Preparation method of catalyst and application of catalyst in preparation of β-isophorone
A technology of isophorone and catalyst, applied in the field of catalyst, can solve the problems of equipment corrosion by strong basic catalyst, low purity of β-isophorone, complicated post-treatment process, etc., so as to reduce the generation of heavy components , the effect of improving the reaction selectivity and the simple preparation method
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Embodiment 1
[0040] 10g glycine, 100g β-cyclodextrin, 30g DCC, 400mL dichloroethane were added to the 1L reaction flask in turn, stirred at 50°C for 7h, the reaction solution was directly filtered, the filter cake was rinsed with ethanol, and a vacuum drying oven (60°C, 2KPa ) drying to obtain 108 g of glycine-modified esterified β-cyclodextrin. The obtained esterified modified cyclodextrin was transferred to a three-necked flask, 108 g of benzaldehyde and 400 mL of ethanol were added in sequence, stirred at 60 °C for 2 h, the reaction solution was directly filtered, and dried in a vacuum drying oven (60 °C, 2KPa) to obtain 119 g Glycine-based Schiff base-modified β-cyclodextrin, denoted as catalyst A.
[0041] Add α-isophorone containing 0.01 wt% catalyst A to the column kettle of a plate column reactor with 10 plates, and carry out refining at 150 ° C, absolute pressure of 0.01 MPa, and reflux ratio of 1:1. Distillation reaction, isomerization reaction occurs.
Embodiment 2
[0043] Add 10g alanine, 200g β-cyclodextrin, 10g DIC, 400mL dichloroethane to the 1L reaction flask in turn, stir at 20°C for 10h, the reaction solution is directly filtered, the filter cake is rinsed with ethanol, and the vacuum drying oven (60°C) , 2KPa) drying to obtain 208g of alanine-modified esterified β-cyclodextrin. The obtained esterified modified cyclodextrin was transferred to a three-necked flask, 416 g of benzaldehyde and 400 mL of ethanol were added in sequence, stirred at 20 °C for 10 h, the reaction solution was directly filtered, and dried in a vacuum drying oven (60 °C, 2KPa) to obtain 217.9 g Alanine-based Schiff base-modified β-cyclodextrin, denoted as catalyst B.
[0044] Add α-isophorone containing 0.1 wt% catalyst B to the column kettle of the plate column reactor with 25 plates, and carry out refining at 180 ° C, absolute pressure of 0.05 MPa, and reflux ratio of 30:1. Distillation reaction, isomerization reaction occurs.
Embodiment 3
[0046]10g serine, 10g β-cyclodextrin, 50g EDCI, 400mL dichloroethane were added to the 1L reaction flask in turn, stirred at 70°C for 5h, the reaction solution was directly filtered, the filter cake was rinsed with ethanol, and a vacuum drying oven (60°C, 2KPa ) and drying to obtain 19.5 g of serine-modified esterified β-cyclodextrin. Transfer the obtained esterified modified cyclodextrin into a three-necked flask, add 195 g of benzaldehyde and 400 mL of ethanol in turn, stir at 70 °C for 0.5 h, filter the reaction solution directly, and dry in a vacuum drying oven (60 °C, 2KPa) to obtain 27.8 g of serine-based Schiff base-modified beta-cyclodextrin, designated as catalyst C.
[0047] Add α-isophorone containing 0.5wt% catalyst C to the column reactor of the plate column reactor with 30 plates, and carry out refining under the conditions of 220 ° C, absolute pressure of 0.1 MPa, and reflux ratio of 3:1. Distillation reaction, isomerization reaction occurs.
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