Preparation method of hydrosilylation reaction catalyst
By using a water-soluble thickener and alkoxysilane hydrolysis reaction in the catalyst preparation, combined with the chloroplatinic acid coordination reaction, a heterogeneous catalyst with high catalytic activity and good stability was prepared, which solved the problem of insufficient catalyst stability and reactivity in the prior art, and long-term storage and multiple use of the catalyst are realized, production process is simplified and cost is reduced.
Patent Information
- Application Number
- CN202510022116.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-07
- Publication Date
- 2025-04-15
- Estimated Expiration
- 2045-01-07
AI Technical Summary
The heterogeneous hydrogen silization catalyst obtained in the prior art cannot take into account good storage stability and high-efficiency reactivity, and the catalyst preparation method is complicated and is not suitable for industrial production.
By mixing and dispersing the water-soluble thickener with a non-polar organic solvent, hydrolysis reaction of alkoxysilane is carried out to obtain a pore-like silica support, and then coordinated with chloroplatinic acid to prepare a heterogeneous catalyst with high catalytic activity and good stability.
The catalytic activity of the obtained catalyst remains basically unchanged after long-term storage at room temperature, the product will hardly turn yellow, and the catalyst can be used repeatedly, simplifying the production process and reducing production costs.
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Figure CN119819281A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of synthesis of organosilicon monomers and polymers, and more specifically, to a method for preparing a hydrosilylation reaction catalyst. Background Art
[0002] The hydrosilylation reaction is an addition reaction between unsaturated bond compounds (including double bonds, triple bonds, aldehydes, ketones, etc.) and organosilicon compounds containing silicon-hydrogen bonds catalyzed by precious metal catalysts (compounds such as platinum, rhodium, palladium, and iridium). This reaction can generate new silicon-carbon bonds and silicon-oxygen bonds, and is an important reaction for synthesizing organosilicon monomers and organosilicon polymers. The reaction has a high atomic utilization rate, but the catalyst is expensive and difficult to recycle, which increases production costs and exacerbates the consumption of precious metal resources.
[0003] At present, there are mainly the following methods for preparing heterogeneous hydrosilation catalysts: one is to obtain a silica-immobilized organic ligand by reacting a functional organic ligand with a specific structure with surface hydroxylated silica, and then reacting it with a platinum-containing compound; the other is to first treat silica powder or inorganic carriers such as silicon-containing molecular sieves with a coupling agent chloropropyl alkyl silane, and then use a functional group-containing compound such as vinyl pyridine or divinyl pyridine to modify the surface of such a carrier, and then coordinate and complex the modified carrier with chloroplatinic acid to obtain a supported platinum catalyst with a specific structural formula. However, the heterogeneous hydrosilation catalysts obtained in the prior art cannot take into account good storage stability and high-efficiency reactivity, and the preparation methods of the catalysts obtained by some methods are too complicated and not suitable for actual industrial production. Summary of the invention
[0004] In order to solve or at least partially solve the problems in the prior art, the present invention provides a method for preparing a hydrosilylation reaction catalyst. The catalyst obtained by the preparation method has good storage stability and high reactivity compared with traditional catalysts, and the product catalyzed by the catalyst does not produce yellowing (or the yellowing phenomenon is significantly reduced). The preparation method provided by the present invention is simple, and the catalytic activity of the catalyst obtained by the present invention remains basically unchanged or changes little after long-term storage at room temperature.
[0005] The present invention provides a method for preparing a hydrosilylation reaction catalyst, comprising the following steps:
[0006] 1) mixing and dispersing an aqueous solution of a water-soluble thickener and a non-polar organic solvent to obtain a suspension;
[0007] 2) adding an alkoxysilanol solution to the suspension obtained in step 1) to carry out a hydrolysis reaction, taking an organic phase after the reaction is completed, and removing water to obtain a mixture (i.e., a carrier);
[0008] 3) adding chloroplatinic acid alcohol solution to the mixture obtained in step 2) to carry out coordination reaction, taking the precipitate after the reaction is completed, and drying to obtain the product.
