Microchannel synthesis method of γ-aminopropyltriethoxysilane

By combining a microchannel reactor with a core-shell bimetallic catalyst, and using cheap and readily available acrylonitrile and hydrogen as raw materials, γ-aminopropyltriethoxysilane is synthesized in one step under mild conditions, solving the problems of high reaction pressure and low production efficiency in the existing technology and achieving efficient KH-550 synthesis.

CN117024468BActive Publication Date: 2025-09-19ZHEJIANG UNIV
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Patent Information

Application Number
CN202310768029.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-06-27
Publication Date
2025-09-19
Estimated Expiration
2043-06-27

AI Technical Summary

Technical Problem

The existing KH-550 synthesis process has problems such as high reaction pressure and low production efficiency. The raw material 2-cyanoethyltriethoxysilane is not easy to obtain and the hydrogenation efficiency of the autoclave reaction is low.

Method used

Using a microchannel reactor and a core-shell bimetallic catalyst, γ-aminopropyltriethoxysilane was synthesized in a single step from triethoxysilane and acrylonitrile under the action of a catalyst. Cheap and readily available acrylonitrile and hydrogen were used as raw materials, and the reaction was carried out under relatively mild conditions.

Benefits of technology

The synthesis of KH-550 with high atom economy and cheap and readily available raw materials is achieved, the reaction time is short, and continuous production is easy, thereby improving reaction efficiency and production efficiency.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention relates to a method for synthesizing a nitrogen-containing silane coupling agent, and specifically discloses a microchannel synthesis method for γ-aminopropyltriethoxysilane. The method comprises the following steps: using acrylonitrile, triethoxysilane and hydrogen as raw materials, and synthesizing γ-aminopropyltriethoxysilane (KH-550) in one step in a microchannel reactor under the action of a catalyst; the microchannel synthesis device used comprises a hydrogen bottle, a triethoxysilane raw material tank and an acrylonitrile raw material tank respectively connected to the inlet of the microchannel reactor; the inner wall of the microchannel reactor is loaded with a core-shell bimetallic catalyst, and the loading amount is 0.01-0.06 mg / cm 2 The present invention loads the core-shell bimetallic catalyst on the inner surface of the microchannel, which promotes the mass transfer effect between the reaction materials and the catalyst and improves the reaction efficiency.
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Description

Technical Field

[0001] The invention relates to a method for synthesizing a nitrogen-containing silane coupling agent, in particular to a method for synthesizing gamma-aminopropyltriethoxysilane through a microchannel. Background Art

[0002] Nitrogen-containing silane coupling agents currently hold the largest market share and are the most widely used. γ-Aminopropyltriethoxysilane (KH-550) was the first widely used coupling agent, boasting a history of over 40 years. Its structure features an amino group at one end that reacts with various synthetic resin molecules. At the other end, an ethoxy group attached to silicon hydrolyzes in the presence of moisture in aqueous solution or air to produce a hydroxyl group that reacts with the surfaces of glass, minerals, and inorganic fillers. It is widely used in glass fiber treatments and dental adhesives, as well as in mineral-filled thermoplastic and thermosetting resins such as phenolic, polyester, epoxy, PBT, polyamide, and carbonate.

[0003] The current reactor format for KH-550 synthesis is primarily a batch reactor. This batch reactor reaction primarily uses γ-chloropropyltriethoxysilane (CAS: 5089-70-3) and liquid ammonia as raw materials, reacting in an autoclave at relatively high pressure to produce KH-550 (e.g., patents CN104961762 and CN101768180). This process operates at reaction pressures of approximately 1-5 MPa, resulting in a significant excess of ammonia and the production of ammonium chloride, significantly impacting agitation and single-reactor production capacity. Furthermore, foreign patents disclose the production of KH-550 via hydrogenation using 2-cyanoethyltriethoxysilane as a raw material (patents PL187626B1 and DE10023003). This method primarily utilizes an autoclave as the reactor, employing a cobalt or nickel catalyst as the active metal, and carrying out the hydrogenation under high pressure. The main drawbacks of this method are the difficulty in obtaining the raw material 2-cyanoethyltriethoxysilane, the high pressures associated with the autoclave hydrogenation reaction, and the low hydrogenation efficiency.

