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Method and device for preparing diphenylmethane series diamine and polyamine with low N-methyl impurity content and catalyst

A technology of diphenylmethane and catalyst, applied in the field of diphenylmethane series di- and polyamines, to achieve the effects of reducing content, improving product quality, and increasing reaction selectivity

Active Publication Date: 2018-03-23
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is no literature disclosing the method of improving the selectivity of the transposition rearrangement reaction through a catalyst in the DAM preparation process to reduce the N-methyl MDA in the product

Method used

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  • Method and device for preparing diphenylmethane series diamine and polyamine with low N-methyl impurity content and catalyst
  • Method and device for preparing diphenylmethane series diamine and polyamine with low N-methyl impurity content and catalyst
  • Method and device for preparing diphenylmethane series diamine and polyamine with low N-methyl impurity content and catalyst

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Experimental program
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Effect test

Embodiment 1

[0044] The reaction process is as figure 1 As shown in the process flow chart, the active component of the transposition rearrangement reaction catalyst vanadium phosphate oxide carrier is γ-Al 2 o 3 , aniline material (mass concentration is 94%) and formaldehyde material (formaldehyde mass concentration is 37%) enters condensation reactor 1, and the mol ratio of hydrochloric acid and aniline is 0.41:1, and formaldehyde and aniline mol ratio are 0.60:1, residence time Are 60min, the condensation reaction occurred. A reaction mixture containing polyaminobenzylaniline salt is generated, which enters a vanadium phosphate oxide catalyst (supported on γ-Al 2 o 3 , based on the metal element, the mass fraction of the active component of the catalyst is 0.01%, and the vanadium phosphate oxide is prepared by roasting a mixture of vanadium pentoxide and phosphoric acid, and the mass ratio of the raw materials is 1:3). In the fixed-bed reactor 2, the catalyst Transposition rearrange...

Embodiment 2

[0046] The reaction process is as figure 1 As shown in the process flow diagram, the transposition rearrangement reaction catalyst active component Pr 2 o 3 -Ce 2 o 3 The solid solution carrier is γ-Al 2 o 3 , aniline material (mass concentration is 94%) and formaldehyde material (formaldehyde mass concentration is 37%) enters condensation reactor 1, and the mol ratio of hydrochloric acid and aniline is 0.41:1, and formaldehyde and aniline mol ratio are 0.60:1, residence time Are 60min, the condensation reaction occurred. A reaction mixture containing polyaminobenzylaniline salt is generated, which is filled with Pr 2 o 3 -Ce 2 o 3 Solid solution catalyst (Pr 2 o 3 50%, Ce 2 o 3 50%, supported on γ-Al 2 o 3 , on the basis of metal element, the mass fraction of catalyst active components is 0.05%, Pr 2 o 3 -Ce 2 o 3 The solid solution is prepared by the co-precipitation method, the co-precipitation agent is NaOH, and the active component is loaded on the car...

Embodiment 3

[0048] The reaction process is as figure 1 As shown in the process flow chart, the active component of the transposition rearrangement reaction catalyst is Nb 2 o 5 -La 2 o 3 Solid solution, the carrier is γ-Al 2 o 3 , aniline material (mass concentration is 94%) and formaldehyde material (formaldehyde mass concentration is 37%) enters condensation reactor 1, and the mol ratio of hydrochloric acid and aniline is 0.21:1, and formaldehyde and aniline mol ratio are 0.40:1, residence time Are 60min, the condensation reaction occurred. A reaction mixture containing polyaminobenzylaniline salt is generated, which enters the Nb-filled 2 o 5 -La 2 o 3 Solid solution (Nb 2 o 5 50% by mass, La 2 o 3 50% by mass, loaded on γ-Al 2 o 3, on the basis of metal element, the mass fraction of catalyst active components is 0.05%, Nb 2 o 5 -La 2 o 3 The solid solution is prepared by the co-precipitation method, the co-precipitation agent is NaOH, and the active component is lo...

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Abstract

The invention relates to a method and a device for preparing diphenylmethane series diamine and polyamine with low N-methyl impurity content and a catalyst. The method comprises the steps as follows:a) phenylamine and formaldehyde are subjected to a condensation reaction in the presence of an acid catalyst, and a reaction mixture containing polyamino benzylaniline salt is obtained; b) the reaction mixture from a) enters a fixed bed reactor loaded with the catalyst for a transposition rearrangement reaction, a mixture containing diphenylmethane series diamine salt and polyamine salt is obtained after the reaction, and active components of the transposition rearrangement reaction catalyst comprise one or more of vanadium phosphate oxide, a Nb2O5-La2O3 solid solution and a Pr2O3-Ce2O3 solidsolution. The reaction selectivity at the transposition rearrangement stage can be improved, so that the content of N-methyl MDA impurities in the product can be decreased, the product quality can besubstantially improved, and the N-methyl MDA content can be decreased to 0.01% or below.

Description

technical field [0001] The present invention relates to a method and device for improving the stage selectivity of transposition rearrangement reaction, greatly suppressing the occurrence of side reactions, and preparing diphenylmethane series di-and-polyamines (DAM) with low N-methyl impurity content and Catalysts used in this process. Background technique [0002] The diamines and polyamines of the diphenylmethane series (DAM for short) should be understood as referring to the mixture of the following types of amines and polyamines:: [0003] [0004] Where n represents a natural number ≥ 0. Formally, all NH in the compound of the above formula can be replaced by NCO groups 2 The corresponding isocyanate obtained by the corresponding group is called diphenylmethane series diisocyanate, diphenylmethane series polyisocyanate or diphenylmethane series diisocyanate and polyisocyanate (MDI). [0005] The preparation process of DAM is generally known, conventionally carrie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/54C07C211/50B01J27/198B01J23/20B01J23/10
CPCB01J23/002B01J23/10B01J23/20B01J27/198C07C209/54C07C211/50
Inventor 崔成成周波吴雪峰张宏科赵东科杨径靖刘小高徐丹吴俊
Owner WANHUA CHEM GRP CO LTD
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