A kind of intramolecular dehydration catalyst of amino alcohol, preparation method and application

A catalyst, amino alcohol technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., can solve the problems of low catalyst activity and selectivity, reduced ethyleneimine selectivity, and short service life, etc. To achieve the effect of stable activity, improved diffusion effect and long life

Active Publication Date: 2016-03-02
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] In the prior art, the intramolecular dehydration reaction of amino alcohol is carried out at a relatively low temperature (~370°C), the catalyst activity and selectivity are low, and the reaction temperature is high. Generally, the reaction can be carried out quickly only when the temperature is higher than 400°C. Deamination and intermolecular condensation reactions are prone to occur, resulting in an increase in by-products, resulting in a decrease in the selectivity of ethyleneimine. Generally, the weight selectivity is lower than 65%, and the service life is short

Method used

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  • A kind of intramolecular dehydration catalyst of amino alcohol, preparation method and application
  • A kind of intramolecular dehydration catalyst of amino alcohol, preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Prepare the catalyst TiP according to the stoichiometric ratio 0.2 B 0.01 Mg 0.1 Cs 0.01 o 2.62 :

[0041] Fully mix 97.86g of metatitanic acid, 26.4g of diammonium hydrogen phosphate and 0.618g of boric acid according to the stoichiometric ratio, then dissolve 14.8g of magnesium nitrate and 1.95g of cesium nitrate in water according to the stoichiometric ratio, and add the above solid mixture , evaporate and dry, then add graphite to the obtained mixture (the amount of graphite is 3% of the mass of the mixture), press molding, and dry at 120°C for 6h, bake at 350°C for 6h in air atmosphere, and bake at 600°C for 6h to obtain catalyst. The specific surface area was measured by low temperature nitrogen adsorption method to be 53.5m 2 / g, pore volume 0.26mL / g, average pore diameter 5.9nm.

[0042] The catalyst of this example is loaded into the reactor with a loading volume of 30mL, heated to a reaction temperature of 370°C, nitrogen as a protective gas, the gas vo...

Embodiment 2

[0044] Prepare the catalyst TiP according to the stoichiometric ratio 0.1 B 0.01 Ba 0.05 K 0.01 o 2.32 :

[0045] The metatitanic acid, ammonium phosphate and boric acid components are fully mixed according to the stoichiometric ratio, and the stoichiometric barium nitrate component and potassium chloride component are dissolved in water, added to the above solid mixture, evaporated and dried, and then the obtained Graphite was added to the mixture (the amount of graphite used was 4% of the mass of the mixture), press-molded, dried at 120°C for 6h, calcined at 350°C for 6h in an air atmosphere, and calcined at 700°C for 6h to obtain a catalyst. Its specific surface area is determined by low temperature nitrogen adsorption method to be 48.1m 2 / g, pore volume 0.21mL / g, average pore diameter 5.3nm.

[0046] This embodiment catalytic reaction condition and analysis condition are the same as embodiment 1. The conversion rate of ethanolamine is 35%, and the selectivity of et...

Embodiment 3

[0048] Prepare the catalyst TiP according to the stoichiometric ratio 0.05 B 0.02 Ba 0.1 K 0.01 o 2.27 :

[0049] Fully mix the metatitanic acid, ammonium dihydrogen phosphate and boric acid components according to the stoichiometric ratio, dissolve the stoichiometric barium nitrate component and potassium nitrate component in water, add to the above solid mixture, evaporate and dry, and then Graphite was added to the obtained mixture (the amount of graphite used was 1% of the mass of the mixture), press-molded, dried at 120°C for 6 hours, calcined at 350°C for 6 hours in an air atmosphere, and then calcined at 800°C for 6 hours to obtain a catalyst. The specific surface area is 51.2m2 measured by low temperature nitrogen adsorption method 2 / g, pore volume 0.26mL / g, average pore diameter 5.8nm.

[0050] This embodiment catalytic reaction condition and analysis condition are the same as embodiment 1. The conversion rate of ethanolamine is 49%, and the selectivity of eth...

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Abstract

The invention relates to an intramolecular dehydration catalyst for alkamine, a preparation method and application. The composition of the catalyst is TiaPbBcXdYeOf, wherein X is alkaline-earth metal, Y is alkali metal and O is oxygen; a, b, c, d, e and f are atomic ratios of elements, when a is 1, b is 0.02-0.2, c is 0.002-0.02, d is 0.01-0.1, and e is 0.001-0.01. The preparation method comprises steps as follows: metatitanic acid, phosphate and boric acid components are mixed in a stoichiometric ratio, then a metal salt water solution containing stoichiometric X component and Y component is added, evaporation and drying are performed, graphite is added into the mixture, the amount of the graphite accounts for 1%-4% of the mass of the mixture, and after compression molding, the mixture is roasted under presence of oxygen at the temperature of 350 DEG C and then roasted at the temperature of 600 DEG C-900 DEG C to obtain the catalyst. The catalyst is used for an intramolecular dehydration reaction of the alkamine, and according to the catalyst, a secondary dehydrogenation reaction, an intermolecular dehydration reaction, an aziridine dimerization reaction and a hydrogen transfer reaction are reduced, and high selectivity is provided at a low temperature.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to an intramolecular dehydration catalyst of amino alcohol, a preparation method and application thereof. Background technique [0002] Amino alcohols have bifunctional groups and active chemical properties, and amino alcohols with adjacent structures can be synthesized into important ethyleneimine compounds through intramolecular dehydration. [0003] Using monoethanolamine as raw material, ethyleneimine can be obtained through intramolecular dehydration reaction. [0004] US433717 discloses a method for producing ethyleneimine with a composite oxide catalyst of Nb or Ta oxide and alkaline earth metal oxide (BaO). Specifically, Nb or Ta chloride is made into an impregnating solution for loading, loaded on the surface of the carrier, and subjected to calcination at 450-550° C. for 2-4 hours to obtain the catalyst. The reaction temperature is 400°C, the conver...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/18C07D203/08C07D301/02C07D303/36
Inventor 杨建明吕剑梅苏宁李亚妮王伟余秦伟赵锋伟袁俊王为强
Owner XIAN MODERN CHEM RES INST
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