[0004] Therefore, the existing intermittent reactor preparation process of KH-550 has many problems such as high reaction pressure and low production efficiency. Summary of the Invention

[0005] The technical problem to be solved by the present invention is to provide a method for continuously preparing KH-550 with low raw material cost, simple operation, and the characteristics of high atomic conversion rate, simple process, and convenient continuous production.

[0006] In order to solve the above technical problems, the present invention provides a microchannel synthesis method for γ-aminopropyltriethoxysilane: using acrylonitrile, triethoxysilane (CAS: 998-30-1) and hydrogen as raw materials, under the action of a catalyst, a microchannel reactor is used to synthesize γ-aminopropyltriethoxysilane (KH-550) in one step;

[0007] The mass flow rate ratio of triethoxysilane, acrylonitrile and hydrogen is 2-4:1:0.1-0.3.

[0008] Reaction formula:

[0009]

[0010] As an improvement of the microchannel synthesis method of γ-aminopropyltriethoxysilane of the present invention:

[0011] The microchannel synthesis device used includes a hydrogen bottle, a triethoxysilane raw material tank, and an acrylonitrile raw material tank respectively connected to the inlet of the microchannel reactor;

[0012] The inner wall of the microchannel reactor is loaded with a core-shell bimetallic catalyst with a loading of 0.01 to 0.06 mg / cm 2 (Preferably 0.02 mg / cm 2 );

[0013] The microchannel synthesis method comprises the following steps:

[0014] 1) Triethoxysilane, acrylonitrile, and hydrogen are pumped into a microchannel reactor at a mass flow rate ratio of 2 to 4:1:0.1 to 0.3 (preferably 2.6 to 3:1:0.18 to 0.2). The reaction temperature of the microchannel reactor is 80 to 110° C. (preferably 100 to 110° C.), the reaction pressure is 1 to 3.5 MPa (preferably 2 to 3.5 MPa), and the reaction time is 40 to 110 min (preferably 60 to 90 min).

[0015] 2) Collecting the reaction product of the microchannel reactor and performing post-processing to obtain γ-aminopropyltriethoxysilane (KH-550).

[0016] As a further improvement of the microchannel synthesis method of γ-aminopropyltriethoxysilane of the present invention: the method of loading the inner wall of the microchannel reactor with a core-shell bimetallic catalyst comprises the following steps:

[0017] A. Preparation of core-shell bimetallic catalysts:

[0018] A 1-2 M (1-2 mol / L) platinum salt solution and propylene carbonate are mixed in a volume ratio of 2-4:1, and the mixture is added to an autoclave. The air in the autoclave is replaced with hydrogen 2-3 times, and then the autoclave is filled with hydrogen to 3-5 MPa. The autoclave is heated to 40-60° C. and kept warm for 3-5 hours to obtain a Pt nano-solution.

[0019] The autoclave was opened, and a lithium salt solution having an equal volume to the platinum salt solution was added to the Pt nanoparticle solution, wherein the concentration of the lithium salt solution was 0.5 to 4 M. After replacing the air in the autoclave with hydrogen 2 to 3 times, the autoclave was filled with hydrogen to 3 to 5 MPa, and the autoclave was heated to 30 to 40° C. and kept warm for 3 to 5 hours to obtain a core-shell bimetallic catalyst solution.

[0020] B. Injecting a core-shell bimetallic catalyst solution into a microchannel reactor in an amount equal to the liquid holdup of the microchannel reactor; maintaining the temperature at 60-90° C. for 7-10 hours under the protection of an inert gas (e.g., in an insulated box with a nitrogen atmosphere) to remove water and hydrogen chloride from the core-shell bimetallic catalyst solution, thereby obtaining a microchannel with an inner layer loaded with a core-shell bimetallic catalyst; the core-shell bimetallic catalyst loading is 0.01-0.06 mg / cm 2 (Preferably 0.02 g / cm 2 ).

