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Catalyst for preparing 4, 4'-diaminodiphenyl ether, preparation method and application of catalyst

A technology of diaminodiphenyl ether and dinitrodiphenyl ether, applied in the field of fine organic product synthesis, can solve the problems of high cost, easy carbon deposition, environmental pollution, etc., and achieve industrial batch production, high conversion rate and production efficiency rate effect

Inactive Publication Date: 2013-02-27
JIANGSU HUALUN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among the existing 4,4'-dinitrodiphenyl ether hydrogenation catalysts, precious metal catalysts such as supported catalysts such as platinum and platinum have high benzene hydrogenation activity, but the cost is high and easy to deposit carbon; while the Raney nickel catalyst Due to the use of a large amount of caustic soda to extract aluminum during preparation, it will cause serious environmental pollution, and there is also the problem of separation of catalyst slurry and product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 1. Preparation of catalyst: 12.3g of Ni(NO 3 ) 2 ·6H 2 O and 4.7g of Cu(NO 3 ) 2 ·3H 2 O is completely dissolved in a certain amount of deionized water to form a mixed aqueous solution of nitrate, and then 21.3g of -Al 2 o 3 Pour into the prepared nitrate mixed aqueous solution to form equal volume impregnation. The mixture was dried in an oven at 100°C for 12 hours, then calcined at 350°C for 3 hours under a nitrogen atmosphere, and finally heated in H 2 -N 2 (H 2 and N 2 The molar ratio is 3:7) and reduced at 300°C for 1 hour in a mixed atmosphere to obtain Ni-Cu / -Al 2 o 3 Catalyst, wherein weight percent is Ni: 10%, Cu: 5%, -Al 2 o 3 : 85%.

[0020] 2. Production of 4,4'-diaminodiphenyl ether: Add 250mL of 1,2-dichloroethane as a reaction solvent into a 500mL autoclave, and then add 100g of raw material 4,4'-dinitrodiphenyl Phenyl ether and 1g of the above-mentioned catalyst were added to the kettle, and the autoclave was purged with nitrogen fo...

Embodiment 2

[0022] 1. Preparation of catalyst: 18.5g of Ni(NO 3 ) 2 ·6H 2 O and 21.4g of Mg(NO 3 ) 2 ·6H 2 O is completely dissolved in a certain amount of deionized water to form a mixed aqueous solution of nitrate, and then 19.3g of -Al 2 o 3 Pour into the prepared nitrate mixed aqueous solution to form equal volume impregnation. The mixture was dried in an oven at 110°C for 15 hours, then calcined at 450°C for 4 hours under a nitrogen atmosphere, and finally heated in H 2 -N 2 (H 2 and N 2 The molar ratio is 3:7) and reduced at 400°C for 2 hours in a mixed atmosphere to obtain Ni-Mg / -Al 2 o 3 Catalyst, wherein weight percent is 15% Ni, 8% Mg and 77% -Al 2 o 3 .

[0023] 2. Production of 4,4'-diaminodiphenyl ether: Add 250mL of 1,2-dichloroethane as a reaction solvent into a 500mL autoclave, and then add 100g of raw material 4,4'-dinitrodiphenyl Phenyl ether and 1.5g of the above-mentioned catalyst were added to the autoclave, and the autoclave was purged with nitr...

Embodiment 3

[0025] 1. Preparation of catalyst: 24.7g of Ni(NO 3 ) 2 ·6H 2 O and 19.2g of Cr(NO 3 ) 3 9H 2 O was completely dissolved in a certain amount of deionized water to form a nitrate mixed aqueous solution, and then 17.5 g of activated carbon was poured into the prepared nitrate mixed aqueous solution to form an equal-volume impregnation. The mixture was dried in an oven at 120°C for 24 hours, then calcined at 500°C for 5 hours under a nitrogen atmosphere, and finally heated in H 2 -N 2 (H 2 and N 2 The molar ratio is 3:7) and reduced at 450°C for 3 hours in a mixed atmosphere to obtain a Ni-Cr / activated carbon catalyst, in which the weight percentage is 20% Ni, 10% Cr and 70% activated carbon.

[0026] 2. Production of 4,4'-diaminodiphenyl ether: Add 250mL of 1,2-dichloroethane as a reaction solvent into a 500mL autoclave, and then add 100g of raw material 4,4'-dinitrodiphenyl Phenyl ether and 2.0g of the above catalyst were added to the kettle, and the autoclave was purg...

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PUM

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Abstract

The invention discloses a catalyst for preparing 4, 4'-diaminodiphenyl ether, a preparation method and application of the catalyst, and relates to a fine organic product synthesis method. Firstly, carriers are impregnated in nitrate mixed water solution to form mixture, and the mixture is dried in a drying oven and then roasted in nitrogenous atmosphere. Secondly, roasted solid is reduced in H2 and N2 mixed atmosphere to manufacture the catalyst comprising 10%-30% of elementary nickel, 5%-10% of other metal elementary substances except for the nickel and 60%-85% of carriers, and the catalyst is used for producing the 4, 4'-diaminodiphenyl ether. The catalyst is low in production cost and simple to operate, and is a supported nickel-based catalyst needed for preparing the high-yield 4, 4'-diaminodiphenyl ether from 4, 4'-dinitrodiphenyl ether by means of catalytic hydrogenation.

Description

technical field [0001] The invention relates to a method for synthesizing fine organic products, and belongs to a catalyst for preparing 4,4'-diaminodiphenyl ether by catalytic hydrogenation of 4,4'-dinitrodiphenyl ether and a preparation method thereof. Background technique [0002] 4,4'-diaminodiphenyl ether is a fine organic product with high added value. It is a new engineering material polyimide, polyamide resin, polymaleimide, polyamide-polyimide One of the important raw materials for heat-resistant high-temperature insulating resin polymer materials such as resin and polyester-polyimide resin. It can also be used as a raw material and crosslinking agent for high molecular compounds such as heat-resistant epoxy resin and polyurethane. At the same time, it is also used to replace the carcinogenic benzidine to produce azo dyes, reactive dyes and spices and other industries. At present, diamines are used as raw materials, and direct dyes with different color levels such...

Claims

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Application Information

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IPC IPC(8): B01J23/755B01J23/86C07C217/90C07C213/02
Inventor 丁建飞吴义彪陈忠平李冬春许飞
Owner JIANGSU HUALUN CHEM
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