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Preparation method of 4,4'-(hexafluoroisopropylene)diphthalic anhydride

A technology of hexafluoroisopropene and diphthalic anhydride, which is applied in the field of material preparation, can solve the problems of high energy consumption in the reaction process, difficult separation of metal ions, cumbersome reaction steps, etc., to avoid the use of metal ions, fewer synthesis steps, and high selective effect

Active Publication Date: 2019-06-25
自贡中天胜新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method is a brand-new solution, which solves the problem of low product yield, low purity, cumbersome reaction steps, strong hygroscopicity, high energy consumption in the reaction process, difficult separation of metal ions in the reaction process, large amount of solvent, and high temperature and high pressure reaction. Insecurity and many other issues

Method used

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  • Preparation method of 4,4'-(hexafluoroisopropylene)diphthalic anhydride
  • Preparation method of 4,4'-(hexafluoroisopropylene)diphthalic anhydride
  • Preparation method of 4,4'-(hexafluoroisopropylene)diphthalic anhydride

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Embodiment 1

[0040] A kind of preparation method of 4,4'-(hexafluoroisopropylene) diphthalic anhydride, it comprises the following steps:

[0041] First, 100g of granular 4,4'-(hexafluoroisopropenyl)-di-o-xylene (6-FXP) is pulverized and dispersed with 20g of water in a wet nano-grinding disperser; the power of the nano-wet pulverizer is 12KW , The fineness of the crushed material is about 80nm.

[0042] Take 100g of dispersed nano-scale 4,4'-(hexafluoroisopropenyl)-di-o-xylene (6-FXP) and 120g of aqueous hydrogen peroxide solution with a mass concentration of 80% and add them into the photoreactor for uniform dispersion. Then 10°C, normal pressure, turn on 2Kw LED cold ultraviolet light with a wavelength of 380nm, and the ultraviolet light power ultraviolet light induces the light source to irradiate the reaction solution for 2 hours, then heat to 55°C for 4.2 hours, and then filter the reaction solution with a nano-membrane filter, the pore size of the nano-membrane filter is 12nm, afte...

Embodiment 2

[0047] A kind of preparation method of 4,4'-(hexafluoroisopropylene) diphthalic anhydride, it comprises the following steps:

[0048] First, 100 g of granular 4,4'-(hexafluoroisopropenyl)-di-o-xylene (6-FXP) was pulverized and dispersed with 200 g of water in a wet nano-grinding disperser. The power of the nano wet pulverizer is 12KW, and the fineness of the pulverized material is about 80nm.

[0049] Take 100g of dispersed nano-scale 4,4'-(hexafluoroisopropenyl)-di-o-xylene (6-FXP) and 48g of aqueous hydrogen peroxide solution with a mass concentration of 80% and add them to the photoreactor for uniform dispersion. Then -6°C, normal pressure, turn on 2Kw LED cold ultraviolet light with a wavelength of 320nm, and the ultraviolet light power ultraviolet light induces the light source to irradiate the reaction solution for 2.5h, and then heat to 50°C for 12h oxidation reaction, and the reaction solution is covered with a nano-film Filtrate through a filter, and after cooling to...

Embodiment 3

[0052] A kind of preparation method of 4,4'-(hexafluoroisopropylene) diphthalic anhydride, it comprises the following steps:

[0053] First, 100 g of granular 4,4'-(hexafluoroisopropenyl)-di-o-xylene (6-FXP) was pulverized and dispersed with 200 g of water in a wet nano-grinding disperser. The power of the nano wet pulverizer is 15KW, and the fineness of the pulverized material is about 80nm.

[0054] Take 100g of dispersed nano-scale 4,4'-(hexafluoroisopropenyl)-di-o-xylene (6-FXP) and 77g of 50% aqueous hydrogen peroxide solution in a photoreactor for uniform dispersion, Then at 32°C and normal pressure, turn on 15Kw LED cold ultraviolet light with a wavelength of 400nm, and the ultraviolet light power ultraviolet light induces the light source to irradiate the reaction solution for 1.2h, and then heats to 60°C for 2.4h oxidation reaction, and then the reaction solution is covered with a nano-film Filtrate through a filter, and after cooling to room temperature, obtain 6-FT...

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Abstract

The invention relates to the field of material preparation, in particular to a preparation method of 4,4'-(hexafluoroisopropylene)diphthalic anhydride. The method comprises the following steps: firstly, crushing and dispersing granular 4,4'-(hexafluoroisopropenyl)-di-ortho-xylene and water in a wet type nano grinding dispersion machine; then respectively adding the dispersed 4,4'-(hexafluoroisopropenyl)-di-ortho-xylene (6-FXP) and a hydrogen peroxide water solution into a photoreactor for uniformly dispersion; at a proper reaction temperature, turning on an LED cold ultraviolet light so that the ultraviolet light induces a light source to irradiate the reaction liquid for reaction for a certain time; then carrying out heating oxidation reaction, filtering the reaction solution after the reaction is completed, and carrying out suction filtration after cooling to obtain 6-FTA; and finally, drying and dehydrating the 6-FTA in a microwave vacuum drying oven to obtain the 6-FDA. The methodis simple in preparation process, green and environment-friendly. The product is high in yield and purity and extremely low in metal ion content, and industrial production is facilitated.

Description

technical field [0001] The invention relates to the technical field of material preparation, in particular to a method for preparing 4,4'-(hexafluoroisopropylene) diphthalic anhydride. Background technique [0002] 4,4'-(hexafluoroisopropylene) diphthalic anhydride (6FDA) is a new type of polyimide monomer material. Polyimide using hexafluorodianhydride as a monomer has the following properties: Advantages: 1) Low dielectric constant. The dielectric constant of ordinary polyimide is about 3.4, but after adding 6FDA, its dielectric constant can be reduced to 2.5. The result of low dielectric constant is the reduction of signal delay and loss, which is of great value in electrical applications. 2) Transparency and controllable refractive index. Because polyimide is slightly yellowish or brown, it can become transparent after adding 6FDA, and its refractive index can be controlled according to the amount of 6FDA added. These properties have great influence on the application...

Claims

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Application Information

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IPC IPC(8): C07D307/89
Inventor 李超程杰黄勇
Owner 自贡中天胜新材料科技有限公司
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