Method for producing substituted benzyl alcohol, substituted benzaldehyde and substituted benzyl acid through oxidizing substituted methylbenzene with air based on gas-liquid-solid heterogeneous reaction separation synchronization reactor

A multiphase reaction and air oxidation technology, applied in chemical instruments and methods, separation/purification of hydroxyl compounds, separation/purification of carbonyl compounds, etc., can solve the problems of large energy consumption and increase the difficulty of product separation, so as to improve the conversion The effect of high-yield and high-yield continuous production

Active Publication Date: 2015-04-01
YUANJIANG HUALONG CATALYST TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But, still there is following problem in this scheme: the one, during the whole reaction period of corresponding substituted benzyl alcohol and substituted benzaldehyde prepared in substituted toluene air oxidation, reaction raw material substituted toluene, air and reaction intermediate oxidation product substituted benzyl alcohol and substituted benzaldehyde coexist In the reaction zone, these oxidation products will be further oxidized into substituted benzoic acid; the second is that the oxidation product benzoic acid is a solid product insoluble in toluene, which is prone to crystallization and blockage at the bottom of the oxidation reactor and in the flow line during the continuous reaction process The pipeline affects the fluidity of the liquid in the production device and cannot be continuously produced; the third is that the process of separating toluene in the toluene distillation and separation tower consumes a lot of energy; the fourth is that the oxidation product replaces benzoic acid and stays in the reaction system for a long time. Under high pressure conditions, some products are further decarboxylated to form by-products, which increases the difficulty of product separation

Method used

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  • Method for producing substituted benzyl alcohol, substituted benzaldehyde and substituted benzyl acid through oxidizing substituted methylbenzene with air based on gas-liquid-solid heterogeneous reaction separation synchronization reactor
  • Method for producing substituted benzyl alcohol, substituted benzaldehyde and substituted benzyl acid through oxidizing substituted methylbenzene with air based on gas-liquid-solid heterogeneous reaction separation synchronization reactor
  • Method for producing substituted benzyl alcohol, substituted benzaldehyde and substituted benzyl acid through oxidizing substituted methylbenzene with air based on gas-liquid-solid heterogeneous reaction separation synchronization reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] use figure 1 The shown gas-liquid-solid multiphase reaction separation synchronous reactor carries out the air oxidation of toluene to prepare benzyl alcohol, benzaldehyde and benzoic acid products; wherein, the ratio of diameter to height of the bubbling gravity reaction tower is 1:20; The diameter ratio is 1:0.8; the angle of the gravity settling plate along the tower axis is 75°; there is a constant temperature settling tower Ⅰ

[0035] Two constant temperature settling towers and constant temperature settling tower II; the outlet of the reaction liquid is 2 / 5 of the height of the tower body from the top of the reaction tower.

[0036] Cobalt tetraphenylporphyrin (concentration up to 10ppm) is added to the toluene raw material with a water content of 1wt% as a catalyst. In the oxidation zone of the settling tower Ⅰ and the bubbling gravity reaction tower, the tee on the pressure balance pipe and the tee pipe at the bottom of the bubbling gravity reaction tower are c...

Embodiment 2

[0040] Attached figure 1 The shown gas-liquid-solid multiphase reaction separation synchronous reactor carries out the air oxidation of p-chlorotoluene to prepare p-chlorobenzyl alcohol, aldehyde and acid products; wherein, the diameter-to-height ratio of the bubbling gravity reaction tower is 1:40; the length of the gravity settling plate The ratio to the diameter of the tower is 1:1.2; the included angle of the gravity settling plate along the tower axis is 45°; there are two constant temperature settling towers, the constant temperature settling tower I and the constant temperature settling tower II; the outlet of the reaction liquid is 3 / 7 away from the top of the reaction tower At the height of the tower.

[0041] Add tetra-p-chlorophenylporphyrin iron μ-dimer (concentration up to 5ppm) and tetraphenylporphyrin manganese (concentration up to 5ppm) into the p-chlorotoluene raw material with a water content of 2wt% as a compound catalyst, and the mixture starts from The re...

