Method for preparing epoxy chloropropane by using novel catalyst
A technology for epichlorohydrin and a catalyst is applied in the field of preparing epichlorohydrin by using a novel catalyst, which can solve the problems of low selectivity of allyl chloride, low yield of epichlorohydrin and the like, and achieve the effects of improving catalytic performance and eliminating acidity
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Embodiment 1
[0014] Dissolve 9.8 kg TPABr in water, then add it into silica sol and stir vigorously to obtain liquid A, take 0.95 kg tetrabutyl titanate and add 10 L isopropanol and stir to obtain liquid B, and add B dropwise into liquid A under vigorous stirring, Then stir vigorously for 1 h, evaporate the alcohol at 80 °C for 3 h, add ammonia water and stir, then transfer to the reaction kettle. Crystallized at 150 °C for 3 days, the obtained product was filtered and washed, dried at 110 °C, and calcined at 540 °C for 5 h to obtain solid powder TS. Take 9 kg of nitric acid (mass fraction=5%), 0.1 kg of solid powder TS, 0.05 kg of HAuCl 4 In a reactor, it was modified at 170 °C for 24 h, then washed by centrifugation, dried at 110 °C, and calcined at 500 °C for 10 h to obtain the Au-TS catalyst.
[0015] Take 2 kg of chloropropene, 0.05 kg of Au-TS catalyst, 0.5 kg of 30% hydrogen peroxide and 10 L of methanol in a 25 L reactor, react in a homogeneous reactor at 80 °C for 2 h, and then t...
Embodiment 2
[0017] Dissolve 9.8 kg TPABr in water, then add it into silica sol and stir vigorously to obtain liquid A, take 0.95 kg tetrabutyl titanate and add 10 L isopropanol and stir to obtain liquid B, and add B dropwise into liquid A under vigorous stirring, Then stir vigorously for 1 h, evaporate the alcohol at 80 °C for 3 h, add ammonia water and stir, then transfer to the reaction kettle. Crystallized at 150 °C for 3 days, the obtained product was filtered and washed, dried at 110 °C, and calcined at 540 °C for 5 h to obtain solid powder TS. Take 10 kg nitric acid (mass fraction=5%), 0.1 kg solid powder TS, 0.07 kgAgNO 3 In a reactor, it was modified at 160 °C for 40 h, then washed by centrifugation, dried at 110 °C, and calcined at 450 °C for 12 h to obtain the Ag-TS catalyst.
[0018] Take 1 kg of chloropropene, 0.05 kg of Ag-TS catalyst, 0.3 kg of 30% hydrogen peroxide and 10 L of methanol in a 25 L reactor, react in a homogeneous reactor at 80 °C for 2 h, and then take it out...
Embodiment 3
[0020] Dissolve 9.8 kg TPABr in water, then add it into silica sol and stir vigorously to obtain liquid A, take 0.95 kg tetrabutyl titanate and add 10 L of isopropanol and stir to obtain liquid B, and add B dropwise into liquid A under vigorous stirring, Then stir vigorously for 1 h, evaporate the alcohol at 80 °C for 3 h, add ammonia water and stir, then transfer to the reaction kettle. Crystallized at 150 °C for 3 days, the obtained product was filtered and washed, dried at 110 °C, and calcined at 540 °C for 5 h to obtain solid powder TS. Take 8.5 kg nitric acid (mass fraction=5%), 0.1 kg solid powder TS, 0.02 kg Ce(NO 3 ) 3 In a reactor, it was modified at 160 °C for 24 h, then washed by centrifugation, dried at 110 °C, and calcined at 550 °C for 10 h to obtain the Ce-TS catalyst.
[0021] Take 2 kg of chloropropene, 0.05 kg of Ce-TS catalyst, 0.7 kg of 30% hydrogen peroxide and 10 L of methanol in a 25 L reactor, react in a homogeneous reactor at 70 °C for 2 h, and then ...
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