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Preparation method of 4, 4 '-diaminodiphenyl ether

A technology of diaminodiphenyl ether and dinitrodiphenyl ether, which is applied in the field of preparation of 4,4'-diaminodiphenyl ether, can solve the problem that hydrazine hydrate is expensive, highly corrosive, highly toxic, diaminodiphenyl ether The problems of low ether yield and high requirements for reaction equipment can achieve the effects of high-efficiency photocatalytic reduction, avoiding synthesis conditions, and high-efficiency stability.

Pending Publication Date: 2021-12-14
SHANDONG ENERGY GRP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the yield of 4,4'-diaminodiphenyl ether prepared by iron powder reduction method, stannous chloride-hydrochloric acid reduction method and alkali sulfide reduction method is very low, and the production process needs to add concentrated hydrochloric acid or alkali sulfide aqueous solution, and produce A large amount of waste liquid and waste residue; although the yield of the hydrazine hydrate reduction method is above 90%, the hydrazine hydrate used is expensive and has strong corrosion and toxicity
At present, the catalytic hydrogenation method commonly used in industry mainly relies on noble metal Pd, Pt modified catalysts, such as Pd / C or Pt / C, which need to be fed with high-pressure pure H 2 As a reducing agent, it requires high-temperature reaction conditions and requires high reaction equipment, which greatly increases production costs.

Method used

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  • Preparation method of 4, 4 '-diaminodiphenyl ether
  • Preparation method of 4, 4 '-diaminodiphenyl ether
  • Preparation method of 4, 4 '-diaminodiphenyl ether

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preparation example Construction

[0024] Aiming at the problems of unenvironmental protection, high price or high production cost of the catalyst in the preparation process of 4,4'-diaminodiphenyl ether in the prior art, this application provides a clean, environmentally friendly, stable, efficient and green economical 4,4' -The preparation method of diaminodiphenyl ether, specifically, the embodiment of the present invention discloses a preparation method of 4,4'-diaminodiphenyl ether, comprising:

[0025] Under the catalysis of twinned zinc cadmium sulfide, 4,4'-dinitrodiphenyl ether and water undergo photocatalytic hydrogenation reaction to obtain 4,4'-diaminodiphenyl ether.

[0026] The preparation of 4,4'-diaminodiphenyl ether in this application is to use photocatalytic means, by selecting twin crystal zinc cadmium sulfide solid solution as the photocatalyst, using 4,4'-dinitrodiphenyl ether as raw material, without the need Access to extra H 2 Under conditions, water is used as a solvent to provide hyd...

Embodiment 1

[0037] Prepare 30vol% ethanol aqueous solution: add 30mL absolute ethanol to 70mL water, and ultrasonically make it form a homogeneous solution; ② Add 5 μmol 4,4'-dinitrodiphenyl ether reaction raw materials to the 30vol% ethanol aqueous solution in step ①, 10mg twinned Zn 0.7 Cd 0.3 S catalyst, add 0.1mol L to the system -1 HCl regulates the pH of the reaction system to 2.12, and stirs for 30 minutes; ③ Seal the reactor and pass in an inert gas N 2 30min, exhaust the air in the reactor; ④ 300W xenon lamp injects visible light with a wavelength ≥ 420nm into the reactor through the top-illumination type, the reactor temperature is controlled by water circulation and condensation to 15°C, and after 40min of reaction, samples are taken and quantified by high-performance liquid chromatography, of which 4, The conversion rate of 4'-dinitrodiphenyl ether is >99%, the product yield of 4,4'-diaminodiphenyl ether is >99%, and good stability and product yield are still maintained aft...

Embodiment 2

[0042] Steps ①, ②, and ④ of this embodiment are the same as in Example 1, the difference is: step ③: seal the reactor, feed inert gas argon for 30 minutes, and discharge the air in the reactor. After 40 minutes of reaction, samples were taken and quantified by high-performance liquid chromatography, wherein the conversion rate of 4,4'-dinitrodiphenyl ether was >99%, the yield of 4,4'-diaminodiphenyl ether was >99%, and the reaction cycle was 5 times After that, good stability and product yield were still maintained.

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Abstract

The invention provides a preparation method of 4, 4 '-diaminodiphenyl ether, which comprises the following step: under the catalytic action of twin-crystal zinc cadmium sulfide, carrying out photocatalytic hydrogenation reaction on 4, 4'-dinitrodiphenyl ether and water to obtain the 4, 4 '-diaminodiphenyl ether. In the process of preparing 4, 4 '-diaminodiphenyl ether, the reaction conditions are carried out at normal temperature and normal pressure, extra hydrogen is not needed in the reaction process, the 4, 4'-dinitrodiphenyl ether is completely converted within 40 minutes by regulating and controlling the zinc and cadmium content of the twin crystal zinc cadmium sulfide catalyst, the ethanol concentration and the acid-base property of the system, the yield of the 4, 4 '-diaminodiphenyl ether is up to 99%, and the catalyst keeps good stability.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a preparation method of 4,4'-diaminodiphenyl ether. Background technique [0002] As a special engineering material, polyimide has been widely used in the fields of aviation, aerospace, microelectronics, nanometer, liquid crystal, separation membrane and laser. In the 1960s, all countries listed the research, development and utilization of polyimide as one of the most promising engineering plastics in the 21st century. Whether it is used as a structural material or as a functional material, its huge application prospects have been fully recognized, and it is believed that "without polyimide, there would be no microelectronics technology today." [0003] 4,4'-diaminodiphenyl ether is an important intermediate in the synthesis of polyimide, which can increase the flexibility of polyimide polymer chains and improve its thermal stability. In addition, 4,4'-diaminodiphenyl Et...

Claims

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Application Information

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IPC IPC(8): C07C213/02C07C217/90B01J27/04
CPCC07C213/02B01J27/04B01J35/39C07C217/90
Inventor 李希友胡玉佳刘昭斌李智于贵阳韩嘉张奎同
Owner SHANDONG ENERGY GRP
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