Method for preparing epoxy chloropropane
A technology of epichlorohydrin and chloropropene, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, organic chemistry, etc., can solve the problem of low selectivity of hydrogen peroxide epoxidation, peroxidation Low hydrogen conversion rate and other problems, to achieve the effect of improving hydrogen peroxide conversion rate and good hydrophobicity
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Embodiment 1
[0011] Silica sol (40% by weight), bis(triethoxysilyl)methane, TiCl 4 , tetrapropylammonium hydroxide, ammoniacal liquor and water are mixed uniformly according to the stoichiometric ratio, wherein the molar ratio of each component of the raw material is inorganic silicon source: organic silicon source: titanium source: organic templating agent: basic compound: water=1: 0.01 :0.01:0.03:0.4:20. Crystallize at 160° C. for 1 day, and the product is filtered, washed with water, and dried to obtain MFI titanium-silicon molecular sieves containing skeleton organic groups.
[0012] In a 250 ml three-necked flask, add 0.2 g of the above synthesized organic silicon titanium silicon molecular sieve catalyst, 20 g of methanol solvent, and 5 g of chloropropene, heat up to 50 ° C, and then add 3 g of 30% H 2 o 2 The solution was reacted under stirring conditions for 1 hour, and after the reaction was completed, the three-neck flask was cooled to 7° C. with ice water. Finally, the molecu...
Embodiment 2
[0014] Solid silica (2000 mesh), bis(triethoxysilyl)methane, TiCl 3 , tetrapropylammonium bromide, ethylamine and water are mixed uniformly by stoichiometric ratio, wherein the molar ratio of each component of the raw material is inorganic silicon source: organic silicon source: titanium source: organic templating agent: basic compound: water=1: 0.05:0.03:0.15:2.0:100. It was crystallized at 170°C for 5 days, and the product was filtered, washed with water and dried to obtain MFI titanium silicon molecular sieves containing skeleton organic groups.
[0015] In a 250 ml three-necked flask, add 0.1 g of the above-mentioned synthesized catalyst containing organosilicon-titanium-silicon molecular sieve, 10 g of 3-chloropropene, raise the temperature to 40° C., and then add 3 g of H with a mass fraction of 30%. 2 o 2 The solution was reacted for 2 hours under stirring conditions, and after the reaction was completed, the three-neck flask was cooled to 7° C. with ice water. Final...
Embodiment 3
[0017] Ethyl orthosilicate, bis(triethoxysilyl)methane, TiOCl 2 , Tetrabutylammonium hydroxide, n-propylamine and water are mixed uniformly in a stoichiometric ratio, wherein the molar ratio of each component of the raw material is inorganic silicon source: organic silicon source: titanium source: organic templating agent: basic compound: water=1: 0.03: 0.02:0.09:1.2:60. Crystallize at 180°C for 10 days, and the product is filtered, washed with water, and dried to obtain an MFI titanium-silicon molecular sieve containing a skeleton organic group.
[0018] Add 0.4 g of the organosilicon-titanium-silicon molecular sieve catalyst synthesized above, 40 g of ethanol solvent, and 20 g of 2-methyl-3-chloropropene into a 250 ml three-necked flask, heat up to 60° C., and then add 3 g of a mass fraction of 30 %H 2 o 2 The solution was reacted under stirring conditions for 3 hours, and after the reaction was completed, the three-neck flask was cooled to 7° C. with ice water. Finally,...
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