[0009] The preparation method provided by the present invention uses a water-soluble thickener as an additive in a specific manner provided by the present invention to synthesize a porous silica carrier through a hydrolysis reaction of alkoxysilane, and then uses the silica carrier as a carrier to immobilize platinum to prepare a catalyst that is a heterogeneous catalyst and can be used in a hydrosilylation reaction. The heterogeneous catalyst prepared by the present invention has high catalytic activity, and the product obtained by catalysis does not turn yellow and can be used repeatedly.
[0010] In a preferred embodiment of the present invention, in step 1), the water-soluble thickener is carboxymethyl cellulose, polyvinyl alcohol, sodium polyacrylate or polyacrylamide. The water-soluble thickener has different dissolution and dispersion in water. Carboxymethyl cellulose will form a spherical colloid in an aqueous solution, and water-soluble thickeners such as polyvinyl alcohol, sodium polyacrylate, polyacrylamide, etc. will form a hydrogel when dissolved in water. By selecting different types of thickeners, carriers of different structures can be obtained. Although the structures of the carriers obtained using different water-soluble thickeners are different, the purpose of the present invention can be achieved. In a preferred embodiment of the present invention, in order to further improve the stability and reactivity of the obtained carrier, the water-soluble thickener is preferably carboxymethyl cellulose. The present invention unexpectedly found that when carboxymethyl cellulose is used as a water-soluble thickener, the main structure of the catalyst obtained is a hollow spherical capsule, and the catalytic activity of the catalyst obtained is also higher.
[0011] In a preferred embodiment of the present invention, the concentration of the aqueous solution of the water-soluble thickener can be 9*10 -5 %~2*10 -3 %. In the scheme of the present invention, if the concentration of the water-soluble thickener aqueous solution is too high, the silane is not easily dispersed in the system and is easily polymerized and agglomerated after hydrolysis; and if the concentration of the thickener aqueous solution is too low, the catalytic effect of the obtained catalyst becomes poor.
[0012] In a preferred embodiment of the present invention, in step 1), the non-polar organic solvent is an organic solvent that can form an azeotrope with water, which can be one or more of cyclohexane, n-octane, isooctane, and toluene, and is more preferably cyclohexane. Wherein, the amount of the non-polar organic solvent is 10 to 50% of the volume of the water-soluble thickener solution in step 1). In the scheme of the present invention, the boiling point of the azeotrope formed by the non-polar solvent and water has an effect on the catalytic activity of the synthesized catalyst. If the azeotropic temperature is too high, the hydrolysis aging temperature is high, the siloxane condenses rapidly, and the catalytic activity of the obtained catalyst is reduced. If the azeotropic temperature is too low, the aging condensation is not thorough, and the catalytic activity of the obtained catalyst is not high.
[0013] In a preferred embodiment of the present invention, in step 2), the alkoxysilane in the alkoxysilanol solution is one or more of vinyltrimethoxysilane, vinyltriethoxysilane, methyltrimethoxysilane, methyltriethoxysilane, propyltrimethoxysilane, propyltriethoxysilane, tetramethoxysilane, tetraethoxysilane, trimethoxysilane of a long-chain alkyl group, triethoxysilane of a long-chain alkyl group (wherein the number of carbon atoms in the long-chain alkyl group is 6 to 18); preferably, vinyltrimethoxysilane is mixed with one or more of vinyltriethoxysilane, methyltrimethoxysilane, methyltriethoxysilane, propyltrimethoxysilane, propyltriethoxysilane, tetramethoxysilane, tetraethoxysilane, trimethoxysilane of a long-chain alkyl group, triethoxysilane of a long-chain alkyl group (wherein the number of carbon atoms in the long-chain alkyl group is 6 to 18). In order to further improve the stability and reaction activity of the obtained catalyst, the alkoxysilane is preferably a mixture of vinyltrimethoxysilane and tetramethoxysilane, and more preferably, in the mixture, the mass ratio of vinyltrimethoxysilane to tetramethoxysilane is (1-10):1, and more preferably (2-5):1. The present invention has found through a large number of parallel experiments that too large or too small a ratio will weaken the catalytic activity of the obtained catalyst, and the stability of the catalyst and the activity after multiple cycles will also deteriorate.