Embodiment 3

[0045] Attached figure 1 The shown gas-liquid-solid multiphase reaction separation synchronous reactor carries out the air oxidation of p-nitrotoluene to prepare p-nitrobenzyl alcohol, aldehyde and acid products; wherein, the ratio of diameter to height of the bubbling gravity reaction tower is 1:35; gravity sedimentation The ratio of the length of the plate to the diameter of the tower is 1:1.2; the inclination angle of the gravity settling plate along the tower axis is 55°; there are two constant temperature settling towers, the constant temperature settling tower I and the constant temperature settling tower II; the outlet of the reaction liquid is 1 / 3 at the height of the tower.

[0046] Cobalt acetate (concentration up to 100ppm) is added as a catalyst to p-nitrotoluene raw material with a water content of 2wt%. In the oxidation zone of tower I and the bubbling gravity reaction tower, connect the tee on the pressure balance pipe and the tee pipe at the bottom of the bub...

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Abstract

The invention discloses a method for producing substituted benzyl alcohol, substituted benzaldehyde and substituted benzyl acid through oxidizing substituted methylbenzene with air on the basis of a gas-liquid-solid heterogeneous reaction separation synchronization reactor, wherein the water-containing substituted methylbenzene is added into the reactor, the reactor comprises a reaction tower and at least two constant temperature settlement towers communicated with the bottom of the reaction tower, and the reaction tower is internally provided with a gas phase area, an oxidization area and a gas outlet; the oxidization area and the constant temperature settlement towers are filled with the substituted methylbenzene in the reaction, the air is introduced continuously from the bottom of the oxidization area and is in contact with the substituted methylbenzene to carry out the oxidization reaction, meanwhile, a mixed phase of the produced substituted benzyl alcohol, substituted benzaldehyde and substituted benzyl acid settles and enters the bottom of the constant temperature settlement tower, the substituted methylbenzene in the constant temperature settlement tower is pushed into the oxidization area to lead to the continuous reaction, the reaction tower is switched to be communicated with the other constant temperature settlement tower filled with the substituted methylbenzene when the constant temperature settlement tower is fully filled with the mixed phase, the operation is conducted on the constant temperature settlement towers alternatively to continuously produce the substituted benzyl alcohol, substituted benzaldehyde and substituted benzyl acid. The method is used to continuously produce the substituted benzyl alcohol, substituted benzaldehyde and substituted benzyl acid with high percent of conversion and high selectivity, the production efficiency is improved, and the production cost is lowered.

Description

technical field [0001] The invention discloses a method for producing substituted benzyl alcohol, aldehyde and acid by using air oxidation to replace toluene based on a gas-liquid-solid multiphase reaction separation synchronous reactor, and belongs to the field of substituted toluene oxidation. Background technique [0002] Oxidation of substituted toluene can give the corresponding oxygenates substituted benzyl alcohol, substituted benzaldehyde and substituted benzoic acid. These oxygen-containing compounds are widely used in chemical industry, materials, medicine and other fields. In the oxidation reaction of substituted toluene, substituted benzyl alcohol and substituted benzaldehyde are intermediate oxidation products, which are easily further oxidized to substituted benzoic acid. In industry, the air liquid phase oxidation reaction of substituted toluene requires high temperature and high pressure conditions, and needs cobalt acetate or manganese acetate to catalyze, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C27/10C07C27/26C07C27/00C07C33/18C07C33/46C07C29/50C07C29/76C07C45/36C07C45/78C07C47/54C07C47/55C07C51/265C07C51/42C07C63/06C07C63/70C07C201/12C07C201/16C07C205/19C07C205/44C07C205/57C07C41/26C07C41/34C07C43/23C07C47/575C07C65/21B01J8/10B01J8/12
CPCB01J8/007B01J8/10B01J8/125C07C27/00C07C27/10C07C27/26C07C29/50C07C29/76C07C41/26C07C41/34C07C45/36C07C45/78C07C51/265C07C51/42C07C201/12C07C201/16C07C33/18C07C33/46C07C47/54C07C47/55C07C47/575C07C63/06C07C63/70C07C65/21C07C205/19C07C205/44C07C205/57C07C43/23
Inventor 郭灿城郭欣
Owner YUANJIANG HUALONG CATALYST TECH
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