Acid-activated montmorillonite cesium-loaded catalyst and application thereof in catalytic synthesis of aziridine from monoethanolamine

A technology of montmorillonite and acid activation, applied in physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, organic chemistry, etc., can solve the problem of affecting the selectivity of aziridine products and the conversion of high monoethanolamine efficiency, aziridine selectivity reduction and other issues, to achieve the effect of improving the diffusion effect, increasing the selectivity, and increasing the conversion rate

Active Publication Date: 2015-12-02
XIAN MODERN CHEM RES INST +1
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  • Summary
  • 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 current patents only use phosphide or boride to adjust the acidity. While the conversion rate is increased, the selectivity is greatly reduced, and it is difficult to obtain a high conversion rate of monoethanolamine and aziridine at the same time.

Method used

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  • Acid-activated montmorillonite cesium-loaded catalyst and application thereof in catalytic synthesis of aziridine from monoethanolamine

Examples

Experimental program
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Effect test

Embodiment 1

[0026] 1. Preparation of acid-activated montmorillonite

[0027] 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 .

[0028] 2. Preparation of acid-activated montmorillonite-supported cesium catalyst

[0029] Using equal volume impregnation method, according to Cs 1 P 0.8 o 7 The stoichiometric ratio, 0.26g cesium nitrate, 0.22g ammonium phosphate trihydrate were added to deionized water, and left to stand for 15 minutes to obtain the impregnation solution; according to Cs 1 P 0.8 o 7 The loading capacity is 18%. Add 2.0g acid-activated montm...

Embodiment 2

[0031] In steps 1 and 2 of Example 1, the calcination temperature was changed to 850°C, and the other steps were the same as in Example 1 to prepare an acid-activated montmorillonite-loaded cesium catalyst with a specific surface area of ​​15.96m 2 / g, the pore volume is 0.042cm 3 / g, the average pore diameter is 23.23nm.

Embodiment 3

[0033] In steps 1 and 2 of Example 1, the calcination temperature was changed to 800°C, and the other steps were the same as in Example 1 to prepare an acid-activated montmorillonite-loaded cesium catalyst with a specific surface area of ​​20.78m 2 / g, the pore volume is 0.052cm 3 / g, the average pore diameter is 19.80nm.

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Abstract

The invention discloses an acid-activated montmorillonite cesium-loaded catalyst and an application of the acid-activated montmorillonite cesium-loaded catalyst in catalytic synthesis of aziridine from monoethanolamine. A carrier for the catalyst is acid-activated montmorillonite, and the composition of active components is CsaXbOc, wherein X is phosphorus, iron or boron element, O is oxygen element, a, b and c are molar ratios of Cs, X and O, when a is equal to 1, b is equal to 0.5-1.5, and the value of c depends on a and b. A preparation method of the catalyst comprises the step of loading the active components by using an equivalent-volume impregnation method after acid-activated treatment of the montmorillonite. The method is simple, and the conditions are controllable. According to the acid-activated montmorillonite cesium-loaded catalyst, and the application and the preparation method of the catalyst disclosed by the invention, the acidity of the catalyst is adjusted by utilizing the acid-activated montmorillonite, and the obtained catalyst is used for synthesis of aziridine by monoethanolamine intramolecular dehydration reaction, improves the conversion rate of the monoethanolamine, and also maintains high selectivity of the product aziridine simultaneously.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular relates to a catalyst for catalyzing the synthesis of aziridine from 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. Therefore, the gas-s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/18B01J23/78B01J23/04C07D203/08C07D203/02
Inventor 刘忠文吕剑黄贵秋刘昭铁杨建明侯艳霞
Owner XIAN MODERN CHEM RES INST
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