[0021] As a further improvement of the microchannel synthesis method of γ-aminopropyltriethoxysilane of the present invention:

[0022] The platinum salt is any one of H2PtCl6, Pt(NO3)2, (NH4)2PtCl6,

[0023] The lithium salt is any one of LiCl, LiNO3, Li2SO4, and Li2CO3.

[0024] As a further improvement of the microchannel synthesis method of γ-aminopropyltriethoxysilane of the present invention:

[0025] The inner diameter of the microchannel reactor is 0.1-100 μm, and the liquid holding capacity is 300-600 μL.

[0026] The present invention has the following technical advantages in producing KH550:

[0027] 1. The process using triethoxysilane, acrylonitrile and hydrogen as raw materials has the advantages of high atom economy and cheap and readily available raw materials;

[0028] 2. A core-shell bimetallic catalyst is used to achieve a one-pot cascade reaction of triethoxysilane and acrylonitrile addition and 2-cyanoethyltriethoxysilane hydrogenation. A microchannel reactor is also used to enhance mass transfer efficiency, allowing the reaction to proceed under milder conditions with shorter reaction times, facilitating continuous process scale-up.

[0029] 3. The catalyst of the present invention uses a core-shell bimetallic catalyst, with a palladium core and a lithium shell. The principle is that after the materials contact the catalyst, they pass through the shell (acrylonitrile and triethoxysilane addition reaction) and the core (2-cyanoethyltriethoxysilane hydrogenation reaction), allowing the reaction to proceed in a one-pot process.

[0030] The present invention loads the core-shell bimetallic catalyst on the inner surface of the microchannel, promotes the mass transfer effect between the reaction material and the catalyst, and improves the reaction efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] The specific embodiments of the present invention are further described in detail below with reference to the accompanying drawings.

[0032] Figure 1 Schematic diagram of the KH550 microchannel reaction device. DETAILED DESCRIPTION

[0033] The present invention is further described below with reference to specific embodiments, but the protection scope of the present invention is not limited thereto:

[0034] Device Example 1: A microchannel reaction device for preparing KH550, the structure of which is as follows Figure 1 As shown, it includes a microchannel reactor;

[0035] The outlet of the hydrogen cylinder is connected to the inlet of the microchannel reactor through a gas mass flow meter and a stop valve 1;

[0036] The outlet of the triethoxysilane raw material tank is connected to the inlet of the microchannel reactor through pump I and stop valve 2 in sequence;

[0037] The outlet of the acrylonitrile raw material tank is connected to the inlet of the microchannel reactor through pump II and stop valve 3 in sequence;

[0038] The outlet of the microchannel reactor is connected to the inlet of the material collection tank after passing through the back pressure valve. The upper outlet of the material collection tank is provided with a vent valve, and the lower material outlet is provided with a stop valve 4. The back pressure valve is used to control the reaction pressure of the microchannel reactor.

[0039] The method for loading the catalyst on the inner wall of the microchannel is to carry out the following steps in sequence:

[0040] A. Preparation of core-shell bimetallic catalysts:

[0041] A chloroplatinic acid aqueous solution (with a concentration of 1 to 2 M) and propylene carbonate are mixed in a volume ratio of 2 to 4:1 and added to an autoclave. The autoclave is closed, and the air in the autoclave is replaced with hydrogen 2 to 3 times. The autoclave is then filled with hydrogen to 3 to 5 MPa, and the autoclave is heated to 40 to 60° C. and kept warm for 3 to 5 hours to prepare a Pt nano-solution.

[0042] Reaction formula: H2PtCl6+2H2→Pt+6HCl

[0043] The autoclave was opened, and an aqueous lithium chloride solution (concentration of 0.5 to 4 M) of an equal volume to the platinum salt solution was added to the Pt nano solution. The autoclave was closed, and the air in the autoclave was replaced with hydrogen 2 to 3 times. The autoclave was then filled with hydrogen to 3 to 5 MPa, and the autoclave was heated to 30 to 40° C. and kept warm for 3 to 5 hours to prepare a core-shell bimetallic catalyst solution (the core was Pt nanometal and the shell was Li nanometal).

