Preparation method and equipment of phenyl organic silicon oxygen compound
By reflux reaction between the benzene source containing lithium and the silicon source, the problem of low yield of phenyl silicone oxygen compounds in the prior art is solved, and high yield and high purity product preparation is achieved, meeting downstream usage requirements and reducing costs.
Patent Information
- Application Number
- CN202510100795.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-22
- Publication Date
- 2025-05-02
AI Technical Summary
In the prior art, the yield of the preparation method of m-methylphenyltrimethoxysilane and (p-tert-butoxy)phenyltrimethoxysilane is relatively low, and the yield of other phenylorganosiloxanes is generally insufficient, and the overall yield of the product is between 30 and 40%.
The reflux reaction is carried out with the silicon source using a lithium-containing benzene source, and the reaction activity and yield are improved by controlling the reaction conditions such as pressure, temperature and stirring conditions. The method includes mixing the benzene source, the silicon source and the organic solvent for reflux reaction, the preferred molar ratio and reaction conditions are 0.5 to 1.1:1 to the molar ratio of the silicon source to the benzene source, the total volume ratio of the organic solvent to the benzene source and the silicon source, the temperature of 40 to 80°C and the pressure of 0 to 50 kPa, and the reaction time is 0.5 to 3 hours.
The high yield preparation of phenyl silicone oxygen compounds is achieved, with a yield of more than 56%, and the product purity reaches more than 99.5%, which meets downstream usage requirements and reduces production costs.
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Figure CN119912483A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of organic compound preparation, and specifically relates to a method and equipment for preparing a phenyl organic silicon oxide compound. Background Art
[0002] As phenyl organic silicon oxide compounds, m-methylphenyltrimethoxysilane (m-Me-PhTMOS) and (p-tert-butyloxy)phenyltrimethoxysilane (t-Bu-PhTMOS) are mainly used as crosslinking agents, surfactants or as intermediates of organic silicon materials. They are usually mixed with integrated circuit photoresists to improve lithography performance.
[0003] However, there is no report on the direct preparation of m-methylphenyltrimethoxysilane and (p-tert-butyloxy)phenyltrimethoxysilane, and the preparation methods of other phenyl organic silicon oxides generally have low yields, with the overall product yield being 30-40%. Summary of the invention
[0004] The purpose of the present invention is to provide a method and equipment for preparing a phenyl organic silicon oxide compound. The yield of the preparation method provided by the present invention is above 56%.
[0005] In order to achieve the above object, the present invention provides the following technical solutions:
[0006] The present invention provides a method for preparing a phenyl organic silicon oxide compound, comprising the following steps:
[0007] A benzene source, a silicon source and an organic solvent are mixed and subjected to a reflux reaction to obtain a phenyl organic silicon oxide compound.
[0008] The phenyl organic silicon oxygen compound is m-methylphenyltrimethoxysilane or (p-tert-butyloxy)phenyltrimethoxysilane; when the phenyl organic silicon oxygen compound is m-methylphenyltrimethoxysilane, the benzene source is m-tolyllithium; when the phenyl organic silicon oxygen compound is (p-tert-butyloxy)phenyltrimethoxysilane, the benzene source is p-tert-butyloxyphenyllithium.
[0009] Preferably, the silicon source is trimethoxychlorosilane.
[0010] Preferably, the molar ratio of the silicon source to the benzene source is 0.5 to 1.1:1; and the ratio of the volume of the organic solvent to the total volume of the benzene source and the silicon source is 6 to 10:1.
[0011] Preferably, the pressure of the reflux reaction is 0-50 kPa, the temperature is 40-80° C., and the insulation reaction time is 0.5-3 h; the reflux reaction is carried out under stirring conditions; and the reflux reaction is carried out in a protective atmosphere.
[0012] Preferably, the reflux reaction further includes purifying the obtained product; the purification is distillation; the distillation includes sequentially performing a first distillation and a second distillation; the temperature of the first distillation is 60 to 100°C, and the distillation pressure is -50 to 0 kPa; the temperature of the second distillation is 100 to 180°C, and the distillation pressure is -90 to -50 kPa.