[0014] In a specific embodiment of the present invention, in step 2), the alcohol in the alkoxysilanol solution may be methanol, ethanol, isopropanol, ethylene glycol, etc. The proportion of alkoxysilane in the alkoxysilanol solution is 10-50%.
[0015] In a preferred embodiment of the present invention, in step 2), the amount of the aqueous solution of the thickener is 2 to 5.5 times the mass of the alkoxysilanol solution. In a preferred embodiment of the present invention, in step 2), the temperature of the hydrolysis reaction is 40 to 45°C and the time is 1.5 to 2 hours.
[0016] In a preferred embodiment of the present invention, in order to avoid damaging the structure of the carrier in the catalyst and further protect the performance of the catalyst, the water removal step in step 2) is performed by solvent reflux.
[0017] In a preferred embodiment of the present invention, in step 3), the amount of chloroplatinic acid in the chloroplatinic acid alcohol solution is 0.01% to 0.2% of the mass of the carrier (i.e., the mixture obtained in step 2). The alcohol in the chloroplatinic acid alcohol solution is usually isopropanol.
[0018] In a specific embodiment of the present invention, in step 3), drying may be a drying method commonly used in the art, such as vacuum drying.
[0019] Another object of the present invention is to provide a hydrosilylation reaction catalyst obtained by the above preparation method.
[0020] The catalyst obtained by the present invention is respectively applied to the synthesis reaction of a long-chain alkyl coupling agent and the synthesis reaction of a polyether-modified silane coupling agent, and the temperature rise phenomenon of the homogeneous catalytic reaction will not occur, and the reaction process is stable. The catalyst can be removed by filtering to achieve recovery, and the recovered catalyst can be repeatedly circulated. The obtained finished product will hardly have yellowing phenomenon, greatly reducing the influence of the catalyst residue on the product quality, and simplifying the production process.
[0021] Another object of the present invention is to provide the use of the above preparation method or the hydrosilylation reaction catalyst obtained by the above preparation method in catalyzing the addition reaction of hydrosilane and olefin.
[0022] Among them, hydrogen-containing silanes may include but are not limited to trimethoxysilane, triethoxysilane, trichlorosilane, methyldichlorosilane, dimethoxymethylsilane, diethoxymethylsilane, etc., and olefins may include but are not limited to 1-hexadecene, allyl polyether, 1-hexene, 1-octene, 1-decene, 1-dodecene, 1-octadecene, allyl glycidyl ether, 4-vinyl epoxycyclohexane, etc. In the specific embodiment of the present invention, the catalytic activity of the catalyst of the present invention is verified by the addition reaction of 1-hexadecene with trimethoxysilane and the addition reaction of allyl polyethylene glycol monomethyl ether (described in detail with Zhejiang Royal Madrid HMS-274M as an example) with trimethoxysilane, but it does not mean that the catalyst provided by the present invention has relatively good activity only in these two catalytic reactions. The present invention has confirmed through a large number of experiments that the obtained catalyst has relatively good activity in the addition reaction of the above-mentioned hydrogen-containing silane with olefins.
[0023] Compared with the prior art, the present invention has the following beneficial effects:
[0024] (1) The present invention uses a common thickener as an additive, self-assembles alkoxysilane in an aqueous solution of the thickener, and adjusts the ratio of different types of alkoxysilanes for structural modification to obtain heterogeneous catalysts of different structural strengths, different appearances, and types of loading / embedded. This method can adjust the structure and size of the carrier and has a wide range of applications.
