Monoethanolamine intramolecular dehydration catalyst

A technology of monoethanolamine and catalyst, which is applied in the field of catalysts for synthesizing aziridine by intramolecular dehydration of monoethanolamine. Improve diffusion effect, increase selectivity, reduce reaction effect

Active Publication Date: 2015-12-09
XIAN MODERN CHEM RES INST +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent CN103657694A reports a composite oxide catalyst composed of titanium, phosphorus, boron, alkaline earth metals and alkali metals. The selectivity of aziridine reaches 92%, but the conversion rate of monoethanolamine is only 63%.
In the prior art, the catalyst is highly acidic and prone to intermolecular condensation reactions to generate piperazine by-products, resulting in a reduction in aziridine selectivity; the catalyst is highly alkaline and prone to deamination reactions to generate by-product acetaldehyde, which further reacts with Product aziridine reacts to generate 1-aziridine base ethanol, thereby affecting the further improvement of aziridine product selectivity
The catalysts reported in the current patents only use phosphides or borides to adjust the acidity. While the conversion rate of raw materials is increased, the selectivity of aziridine will be greatly reduced. It is difficult to obtain a higher conversion rate of monoethanolamine and aziridine at the same time. Conversion rate

Method used

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  • Monoethanolamine intramolecular dehydration catalyst

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Experimental program
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Effect test

Embodiment 1

[0028] 1. Preparation of acid-activated montmorillonite

[0029] Disperse 16.33g montmorillonite in 800g mass fraction of 20% nitric acid aqueous solution, prepare a mass fraction of 2% montmorillonite suspension, stir, activate at 104°C for 24 hours, centrifuge at 8000 rpm for 6 Minutes, the precipitate was washed with distilled water until neutral, dried in an oven at 80°C for 12 hours, then baked in a muffle furnace at 900°C for 4 hours, cooled naturally to room temperature, and ground with a mortar to prepare acid-activated montmorillonite.

[0030] 2. Preparation of monoethanolamine intramolecular dehydration catalyst

[0031] Using equal volume impregnation method, according to Cs 3.0 P 2.4 La 1.0 o 18 The stoichiometric ratio of 0.26g cesium nitrate, 0.19g lanthanum nitrate hexahydrate, and 0.22g ammonium phosphate trihydrate were added to deionized water and allowed to stand for 15 minutes to obtain an impregnation solution; according to Cs 3.0 P 2.4 La 1.0 o 1...

Embodiment 2

[0033] 1. Preparation of acid-activated montmorillonite

[0034] Disperse 16.33g montmorillonite in 800g mass fraction of 20% nitric acid aqueous solution, prepare a mass fraction of 2% montmorillonite suspension, stir, activate at 104°C for 24 hours, centrifuge at 8000 rpm for 6 Minutes, the precipitate was washed with distilled water until neutral, dried in an oven at 80°C for 12 hours, then baked in a muffle furnace at 800°C for 4 hours, cooled naturally to room temperature, and ground with a mortar to prepare acid-activated montmorillonite.

[0035] 2. Preparation of monoethanolamine intramolecular dehydration catalyst

[0036] Using equal volume impregnation method, according to Cs 3.0 P 2.4 Ce 1.0 o 18 The stoichiometric ratio, 0.35g cesium nitrate, 0.26g cerium nitrate hexahydrate, 0.13g pyrophosphoric acid were added to deionized water, and left to stand for 15 minutes to obtain an impregnation solution; according to Cs 3.0 P 2.4 Ce 1.0 o 18 The loading capacit...

Embodiment 3

[0038] 1. Preparation of acid-activated montmorillonite

[0039] Disperse 20g of montmorillonite in 480g of 20% nitric acid aqueous solution by mass fraction to prepare a 4% montmorillonite suspension, stir, activate at 104°C for 24 hours, and centrifuge for 6 minutes at 8000 rpm , the precipitate was washed with distilled water until neutral, dried in an oven at 80°C for 12 hours, then baked in a muffle furnace at 650°C for 4 hours, cooled naturally to room temperature, and ground with a mortar to prepare acid-activated montmorillonite.

[0040] 2. Preparation of monoethanolamine intramolecular dehydration catalyst

[0041] Using equal volume impregnation method, according to Cs 3.0 P 2.4 PR 1.5 o 19.5 The stoichiometric ratio of 0.25g cesium nitrate, 0.38g praseodymium nitrate hexahydrate, and 0.14g diammonium hydrogen phosphate were added to deionized water, and left to stand for 15 minutes to obtain an impregnation solution; according to Cs 3.0 P 2.4 PR 1.5 o 19.5 ...

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Abstract

The invention discloses a monoethanolamine intramolecular dehydration catalyst. The carrier of the catalyst is acid activation montmorillonite. The active component of the catalyst is CsXY<c>O<d>, wherein X is phosphorus element, iron element or boron element, Y is rare earth element, O is oxygen element, a, b, c and d are the molar ratios of Cs, X, Y and O, and when a=1, b=0.5-2, c=0.2-1, and d is determined based on a, b and c. The acidity of the catalyst is regulated by means of the acid activation montmorillonite and phosphides, iron compounds or borides, the alkalinity of the catalyst is regulated by means of the rare earth element and Cs, the obtained catalyst is used for monoethanolamine intramolecular dehydration reaction to synthetize aziridine, and the conversion rate of monoethanolamine and the selectivity of aziridine can be improved at the same time.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular relates to a catalyst for synthesizing aziridine through intramolecular dehydration of monoethanolamine. Background technique [0002] The molecular formula of aziridine is: C 2 h 5 N, also known as ethyleneimine, aziridine, aziridine and ethyleneimine, is an important intermediate in organic synthesis and is widely used in the preparation of anti-cancer drugs, insecticides, reactive dyes, etc. [0003] The initial industrial production method of aziridine is a liquid phase method, and monoethanolamine is used as a raw material to obtain aziridine through intramolecular dehydration reaction. The reaction equation is as follows: [0004] [0005] A large amount of concentrated sulfuric acid and concentrated alkali are required in this reaction, the cost is high, the yield is low, and a large amount of inorganic salt by-products with low utilization value are generated. Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/18B01J23/10B01J23/83B01J35/10C07D203/02C07D203/08
Inventor 刘忠文黄贵秋吕剑侯艳霞刘昭铁杨建明
Owner XIAN MODERN CHEM RES INST
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