Facile and effective method of preparing 1,4-Bis(chlorodifluoromethyl)benzene

一种氯二氟甲基、二氟甲基的技术，应用在批次式或连续式用以制备1领域，能够解决产率低、复杂纯化步骤、反应时间长等问题，达到反应时间短、降低制作成本、成本低的效果

Active Publication Date: 2013-05-15
YUAN SHIN MATERIALS TECH CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the disadvantages of this method are long reaction time, low yield, and the necessity to use environmentally regulated solvents (CCl 4 ) or photoinitiator, and the final product can be obtained through more complicated purification steps and consumes a lot of energy

Method used

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  • Facile and effective method of preparing 1,4-Bis(chlorodifluoromethyl)benzene
  • Facile and effective method of preparing 1,4-Bis(chlorodifluoromethyl)benzene

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preparation example Construction

[0044] The method for preparing 1,4-bis(chlorodifluoromethyl)benzene provided by the invention comprises: (A) providing a method comprising 1,4-bis(difluoromethyl)benzene (1,4-Bis( difluoromethyl)benzene) reaction solution; (B) feed chlorine gas (Cl) at a temperature of 50-90°C 2 ) to the reaction solution, and (C) maintaining the reaction system pressure greater than 1 atm, to obtain 1,4-bis(chlorodifluoromethyl)benzene.

[0045] In the preparation method of the present invention, under a reaction pressure slightly greater than 1 atm, 1,4-bis(difluoromethyl)benzene can be directly reacted with chlorine, and there is no need to 1,4-bis(difluoromethyl)benzene Methyl)benzene is soluble in a solvent, and there is no need to add a photoinitiator, and 1,4-bis(difluoromethyl)benzene can react with chlorine gas under direct light. Since the preparation method of the present invention uses the reactant 1,4-bis(difluoromethyl)benzene as a solvent and reacts completely, there is no nee...

Embodiment 1

[0065] First, 300 g (1.69 mole) of 1,4-bis(difluoromethyl)benzene (TFPX) was added into a glass reactor, stirred evenly with a stirrer, and the reaction temperature was heated to 60° C. The glass reactor was then irradiated with a 400-watt mercury lamp.

[0066] Afterwards, a slight excess of Cl was continuously introduced 2 (approximately 336g, 4.73mole) into a glass reactor for chlorination. During the reaction process, the reaction pressure was maintained slightly higher than 1 atm (about 1.01 atm). After the reaction was continued for 45 minutes, a slightly yellow reactant was obtained. The purity of GC analysis was as high as 99.32%. The yellow reactant was neutralized with lye, and the oil and water phases were separated. And after steps such as distillation (pressure 10torr, b.p.125 ℃), obtain colorless liquid 408g, yield rate is 98.1%.

[0067] The liquid was analyzed by GC, and it was confirmed that the product was 1,4-bis(chlorodifluoromethyl)benzene with a purity ...

Embodiment 2

[0069] First, take 600.01g (3.37mole) of 1,4-bis(difluoromethyl)benzene (TFPX) into the glass reactor, stir evenly with a stirrer, and heat the reaction temperature to 60°C by the water-proof heating method , and then irradiate the glass reactor with a 400-watt mercury lamp.

[0070] Afterwards, a slight excess of Cl was continuously introduced 2 (about 600g, 8.43mole) into a glass reactor for chlorination. During the reaction process, the reaction pressure was maintained slightly higher than 1 atm (about 1.01 atm). After the reaction was continued for 100 minutes, a yellowish liquid was formed.

[0071] After completing the above steps, the light yellow liquid was subjected to GC analysis, and it was confirmed that the product of 1,4-bis(chlorodifluoromethyl)benzene was produced, and the purity was as high as 99.49%.

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Abstract

The present invention relates to a facile method of preparing 1,4-bis(chlorodifluoromethyl)benzene, comprising the steps of: (A) providing a reactant liquid of 1,4-bis(difluoromethyl)benzene; optionally (B) providing a light source for UV radiation; and (C) introducing chlorine gas into the reactant liquid at a temperature of 50-90 DEG C. under a pressure above 1 atm to obtain 1,4-Bis(chlorodifluoromethyl)benzene. The invented facile method can be utilized in a batch process or a continuous process for effective production of 1,4-bis(chlorodifluoromethyl)benzene.

Description

technical field [0001] The invention relates to a method for preparing 1,4-bis(chlorodifluoromethyl)benzene (1,4-Bis(chlorodifluoromethyl)benzene), in particular to a batch process with simple process, short reaction time and high yield. Secondary or continuous method for the preparation of 1,4-bis (chlorodifluoromethyl) benzene. Background technique [0002] Parylene (parylene) is prepared by vacuum pyrolysis chemical vapor deposition (CVD), which can be made into an extremely thin film with excellent electrical properties, heat resistance, chemical stability, colorless and high transparency, etc., mainly Used as film and coating, it is widely used in the electrical isolation of printed circuit boards, the moisture protection of sensors or medical instruments, the electrical insulation medium of electronic components, protective coatings and packaging materials, and the corrosion protection of metal coatings, etc. [0003] Recently, since fluorine-containing parylenes, suc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C22/08C07C17/14
CPCC07C22/08C07C17/14
Inventor 林俊旭鄞弘政孙谦益鄞永裕周娟玉
Owner YUAN SHIN MATERIALS TECH CORP
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