A method for preparing 3,5,5-trimethyl-3-cyclohexen-1-one
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A cyclohexene and trimethyl technology, which is applied in the field of preparation of 3,5,5-trimethyl-3-cyclohexene-1-one, can solve the problem of excessive catalyst dosage, low space-time yield, Strong corrosion of equipment, etc., to achieve high isomeric selectivity, reduce the generation of by-products, and reduce the effects of three wastes
Active Publication Date: 2020-07-28
WANHUA CHEM GRP CO LTD
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The process uses pre-nitrogen phosphatine as a catalyst, which has the advantages of less catalyst consumption, high yield, green environmental protection, and easy realization of industrial production, and solves the problems of low space-time yield and excessive catalyst consumption in the prior art. , many by-products, strong corrosion of equipment and other problems
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Embodiment 1
[0051] Add the α-IP raw material containing 0.05wt% pre-nitrogen phosphatrane catalyst IL-A to the tower reactor of the tower reactor, and the temperature of the tower reactor is 210 ° C, the number of theoretical plates is 30, and the reflux ratio is 3:1. Reactive distillation was carried out under the condition of 0.9 Bar absolute pressure in the reactor, α-IP isomerization reaction occurred, the reaction selectivity was 99.7%, and the crude product β-IP was collected at the top of the tower (the gas phase purity was 70wt%). The crude product β-IP is 1.5kPa in absolute pressure, the number of theoretical plates is 30, and the reflux ratio is 3:1, further vacuum distillation to obtain the product β-IP with a purity of 99.5wt%, and the temperature at the top of the column is 100 ℃.
Embodiment 2-10 and Embodiment 11
[0052] Embodiment 2-10 and embodiment 11 (comparative example)
[0053] On the basis of Example 1, change the catalyst type and consumption, the number of theoretical plates of the reactive distillation column reactor, the temperature of the tower bottom, pressure, reflux ratio, residence time, the results are shown in Table 1.
[0054] Table 1
[0055]
[0056]
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Abstract
A kind of preparation method of 3,5,5-trimethyl-3-cyclohexene-1-ketone: with 3,5,5-trimethyl-2-cyclohexene-1-ketone (α-IP) As a raw material, the former nitrogen phosphatrane base is used as a catalyst, and reactive distillation technology is used to carry out isomerization reaction to prepare 3,5,5-trimethyl-3-cyclohexene-1-ketone (β-IP), product β The purity of ‑IP can reach 99.5wt%‑99.8wt%, and the reaction selectivity can reach 99.2%‑99.9%. The process has the advantages of less catalyst consumption, high selectivity, no alkali precipitation, less high boiling matter, etc., and is an efficient synthesis process.
Description
technical field [0001] The present invention relates to a preparation method of 3,5,5-trimethyl-3-cyclohexen-1-one (β-IP), in particular to the 3,5,5-trimethyl-3,5,5-trimethacrylate catalyzed by pro-nitrophosphatrane base A method for preparing 3,5,5-trimethyl-3-cyclohexen-1-one through isomerization of base-2-cyclohexen-1-one (α-IP). Background technique [0002] 3,5,5-Trimethyl-3-cyclohexen-1-one (β-IP) is an important intermediate for the synthesis of vitamin E, carotenoids, astaxanthin and other natural products and spices, especially The main raw material for the preparation of tea aroma ketone (2,6,6-trimethyl-2-cyclohexene-1,4-dione, KIP), tea aroma ketone is also the main raw material for the preparation of trimethylhydroquinone (VE main ring ) precursor. [0003] β-IP and α-IP are a pair of isomers, there is isomerism equilibrium under acid or base catalysis, β-IP can be prepared by isomerization reaction of α-IP. However, since β-IP is an unstable structure, its...
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