Preparation method of α-isophorone

A technology of isophorone and acetone, applied in the field of preparation of α-isophorone, can solve the problems of difficult to accurately control the residence time of reactants, low selectivity of α-isophorone, unsatisfactory acetone conversion rate and the like , to achieve the effect of low temperature and pressure, short reaction time and lower energy consumption cost

Active Publication Date: 2022-05-20
SHANDONG NHU VITAMIN CO LTD
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Problems solved by technology

The reaction and rectification are integrated into a reactive distillation column, and the disturbance of the gas phase is used for strong stirring. The conversion rate of acetone is 10.4%, and the selectivity of α-isophorone is 82%, but the conversion rate of acetone in this process is low And it is difficult to accurately control the residence time of reactants
CN102516051B adopts a mixer and a microchannel reactor, the effect of mass and heat transfer is good, the conversion rate of acetone is greater than 20%, and the selectivity of α-isophorone can reach more than 90%, but the conversion rate of acetone in this process is still not ideal
[0014] In summary, the existing synthetic methods for α-isophorone still have the problems of low conversion rate of acetone, low selectivity of α-isophorone, and long reaction time

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[0037] The embodiment of the present invention provides a preparation method of α-isophorone, which is characterized in that it comprises the following steps:

[0038] Acetone and a hydrotalcite-based composite oxide catalyst are subjected to a polycondensation reaction under supercritical conditions, and the structural formula of the hydrotalcite-based composite oxide catalyst is Sr x Mg 0.7-x Al 0.2-y m y O, wherein, M is selected from one of Pr, Ga, and In, 0.05≤x≤0.35, 0.02≤y≤0.1;

[0039] The components in the product of the above polycondensation reaction are separated to obtain acetone multimer, and the acetone multimer and water are hydrolyzed in a high-gravity reactor.

[0040] The preparation method of α-isophorone that the embodiment of the present invention provides adopts Sr x Mg 0.7- x Al 0.2-y m y O-type hydrotalcite-based composite oxides are used as catalysts, and combined with the hydrolysis reaction steps under high gravity conditions, the mass trans...

Embodiment 1

[0063] (1) Catalyst 5gSr 0.1 Mg 0.6 Al 0.15 PR 0.05 O and 500g acetone (mass ratio is the ratio of 0.01:1) are mixed uniformly to obtain suspension, and this suspension carries out polycondensation reaction at 8MPa, 270 ℃ of supercritical conditions in tubular reactor, and the reaction time is 1min, suspending The turbid liquid was injected into the tubular reactor at a flow rate of 10 g / min. After the polycondensation reaction, the reaction liquid in the tubular reactor was cooled, and the sample was detected by GC, and the conversion rate of acetone was calculated to be 39.3%, and the selectivity of α-isophorone was 90.1%.

[0064] (2) After the polycondensation reaction finishes, each component of the reaction solution in the tubular reactor is further separated by rectification (each component separated by rectification comprises acetone, isophorone, acetone polymer (acetone four polymer and acetone pentamer), water and other impurities), and the separated acetone poly...

Embodiment 2～ Embodiment 16

[0066] Take acetone as benchmark, the quality of acetone is constant, adjust catalyst and acetone mass ratio and adjust each reaction condition (supercritical pressure, supercritical temperature, polycondensation reaction time, suspension flow rate namely flow rate) in the polycondensation reaction under acetone supercritical condition ), repeat embodiment 1, and reaction result is as shown in table 1. In addition, adjust the mass ratio of acetone multimer and water and each reaction condition (hydrolysis reaction temperature, hydrolysis reaction time, supergravity reactor stirring speed is stirring speed) in the mass ratio of acetone multimer and the high gravity hydrolysis reaction of acetone multimer, repeat embodiment 1, The results are shown in Table 2.

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Abstract

The present invention relates to a preparation method of α-isophorone, comprising the following steps: polycondensing acetone and a hydrotalcite-based composite oxide catalyst under supercritical conditions, and the structural formula of the hydrotalcite-like composite oxide catalyst is for Sr x Mg 0.7‑ x al 0.2‑y m y O, wherein, M is selected from any one of Pr, Ga, In, 0.05≤x≤0.35, 0.02≤y≤0.1; each component in the product of the polycondensation reaction is separated to obtain an acetone polymer, The acetone polymer and water are hydrolyzed in a high gravity reactor.

Description

technical field [0001] The invention relates to the technical field of organic chemical industry, in particular to a preparation method of α-isophorone. Background technique [0002] α-isophorone, namely 3,5,5-trimethyl-2-cyclohexen-1-one, is a colorless or water white to yellow low volatility liquid with a characteristic odor of camphor or mint , naturally present in cranberries, tobacco, mushrooms, wine, chrysanthemum, and pomelo juice. α-isophorone has strong solubility, good dispersion and leveling, and is an excellent high-boiling solvent; in addition, it is also an important organic synthesis raw material for the production of tea aroma ketone, α-isophorone di Fine chemical products such as amine and α-isophorone diisocyanate. [0003] The traditional method of preparing α-isophorone is divided into two kinds of mesityl oxide method and acetone condensation method. [0004] The mesityl oxide method uses mesityl oxide and ethyl acetoacetate under the action of a cata...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/74C07C49/603
CPCC07C45/74C07C2601/16C07C49/603Y02P20/54
Inventor 乔胜超张玉霞毛建拥严宏岳潘洪
Owner SHANDONG NHU VITAMIN CO LTD
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