Synthesis method of trimethylsilane
By using Lewis acid catalyst in trimethylsilane synthesis, the cost problem in the prior art is solved, the amount of reducing agent is used, the reaction rate and efficiency are improved, and the production of trimethylsilane is achieved at a lower cost.
Patent Information
- Application Number
- CN202411151204.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-08-21
- Publication Date
- 2025-01-03
AI Technical Summary
The existing trimethylsilane synthesis method uses lithium tetrahydrogen lithium, high cost, slow reaction rate of calcium hydride and aluminum hydride, and expensive catalysts, resulting in high industrial production costs.
The Lewis acid catalyst is used to reduce the amount of reducing agent used, and trimethylsilane is generated through hydrogenation reduction reaction, and the reaction conditions are controlled to improve the reaction rate and efficiency.
By accelerating the reaction with Lewis acid catalyst, the amount of reducing agent is used is reduced, the production cost of trimethylsilane is reduced, the reaction rate and efficiency are improved, and the synthesis is achieved at a lower cost.
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Figure CN119241581A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of trimethylsilane synthesis, and in particular to a method for synthesizing trimethylsilane. Background Art
[0002] Trimethylsilane (3MS) is an organosilicon compound with the chemical formula (CH3)3SiH. It is a colorless, volatile gas with certain toxicity and danger. Trimethylsilane gas is widely used in many fields, including semiconductor manufacturing, chemical synthesis, surface treatment, coatings and inks, medicine, etc. Thanks to the rapid development of semiconductors and related industries, the demand for trimethylsilane gas in related fields is growing. According to market research reports, the scale of this market is expected to continue to expand in the next few years.
[0003] The main method for synthesizing trimethylsilane is the hydrogenation reduction method. Specifically, during the reduction process of trimethylchlorosilane, the hydrogen atoms in the reducing agent react with the chlorine atoms in trimethylchlorosilane to generate trimethylsilane and the corresponding hydrogen chloride byproduct. Trimethylsilane prepared by the hydrogenation reduction method has the advantages of high purity and stable yield, and can meet the demand for high-quality organosilicon compounds in the fields of semiconductor manufacturing and polymer material synthesis. In addition, because the hydrogenation reduction reaction usually does not produce toxic and harmful byproducts or waste, this method also has certain environmental advantages.
[0004] However, there are some inevitable disadvantages in the preparation of trimethylsilane by hydrogenation reduction method. For example, in the prior art, lithium aluminum hydride is used as a strong reducing agent to reduce trimethylchlorosilane to prepare trimethylsilane, but the amount of lithium aluminum hydride is large and the cost is high. There is also the prior art that calcium hydride and lithium aluminum hydride, which are relatively simple to post-process, are used as hydrogenation reducing agents at the same time, but the reaction rate is slow. Another method for synthesizing trimethylsilane uses iridium-amide complex as a catalyst, which is expensive and costly, and is not conducive to industrial production.
[0005] Therefore, providing a method for synthesizing trimethylsilane with lower cost is a technical problem to be solved urgently. Summary of the invention
[0006] In order to solve the technical problem of high cost in the prior art when using the hydrogenation reduction method to prepare trimethylsilane, the present invention provides a method for synthesizing trimethylsilane, by using a Lewis acid catalyst, reducing the amount of reducing agent used, thereby reducing the reaction cost.
[0007] To achieve the above purpose, the technical solution adopted by the present invention is as follows:
[0008] A method for synthesizing trimethylsilane comprises the following steps:
[0009] S1, pretreatment of the reaction solvent for dehydration: adding a dehydrating agent to the reaction solvent, stirring, filtering, and obtaining a pretreated reaction solvent;
[0010] S2, solution preparation: using the pretreated reaction solvent to prepare a reducing agent solution, a catalyst solution and a trimethylsilyl chloride solution respectively;
[0011] S3, synthesis of trimethylsilane: adding a reducing agent solution and a catalyst solution dropwise to a trimethylchlorosilane solution to carry out a hydrogenation reduction reaction, collecting the gas, and obtaining trimethylsilane.