[0025] (2) The thickener aqueous solution prepared in the process of the present invention can be recycled by distilling off the alcohol after the reaction, thereby reducing the generation of wastewater. In the synthesis process, the organic solvent plays a role in emulsifying with the thickener aqueous solution to form a template during the hydrolysis process and can also be used as an azeotropic solvent for removing water. In addition, the organic solvent can be recycled in the preparation method without generating waste solvent.
[0026] (3) The catalyst synthesized by the method provided by the present invention is a heterogeneous catalyst, the carrier is a silica carrier, has an extremely high specific surface area and a high loading rate for precious metals, and has a built-in steric structure that can improve the selectivity of the hydrosilylation reaction.
[0027] (4) The heterogeneous catalyst prepared by the present invention can be used to catalyze the synthesis of long-chain alkyl coupling agents and polyether-modified silane coupling agents, which can significantly reduce the platinum residue and the yellowing phenomenon of the polyether adduct, simplify the production process, and reduce the production cost. At the same time, the stability of the catalyst prepared by the present invention is higher than that of the Speier and Karstedt catalysts, which are prone to precipitate platinum black when left for a long time at room temperature. The catalyst provided by the present invention does not deactivate during long-term storage at room temperature, that is, the color does not change during long-term storage at room temperature, and the catalytic reaction activity remains high. At the same time, the catalyst provided by the present invention can be used repeatedly (at least 2 times, preferably at least 3 times, and more preferably at least 4 times) without a significant decrease in catalytic activity. BRIEF DESCRIPTION OF THE DRAWINGS
[0028] Figure 1 This is an electron microscope photograph of the silicon-oxygen addition reaction catalyst obtained in Example 1.
[0029] Figure 2 This is an electron microscope photograph of the silicon-oxygen addition reaction catalyst obtained in Example 2.
[0030] Figure 3 This is an electron microscope photograph of the silicon-oxygen addition reaction catalyst obtained in Example 3. DETAILED DESCRIPTION
[0031] The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention.
[0032] Example 1
[0033] (1) Dissolve 0.1 g of carboxymethyl cellulose in 1000 g of deionized water, heat and stir to disperse evenly until no obvious particles are present, then cool to room temperature, filter to obtain a thickener solution, and add 200 ml of cyclohexane to the solution for thorough stirring and dispersion to obtain a suspension. Mix 100 g of a mixture of vinyltrimethoxysilane and tetramethoxysilane in a mass ratio of 3:1 with 100 g of methanol to obtain a uniform alkoxysilanol solution, which is placed in a dropping funnel. Turn on the heating to raise the temperature of the suspension to 40°C, then drop the alkoxysilanol solution, and continue stirring at 40°C for 2 h after the addition is completed to obtain a suspension. Let stand for several hours to cool and separate the liquids. Take the lower aqueous solution, filter the lower aqueous solution to separate the filter cake, and wash the filter cake with a small amount of deionized water. Mix the obtained filter cake with the upper cyclohexane obtained by separation and stir evenly, heat, and azeotropize cyclohexane with water until there are no water droplets condensing in the cyclohexane refluxed in the water separator to obtain a carrier.
[0034] (2) Add chloroplatinic acid isopropanol solution to the carrier obtained in step (1) (the preparation method of chloroplatinic acid isopropanol solution is to dissolve 1 g of chloroplatinic acid hexahydrate in 18 ml of isopropanol, wherein the amount of chloroplatinic acid isopropanol solution used in this step is such that chloroplatinic acid accounts for 0.2% of the weight of the carrier), heat to 100° C. and stir for 2 h, then filter and separate the precipitate, and vacuum dry at -0.1 MPa and 40° C. for 6 h to obtain a heterogeneous catalyst (i.e., the hydrosilylation reaction catalyst obtained in this example).
