Method for preparing 4, 4 '-(hexafluoroisopropenyl) diphthalic anhydride

A technology of hexafluoroisopropenyl and diphthalic anhydride, which is applied in the direction of organic chemistry, can solve the problems of large reaction risk factor, difficulty in industrial scale-up, and environmental protection, and achieve high product quality stability, easy process control, and essential safe effect

Pending Publication Date: 2020-06-26
SHANDONG GUANSEN POLYMER MATERIAL TECH CO LTD
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  • Application Information

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Problems solved by technology

[0006] Chinese patent CN101696199A discloses a process for preparing 6-FDA by oxidizing 6-FXP with potassium permanganate, but the oxidizing operation of potassium permanganate is complicated, and a large amount of manganese dioxide is produced in the process, which requires a large amount of solvent and acid and alkali, and there are many wastes. There are still big problems in actual industrial production
However, these reaction processes are mainly carried out ar

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  • Method for preparing 4, 4 '-(hexafluoroisopropenyl) diphthalic anhydride
  • Method for preparing 4, 4 '-(hexafluoroisopropenyl) diphthalic anhydride

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Embodiment 1

[0015] Example embodiments will now be described more fully with reference to the accompanying drawings. Example embodiments may, however, be embodied in many forms and should not be construed as limited to the examples set forth herein; rather, these embodiments are provided so that this disclosure will be thorough and complete and fully convey the concept of example embodiments to those skilled in the art. Furthermore, the described features, structures, or characteristics may be combined in any suitable manner in one or more embodiments. In the following description, numerous specific details are provided in order to give a thorough understanding of embodiments of the invention. However, those skilled in the art will appreciate that the technical solutions of the present invention may be practiced without one or more of the specific details, or other methods, components, means, steps, etc. may be employed. In other instances, well-known methods, apparatus, implementations...

Embodiment 2

[0017] Add 50kg (138.8 mol) of 4,4'-(hexafluoroisopropenyl) di-o-xylene and 300kg of glacial acetic acid into the mixing kettle, and add 1000g of cobalt bromide and 400g of manganese acetate into the kettle, stir and dissolve to form a solution. The mixed solution is pumped into the microchannel reactor through the feed pump, and oxygen is introduced at the same time. The molar ratio of oxygen to 4,4'-(hexafluoroisopropenyl)di-o-xylene (6-FXP) is 8.0:1 . The reaction pressure is controlled at 1.6MPa, the temperature is 195°C, and the reaction time of the reactants in the microchannel reactor is 55s. After cooling, the oxidized product was transferred to a receiving tank for separation. After cooling, the tetraacid was precipitated, filtered, washed, and recrystallized to obtain 4,4'-(hexafluoroisopropenyl)diphthalic acid (6-FTA). Heated and refluxed in acetic anhydride to obtain 4,4'-(hexafluoroisopropenyl) diphthalic anhydride (6-FDA). After filtering, washing and drying, 55...

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Abstract

The invention relates to a method for preparing 4, 4 '-(hexafluoroisopropenyl) diphthalic anhydride. The method comprises the following steps: step 1, mixing 4, 4'-(hexafluoroisopropenyl) di-o-xylene,a metal ion catalyst, a cocatalyst and a solvent to form a homogeneous solution; step 2, injecting the prepared solution into a continuous reactor at a certain speed through a pump, and introducing corresponding equivalent pure oxygen into the reactor; step 3, enabling a reactant solution and pure oxygen to react in the continuous reactor, carrying out separation from the continuous reactor afterstaying for a certain period of time, and enabling a product to enter a gas-liquid separation tank after passing through a cooling module; step 4, separating the product solution to obtain 4, 4 '-(hexafluoroisopropenyl) diphthalic acid (6-FTA); and step 5, performing refining to obtain 4, 4'-(hexafluoroisopropenyl) diphthalic anhydride (6-FDA).

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a method for preparing 4,4'-(hexafluoroisopropenyl) diphthalic anhydride. Background technique [0002] Polyimide has the advantages of high strength, high dielectric constant, and non-toxicity. It is increasingly used in the electronics industry and is the substrate material for flexible circuit boards. Ordinary polyimide film is yellow and has a light transmittance of less than 70%, so it cannot be used as a flexible display cover. The introduction of fluorine-containing groups into polyimide polymer monomers can effectively improve its light transmittance, and prepare polyimide transparent films that meet the requirements of folding screens. Among the many transparent monomers, 4,4'-(hexafluoroisopropenyl) diphthalic anhydride (6-FDA) is the most critical one. [0003] The current preparation route of 6-FDA is mainly prepared by oxidation and dehydratio...

Claims

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Application Information

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IPC IPC(8): C07D307/89
CPCC07D307/89
Inventor 李晓斐巴广芝盖新世安娜
Owner SHANDONG GUANSEN POLYMER MATERIAL TECH CO LTD
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