[0012] Preferably, in S3, in the hydrogenation reduction reaction system, the molar ratio of trimethylchlorosilane to the catalyst is 1:(0.05-0.15); the volume ratio of the reaction solvent to trimethylchlorosilane is (3-10):1; and the molar ratio of the reducing agent to trimethylchlorosilane is 1:(6-8).
[0013] Preferably, in S1, the reaction solvent is one or more of tetrahydrofuran, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether, butyl ether, dibutyl ether, diethylene glycol dibutyl ether, and toluene mixed in any proportion.
[0014] Preferably, in S1, the dehydrating agent is one or more of anhydrous calcium chloride, molecular sieves and anhydrous magnesium chloride mixed in any proportion; the stirring time is 6-8h; and the volume ratio of the dehydrating agent to the reaction solvent is 3:(6-8).
[0015] Preferably, in S2, the preparing of the reducing agent solution is carried out under nitrogen protection, and the preparing of the reducing agent solution comprises the following steps: weighing the reducing agent, adding it to a reaction bottle, adding a reaction solvent to the reaction bottle, and stirring until the reducing agent is completely dissolved.
[0016] Preferably, the reducing agent is one of LiAlH4, NaBH4, LiH, NaH, and red aluminum solution.
[0017] Preferably, in S2, preparing the catalyst solution comprises the following steps: weighing a catalyst and completely dissolving it in a reaction solvent; the catalyst is a Lewis acid catalyst.
[0018] Preferably, the Lewis acid catalyst is one or more of metal halide, trifluoromethanesulfonic acid or trifluoromethanesulfonate mixed in any proportion; more preferably, the metal halide includes aluminum chloride, zinc chloride, cobalt chloride or nickel chloride; and the trifluoromethanesulfonate includes sodium trifluoromethanesulfonate.
[0019] Preferably, in S3, the dropping speed of the reducing agent solution is controlled at 3d / s-1d / 5s, more preferably, the dropping speed of the reducing agent solution is controlled at 3d / s; the dropping speed of the catalyst solution is controlled at 1d / s-10d / s, more preferably, the dropping speed of the catalyst solution is controlled at 1d / s; and during the dropping of the reducing agent solution, nitrogen is used to gently sweep the reaction system.
[0020] Preferably, during the entire process of S3, the stirring speed is controlled to be 100 r / min-200 r / min, and the temperature is 20°C-100°C, more preferably, the temperature is 20°C-40°C; the reduction hydrogenation reaction time is 1h-7h.
[0021] Based on the above technical solutions, the present invention has the following beneficial effects:
[0022] In the present invention, when synthesizing trimethylsilane, a Lewis acid catalyst is added to accelerate the hydrogenation reduction reaction between trimethylsilyl chloride and a reducing agent, so that the reaction is carried out under milder conditions. In addition, the Lewis acid catalyst reduces the activation energy of the reaction, so that the trimethylsilyl chloride molecules are more likely to reach the energy state required for the reaction, thereby improving the reaction rate and efficiency, thereby achieving the same reaction product with less reducing agent.
[0023] Since the cost of the Lewis acid catalyst is lower than that of the reducing agent, the present invention reduces the amount of the reducing agent used by using the reducing agent and the Lewis acid catalyst at the same time, thereby reducing the production cost of trimethylsilane. BRIEF DESCRIPTION OF THE DRAWINGS
[0024] In order to more clearly illustrate the specific implementation of the present invention or the technical solution in the prior art, the drawings required for use in the specific implementation or the description of the prior art are briefly introduced below.
[0025] Figure 1 The present invention is a process flow chart of the synthesis method of trimethylsilane. DETAILED DESCRIPTION
[0026] In order to further explain the technical means and effects adopted by the present invention to achieve the predetermined application purpose, a clear and complete description is given below in conjunction with the accompanying drawings and preferred embodiments.