[0035] The electron microscope photo of the heterogeneous catalyst obtained in this example is as follows Figure 1 As shown, the size of the spherical structure is approximately distributed between 3-7 μm, which is larger than the pore size of the organic filter membrane (2.5 μm), and contains a large number of broken flake structures. The microsphere structure and broken flakes can prove that the obtained catalyst is a hollow structure, which also proves that the method provided in this embodiment can prepare a hollow structure supported catalyst.
[0036] Example 2
[0037] (1) Dissolve 0.1g of sodium polyacrylate in 1000g of deionized water, heat and stir to disperse evenly until there are no obvious particles, then cool to room temperature, filter to obtain a thickener solution, and add 200ml of toluene to fully stir and disperse to obtain a suspension. Mix 100g of a mixture of vinyltrimethoxysilane and tetramethoxysilane in a mass ratio of 2:1 with 300g of methanol to obtain a uniform alkoxysilanol solution, which is placed in a dropping funnel. Turn on the heating to raise the suspension to 40°C, then add the alkoxysilanol solution dropwise. After the addition is completed, stir at 40°C for 2h to obtain a suspension. Let stand for several hours to cool and separate the liquids. The lower aqueous solution is filtered to separate the filter cake and washed with a small amount of deionized water, then the filter cake is taken out, mixed with the upper toluene, stirred into a slurry, and transferred into a flask, and the temperature is raised to toluene reflux, and toluene and water form an azeotrope, and the water brought out by the azeotrope is separated through a water separator, until there are no water droplets condensed in the toluene refluxed in the water separator, and the carrier is obtained.
[0038] (2) Adding a chloroplatinic acid isopropanol solution to the carrier obtained in step (1) (the preparation method of the chloroplatinic acid isopropanol solution is to dissolve 1 g of chloroplatinic acid hexahydrate in 18 ml of isopropanol, wherein the amount of the chloroplatinic acid isopropanol solution in this step is such that chloroplatinic acid accounts for 0.1% of the weight of the carrier), heating to 100° C. and stirring for 2 h, then filtering and separating the precipitate, and vacuum drying at -0.1 MPa and 40° C. to obtain a heterogeneous catalyst (i.e., the hydrosilylation reaction catalyst of the present invention).
[0039] The electron microscope photo of the heterogeneous catalyst obtained in this example is as follows Figure 2 As shown, most of them are loose flakes, and no spherical structures are observed.
[0040] Example 3
[0041] (1) Dissolve 2g of polyvinyl alcohol in 1000g of deionized water, heat and stir to disperse evenly, then cool to room temperature, filter to obtain a thickener solution, and add 200ml of n-hexane to it for sufficient stirring and dispersion to obtain a suspension. Mix 100g of a mixture of vinyltrimethoxysilane and tetramethoxysilane in a mass ratio of 2:1 with 150g of methanol to obtain an alkoxysilanol solution, which is placed in a dropping funnel. Turn on the heating to heat the solution to 40°C and then add it dropwise. After the addition is completed, stir at 40°C for 2h to obtain a suspension. Let it stand for several hours to cool down and separate the liquids. Filter the lower aqueous solution to separate the filter cake and wash it with a small amount of deionized water. Take out the filter cake, mix it with the upper n-hexane, stir it into a slurry, transfer it to a flask, heat it to reflux n-hexane, and separate the water brought out by the azeotrope through a water separator through the n-hexane and water. No water droplets condense in the n-hexane refluxed in the water separator to obtain a carrier.
[0042] (2) adding a chloroplatinic acid isopropanol solution to the carrier obtained in step (1) (the preparation method of the chloroplatinic acid isopropanol solution is to dissolve 1 g of chloroplatinic acid hexahydrate in 18 ml of isopropanol, wherein the amount of the chloroplatinic acid isopropanol solution in this step is such that chloroplatinic acid accounts for 0.05% of the weight of the carrier), heating to 100° C. and stirring for 2 h, then filtering and separating the precipitate, and vacuum drying at -0.1 MPa and 40° C. to obtain a heterogeneous catalyst (i.e., the hydrosilylation reaction catalyst of the present invention).
