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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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the yield of the catalyst within 3 hours is only 68.3%

Method used

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

Examples

Experimental program
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Example Embodiment

[0034]Example 1

[0035](1) Nitrification reaction

[0036]Taking diphenyl ether as a reaction substrate, 70 wt% nitric acid is nitrate and solvent, with a total flu fluorosulfonic acid resin as a catalyst, wherein the mass ratio of diome ether, nitric acid and perfluorosulfonic acid resin is 1: 10: 0.1, The reaction was stirred at 30 ° C, 1 atm, and the reaction was stirred at 40 ° C, 1 atm, and the reaction was stirred at 50 ° C, 1 atm.

[0037](2) Hot filtration

[0038]The mixture obtained at 65 ° C was centrifuged, and the obtained filter perfluorosulfonic acid resin catalyst was recovered for the next batch reaction, evaporating the resulting filtrate and evaporated. Nitric acid with 80% sulfuric acid. Distillation was carried out, the distillate component was collected, and 99 wt% concentrated nitric acid was collected, and the air was passed into the air, lasting 5 min, and the nitric acid after regeneration was obtained for the next batch nitrification reaction.

[0039](3) Catalytic hydr...

Example Embodiment

[0042]Example 2

[0043](1) Nitrification reaction

[0044]Taking diphenyl ether as a reaction substrate, 70 wt% nitric acid is nitrate and solvent, with a total flu fluorosulfonic acid resin as a catalyst, wherein the mass ratio of diome ether, nitric acid and perfluorosulfonic acid resin is 1: 10: 0.1, The reaction was stirred at 30 ° C, 1 atm, and the reaction was stirred at 40 ° C, 1 atm, and the reaction was stirred at 50 ° C, 1 atm.

[0045](2) Hot filtration

[0046]The mixture obtained at 75 ° C was centrifuged, and the obtained filtrate perfluorosulfonic acid resin catalyst was recovered for the next batch reaction, and the resulting filtrate was evaporated and concentrated. The evaporated nitric acid was mixed with 80% sulfuric acid. Distillation was carried out, the distillate component was collected, and 99 wt% concentrated nitric acid was collected, and the air was passed into the air, lasting 5 min, and the nitric acid after regeneration was obtained for the next batch nitrificati...

Example Embodiment

[0050]Example 3

[0051](1) Fluorosulfonic acid resin catalyst pretreatment

[0052]The perfluorosulfonic acid resin was placed in an ethanol-aqueous solution, and the mixture was stirred at 55 ° C for 2 h, then stirred in an argon atmosphere, stirred 40 hours under 35 MPa, and dissolved with tetrachloride. The lower extract was added to the sodium silicate solution, aged 1.5 h, 95 ° C drying 24 h, and crushed the perfluorosulfonic acid resin catalyst.

[0053](2) Nitrification reaction

[0054]The binnyl ether is a reaction substrate, with 99 wt% nitric acid is nitrate and solvent, with a perfluorosulfonic acid resin as a 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, 1 atm, and the reaction was stirred at 45 ° C, 1 atm, and the reaction was stirred at 65 ° C, 1.5 atm.

[0055](3) Hot filtration

[0056]The mixture obtained at 70 ° C was centrifuged, and the obtained filter perfluorosulfonic acid re...

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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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