[0027] Example 1
[0028] This embodiment provides a method for synthesizing trimethylsilane, in which the dehydrating agent is a molecular sieve, the reaction solvent is tetrahydrofuran, the reducing agent is lithium aluminum tetrahydride (LiAlH4), and the catalyst is trifluoromethanesulfonic acid. The process flow of the synthesis method is as follows: Figure 1 As shown, the specific steps include:
[0029] S1: pretreatment of reaction solvent for dehydration: take tetrahydrofuran, a reaction solvent, add molecular sieves according to a volume ratio of dehydrating agent to reaction solvent of 3:7, stir for 7 hours, filter, and obtain dehydrated tetrahydrofuran. Detect the water content of the dehydrated tetrahydrofuran. If the water content is less than or equal to 100 ppm, the test is qualified and it is ready for use;
[0030] S2: Solution preparation: Prepare a reducing agent solution in a glove box, specifically including: weigh 0.58 g of lithium aluminum tetrahydride solid powder of the reducing agent, add it to a reaction bottle, then add 30 mL of dehydrated tetrahydrofuran to the reaction bottle, and stir until completely dissolved; weigh 1.5 g of catalyst trifluoromethanesulfonic acid, and completely dissolve it in 10 mL of dehydrated tetrahydrofuran to obtain a catalyst solution; weigh 11.6 g of trimethylsilyl chloride, add it to 10 mL of dehydrated tetrahydrofuran, and stir until mixed evenly to obtain a trimethylsilyl chloride solution;
[0031] S3: Synthesis of trimethylsilane: Use a dropping funnel to drop the reducing agent solution and the catalyst solution into the trimethylchlorosilane solution respectively. The dropping speed of the reducing agent is controlled to 3d / s, the dropping speed of the catalyst is controlled to 1d / s, and nitrogen is used to sweep the reaction system when dropping the reducing agent solution. After the dropping is completed, the hydrogenation reduction reaction is carried out for 4h. During the dropping and reaction process, the temperature is controlled to 40℃ and the stirring speed is controlled to 150r / min. After the reaction is completed, the trimethylsilane gas is collected and sample detection is carried out. The yield of trimethylsilane is 95.6%.
[0032] Example 2
[0033] This embodiment provides a method for synthesizing trimethylsilane, in which the dehydrating agent is anhydrous calcium chloride, the reaction solvent is tetrahydrofuran, the reducing agent is lithium aluminum tetrahydride, and the catalyst is aluminum chloride. The process flow of the synthesis method is as follows: Figure 1 As shown, the specific steps include:
[0034] S1: pretreatment of reaction solvent for dehydration: take tetrahydrofuran, a reaction solvent, add anhydrous calcium chloride according to a volume ratio of dehydrating agent to reaction solvent of 1:2, stir for 6 hours, filter, and obtain dehydrated tetrahydrofuran. Detect the water content of the dehydrated tetrahydrofuran. If the water content is less than or equal to 100 ppm, the test is qualified and it is ready for use;
[0035] S2: Solution preparation: Prepare a reducing agent solution in a glove box, specifically including: weigh 0.68 g of reducing agent lithium aluminum hydroxide solid powder, add it to a reaction bottle, then add 30 mL of dehydrated tetrahydrofuran to the reaction bottle, and stir until completely dissolved; weigh 1.4 g of catalyst aluminum chloride, and completely dissolve it in 10 mL of dehydrated tetrahydrofuran to obtain a catalyst solution; weigh 11.6 g of trimethylsilyl chloride, add it to 10 mL of dehydrated tetrahydrofuran, and stir until mixed evenly to obtain a trimethylsilyl chloride solution;
[0036] S3: Synthesis of trimethylsilane: Use a dropping funnel to drop the reducing agent solution and the catalyst solution into the trimethylchlorosilane solution respectively. The dropping speed of the two is controlled to be 1d / s and nitrogen is used to sweep the reaction system when dropping the reducing agent solution. After the dropping is completed, the hydrogenation reduction reaction is carried out for 1h. During the dropping and reaction process, the temperature is controlled to be 100℃ and the stirring speed is 100r / min. After the reaction is completed, the trimethylsilane gas is collected and sample detection is carried out. The yield of trimethylsilane is 94.1%.
