Method for producing KA oil and adipic acid through oxidizing cyclohexane with air on basis of 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 problems such as large energy consumption, affecting liquid fluidity, and blocked pipelines , to avoid oxidation or decomposition, solve the complex structure of the equipment, and improve the conversion rate

Active Publication Date: 2015-07-15
蚌埠启邦科技信息咨询有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the current cyclohexane oxidation industrial technology and other disclosed technologies still have the following problems: one is that during the entire reaction of cyclohexane air oxidation to prepare KA oil and adipic acid, the reaction raw material cyclohexane, air, and oxidation intermediates Peroxide and oxidation products KA oil and adipic acid coexist in the reaction zone, and these oxidation products will be further oxidized and decarboxylated to form other complex oxidation products; the second is that the oxidation product adipic acid is a solid product insoluble in cyclohexane. During the reaction process, it is easy to crystallize at the bottom of the oxidation reactor and in the flow pipeline, which will block the pipeline and affect the fluidity of the liquid in the production device, making continuous production impossible; the third is that the cyclohexane distillation separation tower separates a large amount of unreacted raw material rings The process of hexane needs to consume a lot of energy; the fourth is that the oxidation product adipic acid stays in the reaction system for a long time, and under the conditions of high temperature and high pressure, 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 KA oil and adipic acid through oxidizing cyclohexane with air on basis of gas-liquid-solid heterogeneous reaction separation synchronization reactor
  • Method for producing KA oil and adipic acid through oxidizing cyclohexane with air on basis of gas-liquid-solid heterogeneous reaction separation synchronization reactor
  • Method for producing KA oil and adipic acid through oxidizing cyclohexane with air on basis of 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 cyclohexane to prepare KA oil and adipic acid products; wherein, the diameter-to-height ratio of the bubbling gravity reaction tower is 1:20; the length of the gravity settling plate and the diameter of the tower Ratio 1:0.8; the angle of gravity settling plate tilted along the tower axis is 75°; there are two constant temperature settling towers Ⅰ and Ⅱ; the outlet of the reaction liquid is 2 / 5 away from the top of the reaction tower height.

[0035] Cobalt acetate is added to the cyclohexane raw material with a water content of 1.0wt% as a catalyst (concentration reaches 60ppm). 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 bubbling gravity reaction tower to control the bubbling gravity reaction tower and the constant temperature settli...

Embodiment 2

[0039] Attached figure 1 The shown gas-liquid-solid multiphase reaction separation synchronous reactor carries out the air oxidation of cyclohexane to prepare KA oil and adipic acid products; wherein, the diameter-to-height ratio of the bubbling gravity reaction tower is 1:40; the length of the gravity settling plate and the diameter of the tower The ratio is 1:1.2; the 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. height.

[0040] Add iron tetraphenylporphyrin (concentration up to 10ppm) and manganese naphthenate (concentration up to 100ppm) into the cyclohexane raw material with a water content of 1.5wt% as composite catalysts, and the mixed solution is introduced from the upper reaction material inlet of constant temperature settling t...

Embodiment 3

[0044] Attached figure 1 The shown gas-liquid-solid multiphase reaction separation synchronous reactor carries out the air oxidation of cyclohexane to prepare KA oil and adipic acid products; wherein, the diameter-to-height ratio of the bubbling gravity reaction tower is 1:35; the length of the gravity settling plate and the diameter of the tower The ratio is 1:1.2; the 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 3 / 7 away from the top of the reaction tower. height.

[0045] Copper tetraphenylporphyrin is added to the cyclohexane raw material with a water content of 2.0wt% as a catalyst (concentration reaches 20ppm), and the mixed solution enters the constant temperature settling tower I and the bubbling gravity reaction tower from the reaction material inlet on the upper part of t...

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Abstract

The invention discloses a method for producing KA oil and adipic acid through oxidizing cyclohexane with air on the basis of a gas-liquid-solid heterogeneous reaction separation synchronization reactor, wherein the water-containing cyclohexane 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 cyclohexane in the reaction, the air is introduced continuously from the bottom of the oxidization area and is in contact with the cyclohexane to carry out the oxidization reaction, meanwhile, a mixed phase of the produced KA oil, adipic acid and water settles and enters the bottom of the constant temperature settlement tower, the cyclohexane in the constant temperature settlement tower is pushed and goes up into the oxidization area to lead to the continuous reaction, the mixed phase continues to settle in the constant temperature settlement tower until the constant temperature settlement tower is fully filled with the mixed phase, then the reaction tower is switched to be communicated with the other constant temperature settlement tower filled with the cyclohexane, the operation is conducted on the constant temperature settlement towers alternatively to continuously produce the KA oil and adipic acid. The method is used to continuously produce the KA oil and the adipic 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 relates to a method for producing KA oil and adipic acid by air oxidation of cyclohexane based on a gas-liquid-solid multiphase reaction separation synchronous reactor, and belongs to the technical field of cyclohexane oxidation chemical industry. Background technique [0002] Air oxidation of cyclohexane yields KA oil (a mixture of cyclohexanol and cyclohexanone) and adipic acid. KA oil is the raw material for the production of caprolactam, which can also be further oxidized to adipic acid. Caprolactam is the monomer for the production of Nylon 6 and adipic acid is the monomer for the production of Nylon 66. Therefore, cyclohexane oxidation is an extremely important chemical production process. The process of cyclohexane oxidation to produce KA oil and adipic acid is as follows: [0003] [0004] Industrially, the method for producing KA oil by oxidation of cyclohexane is the non-catalyzed air oxidation method of Stamicka, the Neth...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/31C07C51/42C07C55/14C07C27/12C07C29/50C07C29/76C07C35/08C07C45/33C07C45/78C07C49/403B01J8/10B01J8/12
CPCB01J8/007B01J8/10B01J8/125C07C27/12C07C27/26C07C29/50C07C29/76C07C45/33C07C45/78C07C51/313C07C51/42C07C2601/14C07C55/14C07C35/08C07C49/403
Inventor 郭灿城郭欣
Owner 蚌埠启邦科技信息咨询有限公司
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