[0013] The present invention also provides an equipment used in the preparation method described in the above scheme, comprising a kettle reactor, a first distillation tower and a second distillation tower connected in sequence; the kettle reactor is provided with a mechanical stirrer; the feed port of the kettle reactor is arranged at the top; the entire exterior of the kettle reactor is provided with a temperature control jacket, and the temperature is controlled by a high and low temperature integrated machine; the first distillation tower is a packed tower, and the packing of the first distillation tower includes one or more of stainless steel θ ring packing, triangular spiral packing and glass spring packing; the second distillation tower is a packed tower, and the packing of the second distillation tower includes one or more of stainless steel θ ring packing, triangular spiral packing and glass spring packing.
[0014] Preferably, the equipment further comprises a collecting tank; and the kettle reactor is connected to the first distillation tower via the collecting tank.
[0015] Preferably, the equipment further comprises a filtering device; the kettle reactor is connected to the collecting tank via the filtering device.
[0016] Preferably, the equipment further comprises a first delivery pump and a second delivery pump, the collecting tank is connected to the first distillation tower via the first delivery pump; the first distillation tower is connected to the second distillation tower via the second delivery pump.
[0017] Preferably, the equipment further comprises a solvent tank and a silicon source tank; the solvent tank is connected to the feed port of the autoclave reactor, and the silicon source tank is connected to the feed port of the autoclave reactor.
[0018] The present invention provides a method for preparing a phenyl organic silicon oxide compound. The present invention adopts a lithium-containing benzene source, refluxes a silicon source and a benzene source to obtain a phenyl organic silicon oxide compound, improves the reaction activity, and the increase in the reflux reaction temperature promotes the forward progress of the reaction, the overall yield is high and the yield is stable, the reaction yield is above 56%, the reaction conditions are easy to control, the preparation efficiency is high, the product purity is above 99.5%, the product purity meets the downstream use requirements, and the cost is low.
[0019] The present invention also provides a device used in the preparation method described in the above scheme. The device provided by the present invention has a simple structure, is easy to disassemble, load, operate and repair, and can perform batch and efficient reactions. BRIEF DESCRIPTION OF THE DRAWINGS
[0020] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.
[0021] Figure 1 A schematic diagram of the structure of the equipment used in the method for preparing the phenyl organic silicon oxide compound provided by the present invention;
[0022] Reference numerals: 1 is a kettle reactor, 2 is a first distillation tower, 3 is a second distillation tower, 4 is a collecting tank, 5 is a filtering device, 6 is a first delivery pump, 7 is a second delivery pump, 8 is a solvent tank, 9 is a dryer, and 10 is a silicon source tank. DETAILED DESCRIPTION
[0023] The present invention provides a method for preparing a phenyl organic silicon oxide compound, comprising the following steps:
[0024] A benzene source, a silicon source and an organic solvent are mixed and subjected to a reflux reaction to obtain a phenyl organic silicon oxide compound.
[0025] In the present invention, the phenyl organic silicon oxygen compound is preferably m-methylphenyltrimethoxysilane or (p-tert-butyloxy)phenyltrimethoxysilane; when the phenyl organic silicon oxygen compound is m-methylphenyltrimethoxysilane, the benzene source is preferably m-tolyllithium; when the phenyl organic silicon oxygen compound is (p-tert-butyloxy)phenyltrimethoxysilane, the benzene source is preferably p-tert-butyloxyphenyllithium.
[0026] In the present invention, the method for preparing the m-tolyllithium is preferably: mixing m-substituted toluene, a lithium salt and a good solvent (referred to as a first mixing to obtain a first reaction solution) to carry out a nucleophilic substitution reaction.