[0037] Example 3
[0038] This embodiment provides a method for synthesizing trimethylsilane, wherein the dehydrating agent is anhydrous magnesium chloride, the reaction solvent is toluene, the reducing agent is red aluminum solution, and the catalyst is trifluoromethanesulfonic acid, and specifically comprises the following steps:
[0039] S1: Reaction solvent dehydration pretreatment: Take the reaction solvent toluene, add anhydrous magnesium chloride according to the volume ratio of dehydrating agent to reaction solvent of 3:8, stir for 8 hours, filter, and obtain dehydrated toluene. Detect the water content of the dehydrated toluene. If the water content is less than or equal to 100ppm, it is qualified and ready for use;
[0040] S2: Solution preparation: Prepare a reducing agent solution in a glove box, specifically comprising: weighing 3.81 g of a red aluminum solution with a concentration of 70 wt.% (the mass of red aluminum in the red aluminum solution is 2.67 g), adding it to a reaction bottle, and then adding 30 mL of dehydrated toluene to the reaction bottle, stirring until completely mixed; weighing 1.5 g of catalyst trifluoromethanesulfonic acid, completely dissolving it in 10 mL of dehydrated toluene, to obtain a catalyst solution; weighing 11.5 g of trimethylchlorosilane, adding it to 10 mL of dehydrated toluene, stirring until evenly mixed to obtain a trimethylchlorosilane solution;
[0041] S3: Synthesis of trimethylsilane: Use a dropping funnel to drop the reducing agent solution and the catalyst solution into the trimethylchlorosilane solution respectively. The dropping speed of the reducing agent is controlled to be 1d / 5s, the dropping speed of the catalyst is controlled to be 10d / s, and nitrogen is used to sweep the reaction system when dropping the reducing agent solution. After the dropping is completed, the hydrogenation reduction reaction is carried out for 7h. During the dropping and reaction process, the temperature is controlled to be 20℃ and the stirring speed is 200r / min. After the reaction is completed, the trimethylsilane gas is collected and sample detection is carried out. The yield of trimethylsilane is 93.2%.
[0042] Example 4
[0043] This embodiment provides a method for synthesizing trimethylsilane, wherein the dehydrating agent is a molecular sieve, the reaction solvent is tetrahydrofuran, the reducing agent is lithium aluminum tetrahydride, and the catalyst is nickel chloride, and specifically comprises the following steps:
[0044] S1: pretreatment of reaction solvent for removing water: same as S1 in Example 1;
[0045] S2: Solution preparation: Prepare a reducing agent solution in a glove box, specifically including: weigh 0.5 g of reducing agent lithium aluminum hydroxide solid powder, add it to a reaction bottle, then add 30 mL of dehydrated tetrahydrofuran to the reaction bottle, and stir until completely dissolved; weigh 1.4 g of catalyst nickel chloride, and completely dissolve it in 10 mL of dehydrated tetrahydrofuran to obtain a catalyst solution; weigh 11.5 g of trimethylsilyl chloride, add it to 10 mL of dehydrated tetrahydrofuran, and stir until mixed evenly to obtain a trimethylsilyl chloride solution;
[0046] S3: Synthesis of trimethylsilane: Use a dropping funnel to drop the reducing agent solution and the catalyst solution into the trimethylchlorosilane solution respectively. The dropping speed of both is controlled to be 1d / s and nitrogen is used to sweep the reaction system when dropping the reducing agent solution. After the dropping is completed, the hydrogenation reduction reaction is carried out for 4h. During the dropping and reaction process, the temperature is controlled to be 40℃ and the stirring speed is 150r / min. After the reaction is completed, the trimethylsilane gas is collected and sample detection is carried out. The yield of trimethylsilane is 93.8%.