[0044] Reaction formula: 2LiCl + H2 → 2Li + 2HCl

[0045] B. Inject the prepared core-shell bimetallic catalyst solution into the microchannel reactor in an amount equal to the liquid holdup volume of the microchannel reactor; in a nitrogen atmosphere incubator, keep the temperature at 60-90°C for 7-10 hours to remove water and HCl from the core-shell bimetallic catalyst solution, thereby obtaining a microchannel with an inner layer loaded with a core-shell bimetallic catalyst. The core-shell bimetallic catalyst loading is 0.02 mg / cm 2 ;

[0046] Core-shell bimetallic catalyst loading:

[0047]

[0048] Where c loading is the catalyst loading, c1 is the concentration of the chloroplatinic acid aqueous solution, v1 is the volume of the chloroplatinic acid aqueous solution, c2 is the concentration of the lithium chloride aqueous solution, v2 is the volume of the lithium chloride aqueous solution, S is the inner wall area of ​​the microchannel reactor, and V is the volume of the core-shell bimetallic catalyst solution prepared in step A.

[0049] During actual operation, stop valves 1 to 3 are all in the open state. When the reaction is completed, stop valves 1, 2, 3 and pumps 1 and 2 are closed, and finally stop valve 4 is opened.

[0050] Triethoxysilane, acrylonitrile, and hydrogen are pumped into the microchannel reactor by their respective raw material pumps. The reaction liquid flowing out of the microchannel reactor flows into a collection tank through a back pressure valve. The product KH-550 is purified by vacuum distillation.

[0051] The products obtained in the following cases were verified by conventional NMR and were indeed KH-550.

[0052] Example 1-1: A method for preparing KH-550, comprising the following steps:

[0053] The microchannel reactor has a liquid holding capacity of 385uL and an inner diameter of 25um.

[0054] The catalyst is a core-shell bimetallic catalyst (core is Pt nanometal, shell is Li nanometal), with a molar ratio of 1:1 and a core-shell bimetallic catalyst loading of approximately 0.02 mg / cm 2 .

[0055] The method for loading the catalyst on the inner wall of the microchannel is to carry out the following steps in sequence:

[0056] A. Preparation of core-shell bimetallic catalysts:

[0057] Aqueous chloroplatinic acid solution (1 M concentration) and propylene carbonate were mixed in a volume ratio of 2.5:1 and added to an autoclave. The autoclave was closed and the air in the autoclave was replaced with hydrogen 2 to 3 times. The autoclave was then filled with hydrogen to 3.5 MPa and heated to 50°C for 4 hours to prepare a Pt nanosolution.

[0058] The autoclave was opened, and an aqueous lithium chloride solution (concentration of 1 M) of the same volume as the platinum salt solution was added to the Pt nanosolution. The autoclave was closed, and the air in the autoclave was replaced with hydrogen 2 to 3 times. The autoclave was then filled with hydrogen to 3.5 MPa, and heated to 30°C and kept warm for 4 hours to prepare a core-shell bimetallic catalyst solution (the core was Pt nanometal and the shell was Li nanometal).

[0059] B. The prepared core-shell bimetallic catalyst solution was injected into a microchannel reactor with an injection volume of 385 uL. The reaction was kept at 80°C in an insulated box with a nitrogen atmosphere for 9 hours to remove moisture and HCl from the core-shell bimetallic catalyst solution. A microchannel with an inner layer loaded with a core-shell bimetallic catalyst was obtained. The Pt / Li in the prepared core-shell bimetallic catalyst was 1:1 (molar ratio).

[0060] Triethoxysilane, acrylonitrile, and hydrogen were pumped into the microchannel reactor at flow rates of 60 μg / min, 20 μg / min, and 4 μg / min, respectively. The reaction temperature was 105°C, and the reaction residence time was 60 minutes. The pressure was stabilized at 2.5 MPa by controlling the backpressure valve after the microchannel reactor. The reaction solution flowed through the backpressure valve and into a collection tank. After purification by vacuum distillation, the fraction at 120-122°C at a pressure of -93.8 kPa was collected to obtain the KH-550 product.

