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Method for preparing gama-(2,3-epoxypropoxy) propyl trimethylsilicane combination catalyst
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A technology of propyltrimethoxysilane and combined catalyst, which is applied in the field of catalyst preparation, can solve the problems of insufficient catalyst activity, large amount of catalyst, long reaction time and the like, and achieves the advantages of convenient industrial production, short reaction time and high product quality. Effect
Active Publication Date: 2010-07-21
湖北武大有机硅新材料股份有限公司
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Related literature reports, using different catalysts, such as H 2 PtCl 6 / THF, H 2 PtCl 6 / Isopropanol, H 2 PtCl 6 / acetone, H 2 PtCl 6 / Acetylacetone, Rh(PPh 3 ) 3 , Rh loaded catalyst on carbon, etc., the product yield is 60-90%, but the amount of catalyst is relatively large, and its molar action number is between 10,000 and 85,000, and the activity of the catalyst is not enough; and the reaction time is long and the operation is complicated
It has been reported in China that HSiCl 3 After alcoholysis with anhydrous methanol at a molar ratio of 1.05:1 to obtain trimethoxysilane, trimethoxysilane and glycidyl ether are added at a molar ratio of 1:1 to H 2 PtCl 6 As a catalyst, the synthesis reaction is carried out at 160-180°C, but the yield is only 72.91%
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[0014] A. Preparation of combined catalyst: add H with a mass percentage ratio of: 1.5~3:20~30:60~80:3~5:1.5~3:2~3 2 PtCl 6 ·6H 2 O, isopropanol, acid-binding agent (ether, such as ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, ethylene glycol dimethyl ether, ethylene glycol diethyl ether, 1,2 - Epoxyhexane, 1,2-epoxyoctane, 1,4-dioxane, butyl ether, anisole, phenetole, ethylene glycol phenyl ether, diethylene glycol dimethyl ether, diethyl ether Glycol butyl ether, one of terephthalate, methyl tert-butyl ether, diethylene glycol butyl ether, allyl glycidyl ether), reducing agent (such as vitamin C, glucose, butyraldehyde, valeraldehyde , glyoxal, malondialdehyde, glutaraldehyde, salicylaldehyde, benzaldehyde, p-hydroxybenzaldehyde, p-tolualdehyde, o-tolualdehyde, o-methoxybenzaldehyde, p-methoxybenzaldehyde , o-carboxybenzaldehyde, o-chlorobenzaldehyde, p-chlorobenzaldehyde, m-chlorobenzaldehyde, p-tert-butylbenzaldehyde...
Embodiment 1
[0017] Embodiment 1: the preparation of combined catalyst: in 20ml round flask with magnetic son, add 0.2gH 2 PtCl 6 ·6H 2 O, 2.8g (3.5ml) isopropanol, 7g (7ml) anisole, after the magnetic stirrer stirs evenly, adopt combination technology to add 0.4g vitamin C, 0.2g anhydrous sodium sulfate and 0.3g maleic acid, 60 Stir at ℃ for 1h, cool and filter.
Embodiment 2
[0018] Embodiment 2: the preparation of combined catalyst: in 20ml round flask with magnetic son, add 0.2gH 2 PtCl 6 ·6H 2 O, 2.5g (3.1ml) isopropanol, 7g (7ml) 1,4-dioxane, after stirring evenly with a magnetic stirrer, add 0.4ml valeraldehyde, 0.2g anhydrous magnesium sulfate and 0.28g For p-hydroxybenzoic acid, stir at 55°C for 1h, cool, and filter.
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Abstract
The invention discloses a preparation process for gamma-(2,3-glycidoxypropyl) trimethoxysilane combined catalyzer. H2PtCl6.6H2O / isopropanol is taken as the raw material, the acid-binding agent, the reducing agent, the water absorbent and the promoter are added into the H2PtCl6.6H2O / isopropanol to synthesize into the combined catalyzer. the combined catalyzer, the glycidyl ether and the trimethoxysilane are taken as the raw materials, the methanol anhydrous is taken as the solvent, the synthesis reaction is made at certain temperature after being heated and stirred; after the solvent methanol is vaporized under normal pressure, the pressure reduction distillation is made, the front cut fraction is obtained between 70 and 90 DEG C, the colorless transparent liquid (namely product) is obtained between 100 and 130 DEG C. The mole number of the combined catalyzer of the invention is between 150,000 and 220,000, which greatly exceeds 20,000 to 50,000 of feasible number of catalyzer process. The catalyzer is underdosed and only uses 8g to 11g of H2PtCl6.6H2Os for each ton product; the yields are high, the mole yields are high up to 91 to 93 percent; the content of the product is high up to 99 percent. No waste liquid, waste water and waste slags are produced in the whole process, hence typical green chemical synthesis.
Description
technical field [0001] The invention relates to a preparation method of a catalyst, more specifically to a preparation method of a γ-(2,3-glycidoxy)propyltrimethoxysilane combined catalyst, which is applied to the synthesis of fine chemical products by hydrosilylation reaction. Background technique [0002] γ-(2,3-Glycidoxypropoxy)propyltrimethoxysilane is a widely used silane coupling agent, mainly used in plastics, coatings and adhesives to improve the mechanical strength of composite materials and improve integrated circuit materials And the electrical insulation performance of printed circuit boards in wet state. Greatly improves adhesion in acrylic latex, polyurethane and two-component epoxy resins. [0003] This product is mainly produced by the United States Witco (Witco) company abroad. Related literature reports, using different catalysts, such as H 2 PtCl 6 / THF, H 2 PtCl 6 / Isopropanol, H 2 PtCl 6 / acetone, H 2 PtCl 6 / Acetylacetone, Rh(PPh 3 ) 3 , ...
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Application Information
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