Catalyst for synthesizing morphine through diethylene glycol ammoniation, and preparation method

A diethylene glycol ammonia and catalyst technology, applied in the direction of physical/chemical process catalysts, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problems of expensive, three waste pollution, unsatisfactory, etc. problem, to achieve the effect of easy product separation and purification, excellent selectivity, and low preparation cost

Inactive Publication Date: 2007-02-21
GUANGXI UNIV
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  • Summary
  • Abstract
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AI Technical Summary

Problems solved by technology

Diethanolamine strong acid dehydration method is basically out of use at present due to the high price of raw materials and serious pollution of three wastes
[0007] From the above retrieval results, it is understood that the public documents mainly introduce: although document ① uses relatively cheap active ingredients, the catalytic effect is not ideal; although documents ② and ③ have good catalytic effects, the active components use precious metal cobalt and The preparation process is complex; although literature ④ also uses relatively cheap active ingredients, due to the use of Al(OH) 3 carrier, unsatisfactory catalytic performance
In summary, the synthesis of morpholine catalysts is not yet ideal

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] 80 mesh Al 2 o 3 ·3H 2 O was roasted at 750°C for 8 hours, and naturally cooled to room temperature to obtain a pre-activated carrier; a nitrate mixed solution with a concentration of 2mol / L was prepared according to the molar ratio of copper: nickel: zinc = 1: 1.4: 1.3, and the nitrate mixed solution was prepared at 60°C Add 2mol / L of sodium carbonate to dissolve and make pH=11, and react for 3 hours; after the reactant is filtered and washed, add 25% of the total amount of catalyst to pre-activate the carrier for loading for 1 hour, then wash and filter the filter cake; put the filter cake in Dry at 130°C, then calcined at 450°C for 4 hours, and cool down to room temperature naturally to obtain a morpholine catalyst.

Embodiment 2

[0015] 100 mesh Al 2 o 3 ·3H 2 O was roasted at 800°C for 7 hours, and naturally cooled to room temperature to obtain a pre-activated carrier; according to the molar ratio of copper: nickel: zinc = 1: 1.3: 1.3, a mixed solution of nitrate with a concentration of 2.5mol / L was prepared and stored at 70°C Add 2mol / L of sodium carbonate solution to make pH=11, and react for 2 hours; after the reactant is filtered and washed, add 30% of the total amount of the catalyst to support the carrier for 0.5 hour, then wash and filter the filter cake; filter the cake Dried at 120°C, then calcined at 430°C for 4 hours, and cooled naturally to room temperature to obtain a morpholine catalyst.

Embodiment 3

[0017] 150 mesh Al 2 o 3 ·3H 2 O was roasted at 850°C for 5 hours, and naturally cooled to room temperature to obtain a preactivated carrier; a nitrate mixed solution with a concentration of 2mol / L was prepared according to the molar ratio of copper: nickel: zinc = 1: 1.3: 1.4, and the mixture was prepared at 60°C Add 2mol / L of sodium carbonate to dissolve and make pH=10, and react for 3 hours; after the reactant is filtered and washed, add 30% of the total amount of the catalyst to pre-activate the carrier for loading for 0.5 hour, then wash and filter the filter cake; filter the cake in Dry at 130°C, then bake at 420°C for 5 hours, and cool down to room temperature naturally to obtain a morpholine catalyst.

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PUM

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Abstract

A catalyst for preparing morpholine from diglycol by ammoniation is prepared from Al2O3.3H2O as carrier and the Cu, Ni and Zn as active component through high-temp calcining of Al2O3.3H2O to obtain the pre-activated carrier, preparing the mixed nitrate solution of Cu, Ni and Zn proportionally, depositing reaction in the solution of sodium carbonate, filtering, washing, adding said pre-activated carrier, washing, filtering, drying, and calcining.

Description

technical field [0001] The invention relates to a catalyst preparation technology in chemical engineering, in particular to a catalyst for diethylene glycol ammoniation to synthesize morpholine and a preparation method thereof. Background technique [0002] Morpholine, also known as 1,4-oxazidine, is an important fine chemical, mainly used in rubber accelerators, vulcanizing agents, corrosion inhibitors, anti-scaling agents, pharmaceutical surfactants and textile printing and dyeing auxiliaries raw materials. The synthetic methods of morpholine mainly fall into two categories, one is diethanolamine strong acid dehydration method, and the other is diethylene glycol ammoniation method. The diethanolamine strong acid dehydration method is basically out of use at present due to the high price of raw materials and serious pollution of three wastes. The diethylene glycol ammonification method uses the petrochemical by-product diethylene glycol as raw material, synthesized by cat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/80B01J23/755B01J23/72C07D295/023
Inventor 童张法韦藤幼廖丹葵曾宪化
Owner GUANGXI UNIV
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