[0027] In the present invention, the meta-substituted toluene preferably includes one or more of meta-chlorotoluene, meta-bromotoluene and meta-iodotoluene; the lithium salt is preferably n-butyllithium; the mass ratio of the meta-substituted toluene to the lithium salt is preferably 1:1-2.2, specifically 1:1, 1:1.2, 1:1.5, 1:1.8, 1:2 or 1:2.2; the good solvent is preferably an alkane; the alkane is preferably a C1-C10 alkane; the C1-C10 alkane is preferably n-hexane; the concentration of the lithium salt in the first reaction solution is preferably 1-3 mol / L, specifically is 1mol / L, 1.5mol / L, 2mol / L, 2.5mol / L or 3mol / L; the first mixing is preferably carried out in an ice-water bath; the temperature of the nucleophilic substitution reaction is preferably room temperature, the time is preferably 1-2h, specifically 1.5h; the nucleophilic substitution reaction is preferably carried out under stirring conditions; after the nucleophilic substitution reaction, it is preferably further included to separate the obtained product system into solid and liquid and then concentrate it; the solid-liquid separation is preferably filtration; the concentration is preferably reduced pressure concentration; the multiple of the concentration is preferably 3-5 times, specifically 4 times.
[0028] In the present invention, the method for preparing p-tert-butoxyphenyllithium is preferably as follows: phenyllithium, tert-butanol and a good solvent are mixed (referred to as the second mixing) to carry out a substitution reaction.
[0029] In the present invention, the molar ratio of tert-butanol and phenyllithium is preferably 1:1-2.2, specifically 1:1, 1:1.2, 1:1.5, 1:1.8, 1:2 or 1:2.2; the good solvent is preferably an alkane; the alkane is preferably a C1-C10 alkane; the C1-C10 alkane is preferably n-hexane; the volume ratio of phenyllithium and good solvent is preferably 0.2-0.8:1, specifically 0.4:1; the temperature of the second mixing is preferably 20-30°C, specifically 25°C; after the second mixing, preferably the mixed system is heated; the heating rate is preferably 2-5°C / min, specifically 3°C / min; the temperature of the substitution reaction is preferably 30-50°C, specifically 30°C, 35°C, 40°C, 45°C or 50°C, and the insulation reaction time is preferably 1-2h, specifically 1.5h; after the substitution reaction, preferably the obtained product system is concentrated; the concentration multiple is preferably 3-5 times, specifically 4 times.
[0030] In the present invention, the silicon source is preferably trimethoxychlorosilane.
[0031] In the present invention, the molar ratio of the silicon source to the benzene source is preferably 0.5 to 1.1:1, specifically 0.5:1, 0.6:1, 0.7:1, 0.8:1, 0.9:1, 1:1 or 1.1:1.
[0032] In the present invention, the organic solvent is preferably an alkane; the alkane is preferably a C1-C10 alkane; the C1-C10 alkane preferably includes one or more of n-hexane, n-pentane and n-heptane; the purity of the organic solvent is preferably not less than 99.5%.
[0033] In the present invention, the organic solvent is preferably dried before use; the drying is preferably molecular sieve drying; the molecular sieve used in the molecular sieve drying is preferably one or more of 4A molecular sieve and 5A molecular sieve; the target moisture content of the drying is preferably not higher than 5ppm, specifically 5ppm, 4ppm, 3ppm, 2ppm or 1ppm. The present invention reduces the occurrence of side reactions by using the above organic solvents.
[0034] In the present invention, the ratio of the volume of the organic solvent to the total volume of the benzene source and the silicon source is preferably 6 to 10:1, specifically 6:1, 7:1, 8:1, 9:1 or 10:1.
[0035] In the present invention, the benzene source, silicon source and organic solvent are preferably used in liquid phase; the benzene source, silicon source and organic solvent are preferably added to the reactor by passing them into the reactor; the feed flow rates of the benzene source, silicon source and organic solvent are independently preferably 5 to 10 L / h, specifically 5 L / h, 6 L / h, 7 L / h, 8 L / h, 9 L / h or 10 L / h.
[0036] In the present invention, the pressure of the reflux reaction is preferably 0-50 kPa, specifically 0 kPa, 10 kPa, 20 kPa, 30 kPa, 40 kPa or 50 kPa, the temperature is preferably 40-80 ° C, specifically 40 ° C, 50 ° C, 60 ° C, 70 ° C or 80 ° C, and the insulation reaction time is preferably 0.5-3 h, specifically 0.5 h, 1 h, 1.5 h, 2 h, 2.5 h or 3 h.
