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TFPX synthesizing method

A technology for mixture and p-xylene is applied in the field of preparation of tetrafluoride-p-xylene, which can solve the problems of high cost, high price, and difficulty in handling waste gas and waste liquid.

Inactive Publication Date: 2011-02-09
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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Experimental program
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Effect test

Embodiment 1

[0018] Embodiment one: take sulpholane as solvent

[0019] Grind the reagent-grade KF with a mortar and dry it at 160°C (or grind the industrial-grade KF with a ball mill and dry it at 210°C). The KF of 320 grams and the TCPX of 160 grams are placed in the glass reactor of 1000ml (the molar 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 stirred and heated to 155° C. in an oil bath, and the reaction was continued for 48 hours (the nitrogen flow could be stopped at this time). After the reaction is finished, 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. The filtrate was distilled in sections, and the acetone, TFPX, and sulpholane were distilled off separately to obtain the desired product TFPX (yield 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 synthesis method, especially a preparation method suitable for preparing tetrafluoro-p-xylene (TFPX). Background technique [0002] Since parylene polymer has many processing advantages, such as the coating environment is room temperature, no residual stress occurs after coating and the thickness of the deposited film can be precisely controlled, and the parylene film is uniform, acid-resistant and resistant. Alkali, colorless, high transparency, low dielectric...etc. Therefore, it is widely used in the electrical isolation of printed circuit boards, the moisture protection of sensors or medical instruments, and the corrosion protection of metal coatings...etc. Currently, fluorine-containing polyparaxylylene (fluoroparylene polymer) has a low dielectric constant and a high melting point, and will be used as a dielectric film in the electronics and paint industries. [0003] Fluoro parylene polymer has the structure of the f...

Claims

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Application Information

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Patent Type & Authority Patents(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