[0061] When the amount of triethoxysilane used is 60 g, the amount of KH-550 obtained is 76.8 g. The calculation formula for the KH-550 yield is:

[0062]

[0063] Wherein, m2 is the product mass of KH-550, and m1 is the amount of triethoxysilane used.

[0064] Examples 1-2 to 1-5

[0065] By changing the reaction temperature, the product yield was detected and the following data were obtained (Table 1).

[0066] Table 1. Effect of reaction temperature on KH-550 yield

[0067]

[0068] Examples 2-1 to 2-4

[0069] Compared to Example 1-1, the flow rates of triethoxysilane, acrylonitrile, and hydrogen were changed, but their flow rate ratio remained unchanged, and the residence time of the reaction was changed. The product yield was tested and the following data were obtained (Table 2).

[0070] Table 2. Effect of reaction residence time on KH-550 yield

[0071] Group Residence time (min) KH-550 yield (%) Example 1-1 60 95 Example 2-1 30 63 Example 2-2 48 76 Example 2-3 72 97 Examples 2-4 90 96

[0072] Examples 3-1 to 3-4

[0073] Compared with Example 1-1, the reaction pressure was changed by adjusting the back pressure valve, and the rest was the same as Example 1-1. The product yield was tested and the following data were obtained (Table 3).

[0074] Table 3. Effect of reaction pressure on KH-550 yield

[0075] Group Reaction pressure P (MPa) KH-550 yield (%) Example 1-1 2.5 95 Example 3-1 2 92 Example 3-2 1.5 81 Example 3-3 3 96 Examples 3-4 3.5 97

[0076] Examples 4-1 to 4-4

[0077] Compared to Example 1-1, the mass flow rates of triethoxysilane, acrylonitrile, and hydrogen were varied to adjust their flow ratios accordingly, while maintaining the total flow rate constant. This ensured that the reaction residence time remained unchanged (still 60 min). The remaining conditions were identical to those of Example 1-1. The product yields were measured, yielding the following data (Table 4).

[0078] Table 4. Effect of flow rate ratio on KH-550 yield

[0079]

[0080] Example 5 series

[0081] Compared to Example 1-1, the concentrations of the H2PtCl6 aqueous solution and the LiCl aqueous solution during the preparation of the core-shell bimetallic catalyst were changed; otherwise, the same as in Example 1-1. The product yield was measured, and the following data were obtained (Table 5).

[0082] Table 5. Effect of catalyst on KH-550 yield

[0083]

[0084] Example 6 series

[0085] Compared to Example 1-1, the salts used in the catalyst precursor were changed, specifically the platinum salt and lithium salt used in the preparation of the core-shell bimetallic catalyst. All other conditions were the same as in Example 1-1. The product yield was measured, and the following data was obtained (Table 6).

[0086] Table 6. Effect of catalyst precursor on KH-550 yield

[0087] Group platinum salts lithium salts KH-550 yield (%) Example 1-1 <![CDATA[H2PtCl6]]> LiCl 95 Example 6-1 <![CDATA[Pt(NO3)2]]> LiCl 90 Example 6-2 <![CDATA[(NH4)2PtCl6]]> LiCl 85 Example 6-3 <![CDATA[H2PtCl6]]> <![CDATA[LiNO3]]> 94 Example 6-4 <![CDATA[H2PtCl6]]> <![CDATA[Li2SO4(0.5M)]]> 86

[0088] Note: Except for the concentration of Li2SO4 as described in Table 6 above, the concentrations of other platinum salts and lithium salts are the same as those in Example 1-1.