[0037] In the present invention, the reflux reaction is preferably carried out under stirring conditions; the stirring speed is preferably 100-200 rpm, specifically 140 rpm or 170 rpm; the reflux reaction is preferably carried out in a protective atmosphere; the protective atmosphere is preferably nitrogen.
[0038] In the present invention, after the reflux reaction, the obtained product system is preferably further treated; the post-treatment is preferably cooling and solid-liquid separation in sequence; the final temperature of the cooling is preferably room temperature; the solid-liquid separation is preferably filtration; the filtration accuracy is preferably 50 to 100 nm, specifically 50 nm, 75 nm or 100 nm.
[0039] In the present invention, after the reflux reaction, the obtained product is preferably purified; the purification is preferably distillation; the distillation preferably includes sequentially performing a first distillation and a second distillation; the temperature of the first distillation is preferably 60 to 100°C, specifically 70°C, 80°C or 90°C, and the distillation pressure is preferably -50 to 0 kPa, specifically -40 kPa, -30 kPa, -20 kPa or -10 kPa; the temperature of the second distillation is preferably 100 to 180°C, specifically 120°C or 150°C, and the distillation pressure is preferably -90 to -50 kPa, specifically -80 kPa, -70 kPa or -60 kPa. The present invention can effectively remove metal and non-metal impurities by removing light and heavy impurities through two-stage distillation, and has a good effect on the stability of product quality.
[0040] The present invention also provides an apparatus for the preparation method described in the above scheme, comprising a tank reactor 1, a first distillation tower 2 and a second distillation tower 3 connected in sequence.
[0041] The structure of the device provided by the present invention is as follows Figure 1 As shown below, combined Figure 1 The device provided by the present invention is introduced:
[0042] The equipment provided by the present invention includes a kettle reactor 1; the material of the kettle reactor 1 is preferably stainless steel; the stainless steel is preferably 316L stainless steel; the interior of the kettle reactor 1 is preferably subjected to mechanical polishing treatment; the roughness (Ra) of the polishing treatment is preferably less than 0.4 μm; the kettle reactor 1 is preferably provided with mechanical stirring; the top, left side and bottom of the kettle reactor 1 are preferably provided with multiple inlets and outlets for temperature measurement, pressure measurement and gas inlet and outlet; the feed port of the kettle reactor 1 is preferably arranged at the top; the entire exterior of the kettle reactor 1 is preferably provided with a temperature control jacket, which is temperature controlled by a high and low temperature integrated machine; the temperature of the temperature control jacket is preferably 60 to 100°C.
[0043] The equipment provided by the present invention includes a first distillation tower 2; the first distillation tower 2 is preferably a packed tower; the packing of the first distillation tower 2 preferably includes one or more of stainless steel θ ring packing, triangular spiral packing and glass spring packing, and is more preferably stainless steel θ ring packing; the size of the packing is preferably 3×3mm; the material of the first distillation tower 2 is preferably stainless steel; the stainless steel is preferably 316L; the interior of the first distillation tower 2 is preferably electrolytically polished; the bottom volume of the first distillation tower 2 is preferably 1~2L, and the packing height is preferably 1~2m; the top of the first distillation tower 2 is preferably provided with water cooling; the water cooling preferably uses 7°C water; the bottom of the first distillation tower 2 is preferably provided with a heating device; the heating device is preferably heated by thermal oil.
[0044] The equipment provided by the present invention includes a second distillation tower 3; the second distillation tower 3 is preferably a packed tower; the packing of the second distillation tower 3 preferably includes one or more of stainless steel θ ring packing, triangular spiral packing and glass spring packing, and is more preferably stainless steel θ ring packing; the size of the packing is preferably 3×3mm; the material of the second distillation tower 3 is preferably stainless steel; the stainless steel is preferably 316L; the interior of the second distillation tower 3 is preferably electrolytically polished; the bottom volume of the second distillation tower 3 is preferably 2~3L, and the packing height is preferably 3~4m; the top of the second distillation tower 3 is preferably provided with water cooling; the water cooling preferably uses 7°C water; the bottom of the second distillation tower 3 is preferably provided with a heating device; the heating device is preferably heated by thermal oil.