[0047] Example 5
[0048] This embodiment provides a method for synthesizing trimethylsilane, wherein the dehydrating agent is a molecular sieve, the reaction solvent is tetrahydrofuran, the reducing agent is sodium borohydride (NaBH4), and the catalyst is sodium trifluoromethanesulfonate, and specifically comprises the following steps:
[0049] S1: pretreatment of reaction solvent for removing water: same as S1 in Example 1;
[0050] S2: Solution preparation: Prepare a reducing agent solution in a glove box, specifically including: weigh 1.08 g of reducing agent sodium borohydride solid powder, add it to a reaction bottle, then add 30 mL of dehydrated tetrahydrofuran to the reaction bottle, and stir until completely dissolved; weigh 1.7 g of catalyst sodium trifluoromethanesulfonate, and completely dissolve it in 10 mL of dehydrated tetrahydrofuran to obtain a catalyst solution; weigh 21.7 g of trimethylchlorosilane, add it to 35 mL of dehydrated tetrahydrofuran, and stir until mixed evenly to obtain a trimethylchlorosilane solution;
[0051] S3: Synthesis of trimethylsilane: Use a dropping funnel to drop the reducing agent solution and the catalyst solution into the trimethylchlorosilane solution respectively. The dropping speed of both is controlled to be 1d / s and nitrogen is used to sweep the reaction system when dropping the reducing agent solution. After the dropping is completed, the hydrogenation reduction reaction is carried out for 4h. During the dropping and reaction process, the temperature is controlled to be 40℃ and the stirring speed is 100r / min. After the reaction is completed, the trimethylsilane gas is collected and sample detection is carried out. The yield of trimethylsilane is 92.1%.
[0052] Example 6
[0053] This embodiment provides a method for synthesizing trimethylsilane, wherein the dehydrating agent is a molecular sieve, the reaction solvent is tetrahydrofuran, the reducing agent is lithium hydride (LiH), and the catalyst is zinc chloride, and specifically comprises the following steps:
[0054] S1: pretreatment of reaction solvent for removing water: same as S1 in Example 1;
[0055] S2: Solution preparation: Prepare a reducing agent solution in a glove box, specifically including: weigh 0.26 g of reducing agent lithium hydride solid powder, add it to a reaction bottle, then add 30 mL of dehydrated tetrahydrofuran to the reaction bottle, and stir until completely dissolved; weigh 4 g of catalyst zinc chloride, and completely dissolve it in 10 mL of dehydrated tetrahydrofuran to obtain a catalyst solution; weigh 21.7 g of trimethylsilyl chloride, add it to 210 mL of dehydrated tetrahydrofuran, and stir until mixed evenly to obtain a trimethylsilyl chloride solution;
[0056] S3: Synthesis of trimethylsilane: Use a dropping funnel to drop the reducing agent solution and the catalyst solution into the trimethylchlorosilane solution respectively. The dropping speed of the two is controlled to be 1d / s and nitrogen is used to sweep the reaction system when the reducing agent solution is added. After the addition is completed, the hydrogenation reduction reaction is carried out for 4h. During the addition and reaction process, the temperature is controlled to be 40℃ and the stirring speed is 150r / min. After the reaction is completed, the trimethylsilane gas is collected and sample detection is carried out. The yield of trimethylsilane is 93.3%.
[0057] Example 7
[0058] This embodiment provides a method for synthesizing trimethylsilane, wherein the dehydrating agent is a molecular sieve, the reaction solvent is tetrahydrofuran, the reducing agent is sodium hydride (NaH), and the catalyst is cobalt chloride, and specifically comprises the following steps:
[0059] S1: pretreatment of reaction solvent for removing water: same as S1 in Example 1;
[0060] S2: Solution preparation: Prepare a reducing agent solution in a glove box, specifically including: weigh 0.6 g of reducing agent sodium hydride solid powder, add it to a reaction bottle, then add 30 mL of dehydrated tetrahydrofuran to the reaction bottle, and stir until completely dissolved; weigh 2.6 g of catalyst cobalt chloride, and completely dissolve it in 10 mL of dehydrated tetrahydrofuran to obtain a catalyst solution; weigh 21.7 g of trimethylchlorosilane, add it to 135 mL of dehydrated tetrahydrofuran, and stir until mixed evenly to obtain a trimethylchlorosilane solution;
[0061] S3: Synthesis of trimethylsilane: Use a dropping funnel to drop the reducing agent solution and the catalyst solution into the trimethylchlorosilane solution respectively. The dropping speed of both is controlled to be 1d / s and nitrogen is used to sweep the reaction system when dropping the reducing agent solution. After the dropping is completed, the hydrogenation reduction reaction is carried out for 4h. During the dropping and reaction process, the temperature is controlled to be 40℃ and the stirring speed is 150r / min. After the reaction is completed, the trimethylsilane gas is collected and sample detection is carried out. The yield of trimethylsilane is 91.8%.