[0089] Comparative Example 1-1: Compared with Example 1-1, the catalyst composition was changed, that is, the method for loading the catalyst on the inner wall of the microchannel was to perform the following steps in sequence:

[0090] Chloroplatinic acid solution (concentration of 1 M) and propylene carbonate were mixed in a volume ratio of 2.5:1 and added to an autoclave. The autoclave was closed and the air in the autoclave was replaced with hydrogen 2 to 3 times. The autoclave was then filled with hydrogen to 3.5 MPa and heated to 50°C for 4 hours to prepare a Pt nano-solution.

[0091] The prepared Pt nano solution was injected into the microchannel reactor in the same volume as in Example 1-1, and kept at 80°C in an insulated box under a nitrogen atmosphere for 9 hours to remove water and HCl in the Pt nano solution, thereby obtaining a microchannel with an inner layer loaded with a Pt metal catalyst.

[0092] The rest is the same as Example 1-1.

[0093] Comparative Example 1-2: Compared with Example 1-1, the catalyst composition was changed, that is, the method for loading the catalyst on the inner wall of the microchannel was to perform the following steps in sequence:

[0094] Lithium chloride solution (concentration of 1M) and propylene carbonate were mixed in a volume ratio of 2.5:1 and added to an autoclave. The autoclave was closed and the air in the autoclave was replaced with hydrogen 2 to 3 times. The autoclave was then filled with hydrogen to 3.5 MPa and heated to 30°C for 4 hours to prepare a Li nano-solution.

[0095] The prepared Li nano solution was injected into the microchannel reactor in the same volume as in Example 1-1, and kept at 80° C. for 9 h in an insulated box under a nitrogen atmosphere to remove water and HCl from the Li nano solution, thereby obtaining a microchannel with a Li catalyst loaded in the inner layer.

[0096] The rest is the same as Example 1-1.

[0097] Comparative Example 1-3: Compared with Example 1-1, the catalyst composition was changed, that is, the method for loading the catalyst on the inner wall of the microchannel was to perform the following steps in sequence:

[0098] Preparation of bimetallic catalyst: Chloroplatinic acid solution (concentration of 1M), lithium chloride solution (concentration of 1M) and propylene carbonate were mixed in a volume ratio of 2.5:2.5:1 and added to an autoclave. The autoclave was closed and the air in the autoclave was replaced with hydrogen 2 to 3 times. The autoclave was then filled with hydrogen to 3.5 MPa and heated to 50°C for 4 hours to prepare a Pt and Li mixed nanometal solution.

[0099] The prepared Pt and Li mixed nanometal solution was injected into a microchannel reactor with the same injection volume as in Example 1-1. The solution was kept at 80°C in an insulated box under a nitrogen atmosphere for 9 hours to remove moisture and HCl from the Pt and Li mixed nanometal solution. A microchannel having an inner layer loaded with Pt and Li mixed nanometals was obtained. The Pt / Li in the prepared Pt and Li mixed nanometal catalyst was 1:1 (molar ratio).

[0100] The rest is the same as Example 1-1.

[0101] The results of Comparative Examples 1-1 to 1-3 are shown in Table 7 below.

[0102] Table 7. Effect of catalyst on reaction performance

[0103]

[0104] Comparative Example 2-1: Compared to Example 1-1, the reactor type was changed. Specifically, 60 g of triethoxysilane and 20 g of acrylonitrile were added to an autoclave, followed by 10 mL of a core-shell bimetallic catalyst solution. The air in the autoclave was replaced with hydrogen 2-3 times. The hydrogen pressure in the autoclave was controlled at 2.5 MPa. A stirrer was installed in the reactor for stirring. The reaction temperature was 105°C and the reaction time was 60 min. After the reaction, the hydrogen was discharged, the autoclave was opened, and the reaction solution was purified by vacuum distillation. The fraction at 120-122°C at a pressure of -93.8 kPa was collected to obtain the KH-550 product. The preparation of the core-shell bimetallic catalyst solution was the same as in Example 1-1.

[0105] Comparative Examples 2-2 to 2-4: Compared with Comparative Example 2-1, the core-shell bimetallic catalyst solution was changed to 5 mL, 15 mL, and 20 mL, and the rest was the same as Comparative Example 2-1.