[0045] The device provided by the present invention preferably further comprises a collecting tank 4; the kettle reactor 1 is preferably connected to the first distillation tower 2 via the collecting tank 4. The present invention facilitates analysis and detection of the reaction materials and stores the reaction materials by providing the collecting tank 4.
[0046] The device provided by the present invention preferably further comprises a filtering device 5 ; the kettle reactor 1 is preferably connected to the collecting tank 4 via the filtering device 5 .
[0047] The device provided by the present invention preferably further includes a first delivery pump 6 ; the collecting tank 4 is preferably connected to the first distillation tower 2 via the first delivery pump 6 .
[0048] The device provided by the present invention preferably further includes a second delivery pump 7 ; the first distillation tower 2 is preferably connected to the second distillation tower 3 via the second delivery pump 7 .
[0049] The device provided by the present invention preferably further comprises a solvent tank 8; the solvent tank 8 is preferably connected to the feed port of the autoclave reactor 1, and more preferably connected to the autoclave reactor 1 via a dryer 9; the dryer 9 is preferably a molecular sieve dryer.
[0050] The device provided by the present invention preferably further includes a silicon source tank 10 ; the silicon source tank 10 is preferably connected to the feed port of the autoclave reactor 1 .
[0051] In order to further illustrate the present invention, the scheme of the present invention is described in detail below in conjunction with the accompanying drawings and embodiments, but they should not be understood as limiting the protection scope of the present invention.
[0052] Example 1
[0053] (1) A 10 L autoclave reactor was completely purged with nitrogen to a dew point of -60°C. The water content of n-hexane after drying over 5A molecular sieves was 0.5 ppm.
[0054] (2) The jacket temperature of the reactor was controlled at 10° C. n-hexane and trimethoxysilyl chloride were introduced at a rate of 5 L / h, with a volume of 5 L of n-hexane and 2 kg of trimethoxysilyl chloride. The internal pressure of the reactor was controlled at 30 kPa.
[0055] (3) After the addition is completed, 1.25 kg of pre-prepared m-tolyl lithium is added, the internal pressure of the reactor is controlled to be 50 kPa, the internal reaction temperature is 80° C., and the reaction is stirred at 100-200 rpm for 2 hours. After the reaction, the reactor is cooled to room temperature, and the reaction product is passed through 100 nm and 50 nm precision filters in turn, and then pressed into a collection tank for analysis and detection. The yield of m-methylphenyltrimethoxysilane is 64%.
[0056] (4) The collected reaction liquid is sent to the vacuum distillation tower system at the rear end; the bottom volume of the first distillation tower is 2L, the packing height is 2m, the distillation pressure is -20kPa, and the temperature is 80°C; the bottom volume of the second distillation tower is 3L, the packing height is 3m, the distillation pressure is -90kPa, and the temperature is 120°C. The tower system parameters are controlled to be stable. After the reaction product is removed by light and heavy in the first distillation tower and the second distillation tower, a m-methylphenyltrimethoxysilane product with a purity of 99.5% is obtained.
[0057] Example 2
[0058] (1) A 10 L autoclave reactor was completely purged with nitrogen to a dew point of -60°C. The water content of n-hexane after drying over 5A molecular sieves was 0.5 ppm.
[0059] (2) The jacket temperature of the reactor was controlled at 10° C. n-hexane and trimethoxysilyl chloride were introduced at a rate of 5 L / h, with a volume of 5 L of n-hexane and 2 kg of trimethoxysilyl chloride. The internal pressure of the reactor was controlled at 30 kPa.
