A device and method for preparing cycloaliphatic amines by continuous hydrogenation reduction of aromatic amines

A technology for alicyclic amines and aromatic amines, which is applied in the field of devices for preparing alicyclic amines by continuous hydrogenation reduction of aromatic amines, can solve the problem that the mixing effect is not ideal, secondary mixing of products cannot be achieved, and efficient mixing is difficult to achieve. To solve the problem of reaction heat removal, improve controllability and safety, and achieve the effect of not deactivating catalyst activity

Active Publication Date: 2022-03-29
SHENYANG RES INST OF CHEM IND
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Problems in existing technical solutions: Since the microporous structure of existing micro-reaction equipment has a size of submillimeter to micron in all directions, if the fluid in the treated system has high viscosity or there is slurry or solid , the pressure drop is very large, it is easy to cause some or all of it to be blocked, and the micro-mixing units are connected in parallel, the gas-liquid can only be mixed once in one mixing zone, and when the first mixing is not uniform, it is impossible to adjust The product is mixed twice, the mixing effect is not ideal, and it is difficult to achieve high-efficiency mixing in the application of continuous hydrogenation units

Method used

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  • A device and method for preparing cycloaliphatic amines by continuous hydrogenation reduction of aromatic amines
  • A device and method for preparing cycloaliphatic amines by continuous hydrogenation reduction of aromatic amines
  • A device and method for preparing cycloaliphatic amines by continuous hydrogenation reduction of aromatic amines

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Comparison scheme
Effect test

Embodiment 1

[0035] device such as figure 1 Shown, the present invention comprises raw material tank 9, gas cylinder 8, micro-mixer 1, micro-packed bed 2, delay pipeline 3, gas-liquid separation tank 4 and storage tank 6, wherein as figure 2 As shown, the micro-mixer 1 is provided with two material inlets 101 and a material outlet 105, and the raw material tank 9 is connected to a material inlet 101 of the micro-mixer 1 through a first pipeline, and The first pipeline is provided with an input pump 7, and the input pump 7 is used to input the raw materials into the micro-mixer 1, and the gas bottle 8 is fed into another material of the micro-mixer 1 through the second pipeline. Port 1 is connected, and the second pipeline is provided with an air inlet control valve, a gas flow meter for detecting gas flow, and an air inlet pressure gauge 11 for detecting air pressure, the outlet 105 of the micro mixer 1, the micro filling The bed 2, the delay pipeline 3, and the gas-liquid separation tan...

Embodiment 2

[0047] Using the device shown in the above embodiment, the micro-mixer 1 is provided with five flow plates 103 and five manifolds 104 for hydrogenation and reduction of aromatic amines to prepare cycloaliphatic amines. The specific steps are as follows:

[0048] Reaction equation

[0049]

[0050] (1) Preparation of reaction solution containing aromatic amine

[0051] 4,4'-methylenebis(2-diethyl)aniline (M-OEA for short) was selected as a raw material, and cyclohexane was used as a solvent to prepare a raw material reaction solution with a concentration of 1 mol / L.

[0052] (2) hydrogenation reduction reaction

[0053] Operating conditions: Under the conditions of temperature 110°C and pressure 1MPa, hydrogen gas with a purity of 99.99% and the above-mentioned raw material reaction solution are simultaneously passed into the micro-mixer 1 for dispersion and mixing, and the molar flow ratio of hydrogen gas to M-OEA is 10:1 , the micro-packed bed jacket is heated to 110 ° C...

Embodiment 3

[0057] Using the device shown in the above embodiment, the micro-mixer 1 is provided with 8 flow plates 103 and 8 manifolds 104 for hydrogenation and reduction of aromatic amines to prepare cycloaliphatic amines. The specific steps are as follows:

[0058] Reaction equation

[0059]

[0060] (1) Preparation of working fluid containing aromatic amines

[0061] 4,4'-methylenebis(2-methyl-6-ethylaniline) (M-MEA for short) was selected as a raw material and tetrahydrofuran was used as a solvent to prepare a raw material reaction solution with a concentration of 1.4 mol / L.

[0062] (2) hydrogenation reduction reaction

[0063] Operating conditions: Under the conditions of temperature 120°C and pressure 2MPa, the hydrogen gas with a purity of 99.99% and the raw material reaction solution are simultaneously passed into the micro-mixer 1 for dispersion and mixing, and the molar flow ratio of hydrogen gas and M-MEA is 10: 1. Heat the jacket of the micro-packed bed to 120 ° C, the re...

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Abstract

The invention relates to the technical field of catalytic hydrogenation, in particular to a device and method for preparing alicyclic amines through continuous hydrogenation reduction of aromatic amines. The device comprises a raw material tank (9), a gas cylinder (8), a micro-mixer (1), a micro-packed bed (2), a delay pipeline (3) and a gas-liquid separation tank (4). The method of continuous hydrogenation reduction of aromatic amines to prepare cycloaliphatic amines is to continuously feed the reaction solution containing aromatic amines and hydrogen into the micro-mixer (1) at the same time to fully and uniformly mix the gas-liquid two phases, and then continuously mix with Catalysts are contacted to carry out gas-liquid-solid three-phase hydrogenation reduction reaction, and the liquid phase products after the reaction are rectified to obtain alicyclic amine products. The invention realizes the continuous production of cycloaliphatic amine compounds with large flow rate, realizes the combination of the micro-reaction system and the packed bed, and the stagnation of materials in the micro-reaction system is small, and improves the controllability and safety of the catalytic hydrogenation reaction sex.

Description

technical field [0001] The invention relates to the technical field of catalytic hydrogenation, in particular to a device and method for preparing alicyclic amines through continuous hydrogenation reduction of aromatic amines. Background technique [0002] Aromatic amines include aromatic monoamines, diamines and polyamines, among which aromatic monoamines include aniline and substituted aniline, etc., which are important chemical raw materials. Another example is 4,4'-methylenebis(3-chloro-2,6-diethylaniline), 4,4'-methylenebis(2,6-diisopropylaniline), 4,4 '-Methylenebis(2,6-diethylaniline), 4,4'-methylenebis(2-methyl-6-ethylaniline), 4,4'-methylenebis(2 -Diethyl)aniline, etc., is a standard curing agent for civil engineering, coatings and composite materials. [0003] The hydrogenation reduction of aromatic amines to prepare cycloaliphatic amines can further improve product application performance and expand application fields. The existing hydrogenation reduction metho...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/72C07C211/35
Inventor 鄢冬茂王珂胥维昌龚党生杨林涛明卫星
Owner SHENYANG RES INST OF CHEM IND
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