[0043] The electron microscope photo of the heterogeneous catalyst obtained in this example is as follows Figure 3 As shown, the structure of the obtained catalyst is irregular agglomerates, in which there are no obvious spherical and lamellar structures.
[0044] Example
[0045] The catalysts prepared in Examples 1-3 were used to catalyze the hydrosilylation reaction of 1-hexadecene, allyl polyether and trimethoxysilane, respectively, and the reaction effects of the homogeneous Speier catalyst and the Karstedt catalyst were compared.
[0046] 1. The catalyst obtained in Example 1-3 catalyzes the addition of 1-hexadecene and trimethoxysilane:
[0047] 0.1 mol 1-hexadecene was mixed with 10 ppm (in terms of Pt) of catalyst (Example 1-3, Speier catalyst, Karstedt catalyst), activated at 80°C for 30 min under nitrogen protection, and then 0.11 mol trimethoxysilane was added dropwise. After the addition was completed within 30 min, the temperature was raised to 100°C and kept for 3 h to terminate the reaction. After cooling, the crude product was filtered to obtain a weighed product and the content of hexadecyltrimethoxysilane was determined by gas chromatography. At the same time, the catalyst was filtered and washed with a small amount of methanol and dried at 60°C for standby use. Among them, the hydrosilylation rate = hexadecyltrimethoxysilane content in the crude product / (1-residual 1-hexadecene content in the spectrum)*100%. The results are shown in Table 1.
[0048] Table 1
[0049]
[0050] The crude product obtained by filtering and separating after the catalytic reaction using the catalyst of Examples 1-3 is colorless. At the same time, it can be seen from Table 1 that the catalytic effect of the catalyst obtained by the present invention in the first reaction is similar to that of the homogeneous Karstedt catalyst (the catalytic effect of the embodiment is slightly better). At the same time, the catalyst obtained by the present invention is circulated for 3 times again, and the addition rate does not decrease significantly, which proves that the catalyst has high stability and does not show a significant decrease in activity after three cycles of reaction and separation and washing. The homogeneous catalysts Speier and Karstedt catalysts cannot be separated and circulated from the reaction system and can only react once. The crude products of the two catalysts are golden yellow, and the catalytic effect of the Speier catalyst is poor.
[0051] 2. The catalyst obtained in the example catalyzes the addition of allyl polyether and trimethoxysilane:
[0052] 39g of allyl polyethylene glycol monomethyl ether (0.1mol) (Zhejiang Royal Madrid HMS-274M) was mixed with 10ppm (in terms of Pt) catalyst (Example 1-3, Speier catalyst, Karstedt catalyst), and 13.42g of trimethoxysilane (0.11mol) was added dropwise after activation at 80°C for 30min under nitrogen protection. After the addition was completed, the temperature was raised to 110°C until there was no obvious reflux in the system, and the catalyst was filtered out by cooling to obtain a crude product. The product was removed by vacuum distillation at 80°C and -0.04 to -0.03MPa to obtain a product, which was weighed and the hydrosilylation rate was calculated, wherein the hydrosilylation rate = actual weight of the product / theoretical weight of the product * 100%, wherein the theoretical weight was calculated by the mass sum of 0.1mol of allyl polyether and 0.11mol of trimethoxysilane. At the same time, after the reaction was completed, the catalyst was filtered and washed with a small amount of methanol and dried at 60°C for standby use.
[0053] The results are shown in Table 2.