[0060] (3) After the addition is completed, 2.0 kg of pre-prepared p-tert-butoxyphenyl lithium is added, the internal pressure of the reactor is controlled to be 50 kPa, the internal reaction temperature is 80° C., and the reaction is continued at 100-200 rpm for 2 hours. After the reaction, the reactor is cooled to room temperature, and the reaction product is passed through 100 nm and 50 nm precision filters in turn, and then pressed into a collection tank for analysis and detection. The yield of (p-tert-butoxy)phenyltrimethoxysilane is 56%.
[0061] (4) The collected reaction liquid is sent to the vacuum distillation tower system at the rear end; the bottom volume of the first distillation tower is 2L, the packing height is 2m, the distillation pressure is -20kPa, and the temperature is 90°C; the bottom volume of the second distillation tower is 3L, the packing height is 3m, the distillation pressure is -90kPa, and the temperature is 130°C. The tower system parameters are controlled to be stable. After the reaction product is removed by light and heavy in the first distillation tower and the second distillation tower, a (p-tert-butyloxy)phenyltrimethoxysilane product with a purity of 99.6% is obtained.
[0062] Example 3
[0063] (1) A 10 L autoclave reactor was completely purged with nitrogen to a dew point of -60°C. The water content of n-pentane after drying over 5A molecular sieves was 0.5 ppm.
[0064] (2) The jacket temperature of the reactor was controlled at 10° C. n-pentane and trimethoxysilyl chloride were introduced at a rate of 5 L / h, with a volume of 5 L of n-pentane and 2 kg of trimethoxysilyl chloride. The internal pressure of the reactor was controlled at 30 kPa.
[0065] (3) After the addition is completed, 1.5 kg of pre-prepared m-tolyl lithium is added, the internal pressure of the reactor is controlled to be 50 kPa, the internal reaction temperature is 50° C., and the reaction is continued at 100-200 rpm for 2 hours. After the reaction, the reactor is cooled to room temperature, and the reaction product is passed through 100 nm and 50 nm precision filters in turn, and then pressed into a collection tank for analysis and detection. The yield of m-methylphenyltrimethoxysilane is 68%.
[0066] (4) The collected reaction liquid is sent to the vacuum distillation tower system at the rear end; the bottom volume of the first distillation tower is 2L, the packing height is 2m, the distillation pressure is -20kPa, and the temperature is 40°C; the bottom volume of the second distillation tower is 3L, the packing height is 3m, the distillation pressure is -90kPa, and the temperature is 120°C. The tower system parameters are controlled to be stable. After the reaction product is removed by light and heavy removal in the first distillation tower and the second distillation tower respectively, a m-methylphenyltrimethoxysilane product with a purity of 99.8% is obtained.
[0067] Example 4
[0068] (1) A 10 L autoclave reactor was completely purged with nitrogen to a dew point of -60°C. The water content of n-heptane after drying over 5A molecular sieves was 0.5 ppm.
[0069] (2) The jacket temperature of the reactor was controlled at 10° C. n-heptane and trimethoxysilyl chloride were introduced in sequence at a rate of 5 L / h. The volume of n-heptane was 5 L, and the volume of trimethoxysilyl chloride was 2 kg. At the same time, the internal pressure of the reactor was controlled at 30 kPa.
[0070] (3) After the addition is completed, 2.5 kg of pre-prepared p-tert-butoxyphenyl lithium is added, the internal pressure of the reactor is controlled to be 50 kPa, the internal reaction temperature is 110° C., and the reaction is continued at 100-200 rpm for 2 hours. After the reaction, the reactor is cooled to room temperature, and the reaction product is passed through 100 nm and 50 nm precision filters in turn, and then pressed into a collection tank for analysis and detection. The yield of (p-tert-butoxy)phenyltrimethoxysilane is 56%.
[0071] (4) The collected reaction liquid is sent to the vacuum distillation tower system at the rear end; the bottom volume of the first distillation tower is 2L, the packing height is 2m, the distillation pressure is -20kPa, and the temperature is 90°C; the bottom volume of the second distillation tower is 3L, the packing height is 3m, the distillation pressure is -90kPa, and the temperature is 130°C. The tower system parameters are controlled to be stable. After the reaction product is removed by light and heavy in the first distillation tower and the second distillation tower, a (p-tert-butyloxy)phenyltrimethoxysilane product with a purity of 99.7% is obtained.
