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TFPX synthesizing method

A synthesis method and mixture technology, applied in the field of preparation of tetrafluoride-p-xylene, can solve the problems of high price, increased TFPX development cost, high cost, etc.

Inactive Publication Date: 2007-06-13
YUAN SHIN MATERIALS TECH CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] However, the current methods for synthesizing TFPX are very expensive, time-consuming, and cannot be used for scale-up processes
For example, after mixing α, α, α', α'-tetrachloro-p-xylene (α, α, α', α'tetrachloro-p-xylene, TCPX) and KF in an appropriate proportion, in a closed Or carry out the reaction in an open reaction vessel. The reaction lasts for 12 hours at a temperature of about 260-280°C. Although TFPX products can be obtained, since no other solvents are added, it is a similar solid-phase reaction. If the stirring is not good, serious gums are likely to occur The problem of agglomeration not only affects the yield, but also is not suitable for the expansion process
Some organic compounds containing carbonyl functional groups (carbonyl group), such as terephthalaldehyde (terephthaaldehyde), and fluorinating agent SF 4 、MoF 6 , DAST or HF / Py in appropriate solvent and temperature for fluorination reaction, although higher yields of TFPX can be obtained, but the price of these fluorinating agents is expensive, the reaction equipment and operating conditions are relatively harsh, and waste gas and waste liquid Difficult to handle
It can be seen that these methods not only greatly increase the development cost of TFPX, but also are not conducive to the expansion of production.

Method used

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Examples

Experimental program
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Embodiment 1

[0018] Example 1: Using sulpholane as solvent

[0019] The reagent grade KF is ground finely with a research pot and dried at 160°C (or industrial grade KF is ground with a ball mill and dried at 210°C). Take 320 grams of KF and 160 grams of TCPX and place them in a 1000 ml glass reactor (the Moore ratio of TCPX and KF is 1:8). In a nitrogen atmosphere, 8.0 g of PTC (tetraphenylphosphonium bromide) and 320 g of sulpholane were added to form a slurry. Then, it was heated to 155°C with stirring in an oil bath, and the reaction was continued for 48 hours (at this time, the nitrogen flow can be stopped). After the reaction is over, the slurry is cooled, and acetone is added to clean the slurry. The slurry is then filtered to obtain a filtrate and a filter cake. Distill the filtrate in stages, distill acetone, TFPX, and sulpholane separately to obtain the desired product TFPX (the yield is about 70%).

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Abstract

The invention relates to a synthesis method for TFPX (alpha,alpha,alpha', alpha'tetrafluoro-p-xylene), including the following steps: (a)supplying a sulpholane solution containing TCPX (alpha,alpha,alpha', alpha'tetrachloro-p-xylene), (b) making a mixture of the sulpholane solution, a fluoride salt and a PTC, in which, PTC is quatermary phosphate, and (c) heating the mixture to get a product.

Description

Technical field [0001] The invention relates to a synthetic method, in particular to a preparation method suitable for preparing tetrafluoro-p-xylene (TFPX). Background technique [0002] Because parylene polymer has many processing advantages, such as the coating environment at room temperature, there is no residual stress after coating and the thickness of the deposited film can be precisely controlled. Moreover, the parylene polymer has uniform, acid and acid resistance. Alkali, colorless, high transparency, low dielectric... and other characteristics. Therefore, it is widely used in electrical isolation of printed circuit boards, moisture protection of sensors or medical instruments, and corrosion protection of metal coatings... etc. At present, fluorine-containing parylene polymer has a low dielectric constant and a high melting point, and it will be used in the dielectric film of the electronics and coatings industry to attract attention. [0003] Fluoro parylene polymer ha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/20C07C22/08
Inventor 何潜渊林材峰林俊旭王时俊
Owner YUAN SHIN MATERIALS TECH CORP