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Preparation method of diamino diphenyl ether

A technology of diaminodiphenyl ether and aromatic ether, which is applied in the field of preparation of fine chemicals, can solve the problems of not meeting the demand for nitration of diphenyl ether, and achieve the effect of less three wastes, low cost, and reduced loss

Active Publication Date: 2021-06-01
泰兴中科艾德膜材料科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the yield of the catalyst within 3 hours is only 68.3%, which is far below the requirement of diphenyl ether nitration

Method used

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  • Preparation method of diamino diphenyl ether
  • Preparation method of diamino diphenyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) Nitrification reaction

[0036] With diphenyl ether as reaction substrate, with 70wt% nitric acid as nitrating agent and solvent, with perfluorosulfonic acid resin as catalyst, wherein the mass ratio of diphenyl ether, nitric acid and perfluorosulfonic acid resin is 1:10:0.1, The reaction was stirred at 30° C. and 1 atm for 0.5 h, at 40° C. and 1 atm for 0.5 h, and at 50° C. and 1 atm for 1 h.

[0037] (2) hot filter

[0038] Centrifuge the mixture obtained in step (1) at 65°C, recover the perfluorosulfonic acid resin catalyst obtained from the filter for the next batch of reactions, evaporate and concentrate the obtained filtrate, and mix the evaporated nitric acid with 80% sulfuric acid Carry out distillation, collect distilled components, obtain 99wt% concentrated nitric acid, pass air into it, continue 5min, obtain the nitric acid after regeneration, be used for the next batch of nitration reaction.

[0039] (3) Catalytic hydrogenation

[0040] Dilute the pro...

Embodiment 2

[0043] (1) Nitrification reaction

[0044] With diphenyl ether as the reaction substrate, with 70wt% nitric acid as nitrating agent and solvent, with perfluorosulfonic acid resin as catalyst, wherein the mass ratio of diphenyl ether, nitric acid and perfluorosulfonic acid resin is 1:10:0.1, The reaction was stirred at 30° C. and 1 atm for 0.5 h, at 40° C. and 1 atm for 0.5 h, and at 50° C. and 1 atm for 1 h.

[0045] (2) hot filter

[0046] Centrifuge the mixture obtained in step (1) at 75°C, recover the perfluorosulfonic acid resin catalyst obtained from the filter for the next batch of reactions, evaporate and concentrate the obtained filtrate, and mix the evaporated nitric acid with 80% sulfuric acid Carry out distillation, collect distilled components, obtain 99wt% concentrated nitric acid, pass air into it, continue 5min, obtain the nitric acid after regeneration, be used for the next batch of nitration reaction.

[0047] (3) Catalytic hydrogenation

[0048] Dilute the p...

Embodiment 3

[0051] (1) Perfluorosulfonic acid resin catalyst pretreatment

[0052] Put the perfluorosulfonic acid resin in the ethanol-water solution, first stir the mixture at 55°C for 2h, then stir and dissolve it at 135°C and 35MPa for 40 hours in an argon atmosphere, and extract the solution with carbon tetrachloride. The extract from the lower layer was added to the sodium silicate solution, aged for 1.5 hours, dried at 95°C for 24 hours, and ground to obtain a perfluorosulfonic acid resin catalyst.

[0053] (2) Nitrification reaction

[0054] With diphenyl ether as reaction substrate, 99wt% nitric acid as nitrating agent and solvent, perfluorosulfonic acid resin as catalyst, wherein the mass ratio of diphenyl ether, nitric acid and perfluorosulfonic acid resin is 1:5:0.001, The reaction was stirred at 30° C. and 1 atm for 0.5 h, at 45° C. and 1 atm for 0.5 h, and at 65° C. and 1.5 atm for 1 h.

[0055] (3) hot filter

[0056] Centrifuge the mixture obtained in step (1) at 70°C, r...

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Abstract

The invention provides a preparation method of diaminodiphenyl ether. The method comprises the following steps: under the catalysis of solid acid, mixing aromatic ether and nitric acid for nitration reaction; carrying out hot filtration on the nitration reaction product, recovering the filtrate, and carrying out post-treatment on the filtrate; and reducing the filtrate subjected to post-treatment to obtain the diamino diphenyl ether. According to the invention, the requirement of nitration reaction on the concentration of nitric acid is greatly reduced, the yield of the diamino diphenyl ether is increased, and the preparation process is environmentally friendly, efficient and low in cost.

Description

technical field [0001] The invention relates to a preparation method of fine chemicals, in particular to a preparation method of diaminodiphenyl ether. Background technique [0002] Diaminodiphenyl ether is an important monomer for the synthesis of polyimide special materials. 4,4'-diaminodiphenyl ether has been produced in industrialized production facilities. With the deepening of the research, it was found that the polyimide products obtained by using mixed, isomeric diacid or diamine monomers for polymerization showed higher heat dissipation compared with symmetric and homopolymers. properties and mechanical properties. The present invention adopts a one-step nitration method to obtain a diamine monomer mixture at an isomeric position for polymerization with dianhydride, and can obtain a polyimide product with excellent performance. [0003] The nitration of diphenyl ether mostly adopts mixed acid method and nitric acid nitration method. For the mixed acid method, it...

Claims

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Application Information

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IPC IPC(8): C07C201/08C07C205/38C07C213/02C07C217/90B01J31/10
CPCC07C201/08C07C213/02B01J31/10C07C205/38C07C217/90
Inventor 梅雪杜庶铭孟天颢王贺王琪王文宾
Owner 泰兴中科艾德膜材料科技有限公司
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