[0072] It can be seen from the above embodiments that the preparation method provided by the present invention has a high and stable yield, a reaction yield of more than 56%, easily controllable reaction conditions, high preparation efficiency, a product purity of more than 99.5%, and the product purity meets the requirements of downstream use with low cost.
[0073] Although the above embodiment describes the present invention in detail, it is only a part of the embodiments of the present invention, not all of the embodiments. Other embodiments can be obtained based on this embodiment without creativity, and these embodiments all fall within the protection scope of the present invention.
Claims
1. A method for preparing a phenyl organic silicon oxide compound, characterized in that: The following steps are involved: A benzene source, a silicon source and an organic solvent are mixed and subjected to a reflux reaction to obtain a phenyl organic silicon oxide compound. The phenyl organic silicon oxygen compound is m-methylphenyltrimethoxysilane or (p-tert-butyloxy)phenyltrimethoxysilane; when the phenyl organic silicon oxygen compound is m-methylphenyltrimethoxysilane, the benzene source is m-tolyllithium; when the phenyl organic silicon oxygen compound is (p-tert-butyloxy)phenyltrimethoxysilane, the benzene source is p-tert-butyloxyphenyllithium.
2. The preparation method according to claim 1, characterized in that: The silicon source is trimethoxychlorosilane.
3. The preparation method according to claim 1 or 2, characterized in that: The molar ratio of the silicon source to the benzene source is 0.5-1.1:1; the ratio of the volume of the organic solvent to the total volume of the benzene source and the silicon source is 6-10:
1.
4. The preparation method according to claim 1, characterized in that: The pressure of the reflux reaction is 0-50 kPa, the temperature is 40-80° C., and the insulation reaction time is 0.5-3 h; the reflux reaction is carried out under stirring conditions; and the reflux reaction is carried out in a protective atmosphere.
5. The preparation method according to claim 1 or 4, characterized in that: After the reflux reaction, the obtained product is purified; the purification is distillation; the distillation includes a first distillation and a second distillation in sequence; the temperature of the first distillation is 60 to 100°C, and the distillation pressure is -50 to 0 kPa; the temperature of the second distillation is 100 to 180°C, and the distillation pressure is -90 to -50 kPa.
6. An apparatus for the preparation method according to any one of claims 1 to 5, comprising a kettle reactor (1), a first distillation tower (2) and a second distillation tower (3) connected in sequence; the kettle reactor (1) is provided with a mechanical stirrer; the feed port of the kettle reactor (1) is arranged at the top; the entire exterior of the kettle reactor (1) is provided with a temperature control jacket, and the temperature is controlled by a high and low temperature integrated machine; the first distillation tower (2) is a packed tower, and the packing of the first distillation tower (2) includes one or more of stainless steel θ ring packing, triangular spiral packing and glass spring packing; the second distillation tower (3) is a packed tower, and the packing of the second distillation tower (3) includes one or more of stainless steel θ ring packing, triangular spiral packing and glass spring packing.
7. The device according to claim 1, characterized in that It also comprises a collecting tank (4); the kettle reactor (1) is connected to the first distillation tower (2) via the collecting tank (4).
8. The device according to claim 1 or 7, characterized in that It also comprises a filtering device (5); the kettle reactor (1) is connected to the collecting tank (4) via the filtering device (5).
9. The device according to claim 1, characterized in that It also comprises a first delivery pump (6) and a second delivery pump (7), wherein the collecting tank (4) is connected to the first distillation tower (2) via the first delivery pump (6); and the first distillation tower (2) is connected to the second distillation tower (3) via the second delivery pump (7).
10. The device according to claim 1, characterized in that It also comprises a solvent tank (8) and a silicon source tank (10); the solvent tank (8) is connected to the feed port of the autoclave reactor (1), and the silicon source tank (10) is connected to the feed port of the autoclave reactor (1).