[0054] Table 2
[0055]
[0056] The catalyst prepared in the embodiment of the present invention is almost colorless after catalyzing the addition reaction of allyl polyether and trimethoxysilane by filtering, and the addition product of allyl polyether and trimethoxysilane is heated at 150°C after vacuum distillation, and no yellowing phenomenon occurs. As can be seen from Table 2, in the first reaction, the catalytic effect of the catalyst provided by the present invention is similar to that of the homogeneous catalyst in the prior art, and is even slightly better than the homogeneous catalyst, and the addition rate is not significantly reduced when the catalyst of the present invention is cycled three times. The crude product after the reaction of the homogeneous catalyst Speier and Karstedt is golden yellow, and the viscosity increases after the low boiling point is removed by vacuum distillation. After adsorption and decolorization by adding 0.5% mass fraction of 600 mesh activated carbon, the color is still golden yellow and cannot be removed, proving that the platinum residue in the system is too high. The catalyst obtained by the present invention also has a strong advantage in this catalytic reaction.
[0057] Finally, the method of the present invention is only a preferred embodiment and is not intended to limit the protection scope of the present invention. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims
1. A method for preparing a hydrosilylation reaction catalyst, characterized in that: The steps include: 1) mixing and dispersing an aqueous solution of a water-soluble thickener and a non-polar organic solvent to obtain a suspension; 2) adding an alkoxysilanol solution to the suspension obtained in step 1) to carry out a hydrolysis reaction, taking an organic phase after the reaction is completed, and removing water to obtain a mixture; 3) adding chloroplatinic acid alcohol solution to the mixture obtained in step 2) to carry out coordination reaction, taking the precipitate after the reaction is completed, and drying to obtain the product.
2. The preparation method according to claim 1, characterized in that: In step 1), the water-soluble thickener is carboxymethyl cellulose, polyvinyl alcohol, sodium polyacrylate or polyacrylamide, preferably carboxymethyl cellulose.
3. The preparation method according to claim 1, characterized in that: In step 1), the non-polar organic solvent is an organic solvent that can form an azeotrope with water, preferably one or more of n-hexane, cyclohexane, n-octane, isooctane and toluene.
4. The preparation method according to claim 1, characterized in that: In step 2), the alkoxysilane in the alkoxysilanol solution is one or more of vinyltrimethoxysilane, vinyltriethoxysilane, methyltrimethoxysilane, methyltriethoxysilane, propyltrimethoxysilane, propyltriethoxysilane, tetramethoxysilane, tetraethoxysilane, trimethoxysilane with a long-chain alkyl group, and triethoxysilane with a long-chain alkyl group, wherein the number of carbon atoms in the long-chain alkyl group is 6 to 18; preferably, vinyltrimethoxysilane is mixed with one or more of vinyltriethoxysilane, methyltrimethoxysilane, methyltriethoxysilane, propyltrimethoxysilane, propyltriethoxysilane, tetramethoxysilane, and tetraethoxysilane.
5. The preparation method according to claim 4, characterized in that: In step 2), the alkoxysilane in the alkoxysilanol solution is a mixture of vinyltrimethoxysilane and tetramethoxysilane; preferably, the mass ratio of the vinyltrimethoxysilane to the tetramethoxysilane is (1-10):
1.
6. The preparation method according to claim 1, characterized in that: In step 2), the amount of the aqueous solution of the thickener used is 2 to 5.5 times the mass of the alkoxysilanol solution.
7. The preparation method according to claim 1, characterized in that: In step 2), the temperature of the hydrolysis reaction is 40-45° C. and the time is 1.5-2 h.
8. The preparation method according to any one of claims 1 to 7, characterized in that In step 3), the amount of chloroplatinic acid in the chloroplatinic acid alcohol solution is 0.01% to 0.2% of the amount of the mixture obtained in step 2).
9. The hydrosilylation reaction catalyst obtained by the preparation method according to any one of claims 1 to 8.
10. Use of the preparation method according to any one of claims 1 to 8 or the hydrosilylation reaction catalyst according to claim 9 in catalyzing the addition reaction of hydrosilane and olefin.
Citation Information
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