[0062] The reaction solvent tetrahydrofuran in Examples 1-2 and 4-7 can be replaced by a mixture of one or more of diethylene glycol dimethyl ether, triethylene glycol dimethyl ether, butyl ether, dibutyl ether, diethylene glycol dibutyl ether, and toluene.
[0063] Comparative Example 1
[0064] The difference between this comparative example and Example 1 is that the catalyst trifluoromethanesulfonic acid is not added into the reaction system, and other reaction conditions are the same. The yield of trimethylsilane finally obtained is 65%.
[0065] The experimental results of this comparative example and Example 1 show that the catalyst can increase the reaction rate and efficiency, thereby increasing the yield of trimethylsilane.
[0066] Comparative Example 2
[0067] The difference between this comparative example and Example 1 is that the amount of lithium aluminum tetrahydride added is 5.8 g, and the catalyst trifluoromethanesulfonic acid is not added to the reaction system. The final yield of trimethylsilane is 81.3%.
[0068] Compared with Example 1, the yield of trimethylsilane prepared in this comparative example without using a catalyst requires more lithium aluminum tetrahydride and is 81.3%, which further illustrates that the use of a catalyst can not only reduce the amount of lithium aluminum tetrahydride used as a reducing agent but also increase the yield of trimethylsilane. Moreover, since the price of lithium aluminum tetrahydride is higher than that of the catalyst, the production cost of trimethylsilane is reduced.
[0069] Comparative Example 3
[0070] The difference between this comparative example and Example 3 is that the amount of red aluminum solution with a concentration of 70wt.% is 5.8g (the mass of red aluminum in the red aluminum solution is 4.06g), and the catalyst trifluoromethanesulfonic acid is not added to the reaction system, and the final yield of trimethylsilane is 76.8%.
[0071] Compared with Example 3, this comparative example uses more red aluminum solution, but the yield of trimethylsilane is lower, which shows that the addition of catalyst can not only reduce the usage of red aluminum solution but also increase the yield of product trimethylsilane.
[0072] Comparative Example 4
[0073] The difference between this comparative example and Example 5 is that the amount of sodium borohydride solid powder added as the reducing agent is 3.5 g and no catalyst sodium trifluoromethanesulfonate is added to the reaction system. The yield of trimethylsilane finally obtained is 70.1%.
[0074] Compared with Example 5, this comparative example uses more sodium borohydride, but the yield of trimethylsilane is lower, which shows that the addition of catalyst can not only reduce the usage of sodium borohydride but also increase the yield of product trimethylsilane.
[0075] Comparative Example 5
[0076] The difference between this comparative example and Example 6 is that the amount of the reducing agent lithium hydride solid powder added is 1.8 g and the catalyst zinc chloride is not added to the reaction system, and the final yield of trimethylsilane is 75.7%.
[0077] Compared with Example 6, this comparative example uses more lithium hydride, but the yield of trimethylsilane is lower, which shows that the addition of catalyst can not only reduce the usage of lithium hydride but also increase the yield of product trimethylsilane.
[0078] Comparative Example 6
[0079] The difference between this comparative example and Example 7 is that the amount of sodium hydride solid powder added as the reducing agent is 3.0 g and no catalyst cobalt chloride is added to the reaction system. The yield of trimethylsilane finally obtained is 72.8%.
