in tetrahydrofuran after the dehydration pretreatment, wherein the volume ratio of the tetrahydrofuran after the dehydration pretreatment to the trimethylchlorosilane is 1:1-1.3:1. Preferably, the dosage of the transition metal catalyst in the step S3 is 0.5-3% of the molar weight of trimethylchlorosilane, and the molar ratio of trimethylchlorosilane to reducing agent is 1 (0.3-0.8). Preferably, the drop acceleration of the reducing agent solution in the step S3 is 3d/S-1d/5S, and the drop acceleration of the