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Morpholine synthetic catalyst and preparation method thereof

A catalyst and morpholine technology, which are applied to the catalyst for synthesizing morpholine by the low-pressure catalytic ammonia decyclization method of diethylene glycol and the field of preparation thereof, can solve the problems of low preparation cost and high use pressure conditions, and achieve the increase of specific surface and the reduction of use effect of stress

Inactive Publication Date: 2013-07-24
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The advantage of the catalyst of this invention is that non-precious metals are used as active components and the traditional co-precipitation preparation method, the preparation cost is low, but its operating pressure is 1.0-2.4MPa, and the operating pressure condition is relatively high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0007] 80 mesh Al 2 o 3 Roast at 750°C for 6 hours, cool to room temperature to obtain a pre-activated carrier; prepare a nitrate mixed solution with a concentration of 2mol / L according to the molar ratio of copper: nickel: zinc: lanthanum = 1: 1.4: 1.3: 0.02, and place it at 60°C Add the sodium carbonate solution of 1.8mol / L down to make pH=10, react for 3 hours; After the reactant is filtered and washed, add 25% pre-activated carrier that accounts for the total amount of catalyst to support for 40 minutes, then wash and filter the filter cake; filter cake Dried at 130°C, then calcined at 450°C for 4 hours, and cooled naturally to room temperature to obtain a morpholine catalyst. After the catalyst is reduced and activated by hydrogen, when used at a temperature of 215°C and a pressure of 1.0 MPa, the conversion rate of diethylene glycol is 99.7%, and the selectivity of morpholine is 99.5%.

Embodiment 2

[0009] 100 mesh Al 2 o 3 Roasting at 800°C for 5 hours, cooling to room temperature to obtain a preactivated carrier; preparing a nitrate mixed solution with a concentration of 2.3mol / L at 70 Add 2mol / L sodium carbonate solution at ℃ to make pH=10, and react for 2 hours; after the reactant is filtered and washed, add 30% of the total amount of catalyst to support the carrier for 30 minutes, then wash and filter out the filter cake; filter the cake Dried at 120°C, then calcined at 430°C for 5 hours, and cooled naturally to room temperature to obtain a morpholine catalyst. After the catalyst is reduced and activated by hydrogen, when the catalyst is used at a temperature of 220°C and a pressure of 0.8 MPa, the conversion rate of diethylene glycol is 99.6%, and the selectivity of morpholine is 99.4%.

Embodiment 3

[0011] 150 mesh Al 2 o 3 Roast at 850°C for 5 hours, cool to room temperature to obtain a pre-activated carrier; prepare a nitrate mixed solution with a concentration of 2mol / L according to the molar ratio of copper: nickel: zinc: lanthanum = 1: 1.3: 1.4: 0.08, and place it at 60°C Add the sodium carbonate solution of 2mol / L down to make pH=10, react for 3 hours; After the reactant is filtered and washed, add and account for 30% pre-activated carrier loading of the total amount of catalyst for 30 minutes, then wash and filter out the filter cake; filter the cake in Dried at 130°C, then calcined at 460°C for 3 hours, and cooled naturally to room temperature to obtain a morpholine catalyst. After the catalyst is reductively activated by hydrogen, when used at a temperature of 210° C. and a pressure of 0.7 MPa, the conversion rate of diethylene glycol is 99.1%, and the selectivity of morpholine is 99.0%.

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Abstract

The invention relates to a morpholine synthetic catalyst by diethylene glycol-ammoniation under low pressure and a preparation method of the catalyst. The catalyst uses Al2O3 as a carrier for loading active components Ni, Cu and Zn, and an additive La is added. The concrete preparation method comprises the following steps: adding nickel, copper, zinc, and lanthanum into a nitrate solution in accordance with a certain concentration, so as to prepare a nitrate mixture solution with the weight of the lanthanum accounting for 0.2%-2.5% of the weight of nitrates; adding a sodium carbonate solution into the nitrate mixture solution to carry out the precipitation reaction; and filtering and cleaning the reaction precipitates, adding the pre-activated carrier Al2O3 which is fired at high temperature, into the filtered and cleaned reaction precipitates, cleaning, filtering, drying and firing the precipitates with the carrier, so as to prepare the morpholine catalyst. The judgment shows that the using pressure of the catalyst is reduced from 1.0-2.3MPa to 0.3-1.0MPa after the lanthanum is added into the catalyst, and the production difficulty of morpholine is greatly reduced.

Description

technical field [0001] The invention belongs to the field of catalyst preparation technology and fine chemical engineering in chemical engineering and technology, and in particular relates to a catalyst for synthesizing morpholine by a low-pressure catalytic ammonolysis cyclization method of diethylene glycol and a preparation method thereof. Background technique [0002] Morpholine, also known as 1,4-oxazidine, is a raw material for the production of many fine chemical products and is widely used in the fields of pesticides, medicines, dyes, rubber and coatings. The existing technology is improved to prepare a catalyst with excellent performance, which can reduce energy consumption and cost in the morpholine production process. Diethylene glycol catalyzed ammonolysis and cyclization method is the main morpholine synthesis process route at home and abroad. This method uses a hydrogenation catalyst. Diethylene glycol can react with ammonia water or liquid ammonia to obtain mo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/83C07D295/023C07D295/027
Inventor 童张法闵楠韦藤幼廖丹葵邓红黄世勇
Owner GUANGXI UNIV