[0080] Compared with Example 7, this comparative example uses more sodium hydride, but the yield of trimethylsilane is lower, which shows that the addition of catalyst can not only reduce the usage of sodium hydride but also increase the yield of product trimethylsilane.
[0081] In summary of the above technical solutions, the present invention uses a reducing agent and a Lewis acid catalyst to prepare trimethylsilane, thereby reducing the amount of reducing agent used and thus reducing the production cost of trimethylsilane.
[0082] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any form. Although the present invention has been disclosed as a preferred embodiment as above, it is not used to limit the present invention. Any technical personnel in this field can make some changes or modify the technical contents disclosed above into equivalent embodiments without departing from the scope of the technical solution of the present invention. However, any brief modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention without departing from the content of the technical solution of the present invention are still within the scope of the technical solution of the present invention.
Claims
1. A method for synthesizing trimethylsilane, characterized in that: The steps include: S1, pretreatment of the reaction solvent for dehydration: adding a dehydrating agent to the reaction solvent, stirring, filtering, and obtaining a pretreated reaction solvent; S2, solution preparation: using the pretreated reaction solvent to prepare a reducing agent solution, a catalyst solution and a trimethylsilyl chloride solution respectively; S3, synthesis of trimethylsilane: adding a reducing agent solution and a catalyst solution dropwise to a trimethylchlorosilane solution to carry out a hydrogenation reduction reaction, collecting the gas, and obtaining trimethylsilane.
2. The method for preparing trimethylsilane according to claim 1, characterized in that: In S3, in the hydrogenation reduction reaction system, the molar ratio of trimethylchlorosilane to the catalyst is 1:(0.05-0.15); the volume ratio of the reaction solvent to trimethylchlorosilane is (3-10):1; and the molar ratio of the reducing agent to trimethylchlorosilane is 1:(6-8).
3. The method for preparing trimethylsilane according to claim 1, characterized in that: In S1, the reaction solvent is one or more of tetrahydrofuran, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether, butyl ether, dibutyl ether, diethylene glycol dibutyl ether, and toluene mixed in any proportion.
4. The method for preparing trimethylsilane according to claim 1, characterized in that: In S1, the dehydrating agent is one or more of anhydrous calcium chloride, molecular sieve and anhydrous magnesium chloride mixed in any proportion; the stirring time is 6-8h; and the volume ratio of the dehydrating agent to the reaction solvent is 3:(6-8).
5. The method for preparing trimethylsilane according to claim 1, characterized in that: In S2, the reducing agent solution is prepared under nitrogen protection, and the reducing agent solution is prepared including the following steps: weighing the reducing agent, adding it to a reaction bottle, adding a reaction solvent to the reaction bottle, and stirring until the reducing agent is completely dissolved.
6. The method for preparing trimethylsilane according to claim 5, characterized in that: The reducing agent is one of LiAlH4, NaBH4, LiH, NaH, and red aluminum solution.
7. The method for preparing trimethylsilane according to claim 1, characterized in that: In S2, preparing the catalyst solution comprises the following steps: weighing the catalyst and completely dissolving it in a reaction solvent; the catalyst is a Lewis acid catalyst.
8. The method for preparing trimethylsilane according to claim 7, characterized in that: The Lewis acid catalyst is one or more of metal halides, trifluoromethanesulfonic acid or trifluoromethanesulfonate mixed in any proportion.
9. The method for preparing trimethylsilane according to claim 1, characterized in that: In S3, the dropping speed of the reducing agent solution is controlled at 3d / s-1d / 5s; the dropping speed of the catalyst solution is controlled at 1d / s-10d / s; and during the dropping of the reducing agent solution, nitrogen is used to gently sweep the reaction system.
10. The method for preparing trimethylsilane according to claim 1, characterized in that: During the whole process of S3, the stirring speed is controlled to be 100 r / min-200 r / min, and the temperature is 20° C.-100° C.; the reduction hydrogenation reaction time is 1 h-7 h.