[0106] The results of Comparative Examples 2-1 to 2-4 are shown in Table 8 below.

[0107] Table 8. Reaction effects in tank reactor

[0108]

[0109] Comparative Examples 3-1 to 3-3: Compared to Example 1-1, H₂PtCl₆ was replaced with NiCl, NaAuCl₄, and CoCl₂. The molar concentrations in the solutions remained unchanged; all other conditions were the same as in Example 1-1. The results are shown in Table 9 below.

[0110] Table 9. Effect of Ni, Au, and Co-based bimetallic catalysts on KH550 yield

[0111]

[0112] Finally, it should be noted that the above examples are merely specific embodiments of the present invention. Obviously, the present invention is not limited to the above examples and is subject to numerous variations. All variations that can be directly derived or conceived by a person of ordinary skill in the art from the disclosure of the present invention are considered to be within the scope of protection of the present invention.

Claims

1. A microchannel synthesis method for γ-aminopropyltriethoxysilane, characterized in that: γ-Aminopropyltriethoxysilane was synthesized in one step in a microchannel reactor using acrylonitrile, triethoxysilane and hydrogen as raw materials in the presence of a catalyst. Triethoxysilane, acrylonitrile, and hydrogen are pumped into the microchannel reactor at a mass flow rate ratio of 2-4:1:0.1-0.3; the reaction temperature of the microchannel reactor is 80-110° C., the reaction pressure is 1-3.5 MPa, and the reaction time is 40-110 min; The catalyst is a core-shell bimetallic catalyst, and the inner wall of the microchannel reactor is loaded with the core-shell bimetallic catalyst; The method for loading a core-shell bimetallic catalyst on the inner wall of a microchannel reactor comprises the following steps: A. Preparation of core-shell bimetallic catalysts: A 1-2M platinum salt solution and propylene carbonate are mixed in a volume ratio of 2-4:1, and the mixture is added to an autoclave. The air in the autoclave is replaced with hydrogen 2-3 times, and then the autoclave is filled with hydrogen to 3-5 MPa. The autoclave is heated to 40-60°C and kept warm for 3-5 hours to obtain a Pt nano-solution. The autoclave was opened, and a lithium salt solution having an equal volume to the platinum salt solution was added to the Pt nanoparticle solution, wherein the concentration of the lithium salt solution was 0.5 to 4 M. After replacing the air in the autoclave with hydrogen 2 to 3 times, the autoclave was filled with hydrogen to 3 to 5 MPa, and the autoclave was heated to 30 to 40° C. and kept warm for 3 to 5 hours to obtain a core-shell bimetallic catalyst solution. B. Injecting the core-shell bimetallic catalyst solution into the microchannel reactor in an amount equal to the liquid holdup of the microchannel reactor; maintaining the temperature at 60-90° C. for 7-10 hours under inert gas protection to remove moisture from the core-shell bimetallic catalyst solution, thereby obtaining a microchannel with an inner layer loaded with the core-shell bimetallic catalyst, wherein the core-shell bimetallic catalyst loading is 0.01-0.06 mg / cm 2 .

2. The microchannel synthesis method of γ-aminopropyltriethoxysilane according to claim 1, characterized in that: The microchannel synthesis device used includes a hydrogen bottle, a triethoxysilane raw material tank, and an acrylonitrile raw material tank respectively connected to the inlet of the microchannel reactor; The reaction product of the microchannel reactor is collected and subjected to post-processing to obtain gamma-aminopropyltriethoxysilane.

3. The microchannel synthesis method of γ-aminopropyltriethoxysilane according to claim 1 or 2, characterized in that: The platinum salt is any one of H2PtCl6, Pt(NO3)2, (NH4)2PtCl6, The lithium salt is any one of LiCl, LiNO3, Li2SO4, and Li2CO3.

4. The microchannel synthesis method of γ-aminopropyltriethoxysilane according to claim 3, characterized in that: The inner diameter of the microchannel reactor is 0.1 to 100 μm, and the liquid holding capacity is 300 to 600 μL.

Citation Information

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