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A kind of method for ethylbenzene continuous oxidation separation coupling strengthening synthesis acetophenone and α-phenethyl alcohol

A technology of acetophenone and phenylethanol, which is applied in the field of preparation of acetophenone and α-phenylethanol by oxidation of ethylbenzene, biomimetic metalloporphyrin catalyst catalyzed air oxidation of ethylbenzene to prepare acetophenone and α-phenylethanol, which can solve the problem of improving Problems such as cost and difficulty of product separation, unfavorable production of α-phenylethanol, increased difficulty of product separation, etc., to achieve the effects of being beneficial to industrial production, avoiding side reactions, and high conversion rate

Active Publication Date: 2021-03-16
YUANJIANG HUALONG CATALYST TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The conversion rate of its ethylbenzene is increased to about 45%, but the selectivity of its α-phenylethanol is only about 10%, and it needs to adopt pure oxygen as an oxidant, and needs to use solvent and hydrogen transfer agent, which increases the product difficulty of separation
[0004] In summary, there are some substantial defects in the method of using metalloporphyrins to catalyze ethylbenzene to synthesize acetophenone and α-phenylethanol: 1) these reactions are batch reactions, which are difficult to industrialized large-scale production; To ensure the high conversion rate of ethylbenzene, the oxidation efficiency of ethylbenzene is usually improved by prolonging the reaction time or increasing the amount of oxidant and catalyst, but these conditions are not conducive to the formation of α-phenylethanol. However, only acetophenone can be obtained as the absolute main product; 3) the existing catalytic oxidation reaction usually requires the addition of solvents and catalytic promoters, which increases the cost and the difficulty of product separation

Method used

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  • A kind of method for ethylbenzene continuous oxidation separation coupling strengthening synthesis acetophenone and α-phenethyl alcohol
  • A kind of method for ethylbenzene continuous oxidation separation coupling strengthening synthesis acetophenone and α-phenethyl alcohol
  • A kind of method for ethylbenzene continuous oxidation separation coupling strengthening synthesis acetophenone and α-phenethyl alcohol

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Experimental program
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Effect test

Embodiment 1

[0058] The ethylbenzene raw material whose water content is 1wt% and tetra-methoxyphenyl porphyrin manganese concentration is 5ppm enters the constant temperature settling tower I and the bubbling gravity reaction tower from the reaction material inlet on the upper part of the constant temperature settling tower I, and is full of the constant temperature settling tower I and the oxidation zone of the bubbling gravity reaction tower, the tee on the circulation pipe and the tee pipe at the bottom of the bubbling gravity reaction tower are connected to the constant temperature settling tower I, and the gas raw material from the bubbling gravity reaction tower Air is introduced into the inlet port, and the volume content of oxygen in the reaction gas exported from the outlet port of the reaction gas is controlled to be 5%. The ethylbenzene in the bubble gravity reaction tower is circulated through the external circulation system, and the circulation speed ensures that the average r...

Embodiment 2

[0064]Water content is 0.5wt%, tetra-p-butylphenyl porphyrin ferric chloride concentration is that the ethylbenzene raw material of 8ppm enters constant temperature settling tower I and bubbling gravity reaction tower from constant temperature settling tower I upper reaction material inlet, is full of constant temperature settling In the oxidation zone of tower I and the bubbling gravity reaction tower, the tee on the circulation pipe and the tee pipe at the bottom of the bubbling gravity reaction tower are connected to the constant temperature settling tower I, from the bubbling gravity reaction tower The gas raw material inlet is fed with air, and the volume content of oxygen in the reaction gas exported from the reaction gas outlet is controlled to be 8%, the temperature of the bubbling gravity reaction tower is adjusted to 75°C, the pressure inside the tower is kept at 2.5atm for oxidation reaction, and constant temperature sedimentation The ethylbenzene in the tower and th...

Embodiment 3

[0066] Water content is 1.5wt%, tetra-p-propylphenylporphyrin iron μ-dimer concentration is that the ethylbenzene raw material of 3ppm enters constant temperature settling tower 1 and bubbling gravity reaction tower from constant temperature settling tower 1 top reaction material import port, Fill the oxidation zone of the constant temperature settling tower I and the bubbling gravity reaction tower, connect the tee on the circulating pipe and the tee pipe at the bottom of the bubbling gravity reaction tower to communicate with the constant temperature settling tower I, from the bubbling gravity The gas raw material inlet of the reaction tower is fed with air, and the volume content of oxygen in the reaction gas exported from the reaction gas outlet is controlled to be 3%, the temperature of the bubbling gravity reaction tower is adjusted to 95°C, and the internal pressure of the tower is kept at 1.5atm for oxidation reaction , the ethylbenzene in the constant temperature settl...

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Abstract

The invention discloses a method for synthesizing acetophenone and alpha-phenethyl alcohol through continuous ethylbenzene oxidation, separation and coupling reinforcement. An ethylbenzene material containing water and metalloporphyrin is added to a reactor, wherein the reactor comprises a reaction tower and at least two constant-temperature settling towers, and a gas phase zone, an oxidation zoneand a gas outlet are arranged in the reaction tower; the oxidation zone and the constant-temperature settling towers of the reactor are filled with ethylbenzene, air is continuously introduced from the bottom of the oxidation zone to contact with ethylbenzene for a reaction, produced acetophenone and alpha-phenethyl alcohol products and water form a mixed phase to settle and enter one constant-temperature settling tower, ethylbenzene in the constant-temperature settling tower enters the oxidation zone of the reactor through external circulation, so that the reaction is performed continuously,when the mixed phase continuously settles until the constant-temperature settling tower is full of ethylbenzene, the reaction tower is switched to be communicated with another constant-temperature settling tower, and the process is alternately performed for continuous production. With the adoption of the method, the yield of acetophenone and alpha-phenethyl alcohol is high, the alcohol-ketone ratio is high, the method can be applied to continuous production, the production efficiency is greatly improved, and the production cost is reduced.

Description

technical field [0001] The invention relates to a method for preparing acetophenone and α-phenylethanol by oxidation of ethylbenzene, in particular, a method for preparing acetophenone and α-phenylethanol by catalyzing air oxidation of ethylbenzene with a biomimetic metalloporphyrin catalyst; In particular, it relates to a method for realizing the continuous oxidation, separation, coupling and enhanced synthesis of acetophenone and α-phenylethanol by using a reaction separation synchronous reactor, and belongs to the technical field of organic intermediate synthesis. Background technique [0002] Acetophenone and α-phenylethanol are common organic raw materials and intermediates. Acetophenone can be widely used in the preparation of drugs, resins, flavoring agents and tear gas, such as the preparation of sleeping pills, etc., the synthesis of mandelic acid, α-phenylindole, ibuprofen, etc., and also as cellulose ester and resin and other solvents and plasticizers in the prod...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C27/12C07C45/36C07C49/78C07C29/50C07C33/22
CPCC07C29/50C07C45/36C07C49/78C07C33/22
Inventor 郭欣郭灿城罗伟平刘强
Owner YUANJIANG HUALONG CATALYST TECH
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