Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Device and method for preparing alicyclic amine through continuous hydrogenation reduction of aromatic amine

A technology for cycloaliphatic amines and aromatic amines, which is applied in the field of continuous hydrogenation reduction of aromatic amines to prepare cycloaliphatic amines, which can solve the problem of unsatisfactory mixing effects, difficulty in achieving high-efficiency mixing, and inability to remix products, etc. problem, achieve the effect of solving the problem of reaction heat removal, improving controllability and safety, and not inactivating the activity

Active Publication Date: 2019-06-25
SHENYANG RES INST OF CHEM IND
View PDF10 Cites 5 Cited by
  • Summary
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Device and method for preparing alicyclic amine through continuous hydrogenation reduction of aromatic amine
  • Device and method for preparing alicyclic amine through continuous hydrogenation reduction of aromatic amine
  • Device and method for preparing alicyclic amine through continuous hydrogenation reduction of aromatic amine

Examples

Experimental program
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 5 flow plates 103 and 5 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, the ...

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...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
diameteraaaaaaaaaa
sizeaaaaaaaaaa
porosityaaaaaaaaaa
Login to View More

Abstract

The invention relates to the technical field of catalytic hydrogenation, in particular to a device and method for preparing alicyclic amine through continuous hydrogenation reduction of aromatic amine. The device comprises a raw material tank (9), a gas cylinder (8), a micromixer (1), a micro filling bed (2), a delay pipeline (3) and a gas-liquid separation tank (4). The method for preparing the alicyclic amine through continuous hydrogenation reduction of the aromatic amine comprises the steps that a reaction solution containing the aromatic amine and hydrogen are simultaneously and continuously introduced into the micromixer (1) to enable gas and liquid phases to be fully and evenly mixed, after mixing, a gas and liquid mixture continuously makes contact with a catalyst for a gas, liquidand solid three-phase hydrogenation reduction reaction, after the reaction, a liquid-phase product is rectified, and thus an alicyclic amine product is obtained. Continuous production of a large-flowalicyclic amine compound is achieved, a micro-reaction system and the filling bed are combined, the idle stock of materials in the micro-reaction system is small, and the controllability and safety of the catalytic hydrogenation reaction are improved.

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products