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Preparation method of vinylbenzyl-polyphenyl ether composition

A technology of vinylbenzyl and polyphenylene ether, which is applied in the field of preparation of vinylbenzyl-polyphenylene ether compounds, and can solve the problems of low yield, long engineering time, difficult decompression fractionation and removal, etc.

Active Publication Date: 2014-10-01
DAI ICHI KOGYO SEIYAKU CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Although the preparation method of Patent Document 1 may remove halogen compounds and halide ions, it is expected to improve in terms of low yield, long engineering time, and preparation cost because it includes a reprecipitation purification process.
[0006] In addition, as a method of removing halogenated compounds (epichlorohydrin: boiling point about 118°C) derived from unreacted raw materials, for example, the vacuum fractionation method described in the examples of Patent Document 2 is used, but the methyl halide used in the present invention The boiling point of methyl styrene (chloromethyl styrene) is 229-240 °C, it is difficult to remove it by vacuum fractionation

Method used

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  • Preparation method of vinylbenzyl-polyphenyl ether composition
  • Preparation method of vinylbenzyl-polyphenyl ether composition
  • Preparation method of vinylbenzyl-polyphenyl ether composition

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] In a 2L four-neck flask equipped with a temperature regulator, a stirring device, a condenser and a dropping funnel, put 158g (0.1 moles) of polyphenylene ether represented by general formula (1) (R in general formula (1) 1 , R 3 , R 5 , R 7 , R 10 , R 12 , R 14 , R 16 is methyl, R 2 , R 4 , R 6 , R 8 , R 9 , R 11 , R 13 , R 15 hydrogen, A is isopropylidene, m+n=average 12, number average molecular weight is 1580), 221g toluene, 94.8g isopropanol, mix well, then add 0.96g tetra-n-butylammonium bromide, 33.6 g (0.22 mol) of vinyl benzyl chloride (meta body / para body = 50 / 50, trade name: CMS-P, manufactured by Seimichemical Co.), and the temperature was raised to 75°C. Here, 53.3 g (0.64 mol) of 48% sodium hydroxide aqueous solution was dripped over 30 minutes, and the reaction was carried out at 75° C. for 5 hours, and the reaction rate was 98% or more.

[0074] Next, as a step of removing unreacted vinylbenzyl chloride, 16.7 g (2.0 equivalents to 1 equiva...

Embodiment 2

[0077] In a 2L four-necked flask equipped with a temperature regulator, a stirring device, a condenser and a dropping funnel, put 240g (0.1 mol) of polyphenylene ether represented by general formula (2) (R in general formula (2) 17 for hydrogen, R 18 is methyl, R 19 for hydrogen, R 20 Methyl, o=20, number average molecular weight 2400), 336g toluene, 144g isopropanol, mix well, then add 1.30g tetra-n-butylammonium bromide, 19.8g (0.13 mole) vinylbenzyl Chloride (metasite / parasite = 50 / 50, trade name: CMS-P, manufactured by Seimichemical Co.), the temperature was raised to 75°C. Here, 27.5 g (0.33 mol) of 48% sodium hydroxide aqueous solution was dripped over 30 minutes, and the reaction was carried out at 75° C. for 5 hours, and the reaction rate was 98% or more.

[0078]Next, as a step of removing unreacted vinylbenzyl chloride, 16.7 g (2.0 equivalents to 1 equivalent of polyphenylene ether) 48% sodium hydroxide, 6.0 g (to 100 Parts by mass of polyphenylene ether is 2.5 p...

Embodiment 3

[0081] Except that the tetra-n-butylammonium bromide used in the step of removing unreacted vinylbenzyl halide was replaced with 8.0 g (5.0 parts by mass relative to 100 parts by mass of polyphenylene ether), and the same as the implementation Example 1 was carried out in the same manner to obtain 345 g of the product (yield based on polyphenylene ether: 95%). The amount of vinylbenzyl chloride remaining in the obtained product (solid content conversion value, the same below) is less than 0.1%, the halide ion concentration is 4ppm, and the number average molecular weight of vinylbenzyl-polyphenylene ether compound is 2170, The weight average molecular weight was 3650.

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Abstract

The invention discloses a preparation method of a vinylbenzyl-polyphenyl ether composition. Under the existence of the alkali metalhydroxide aqueous solution, in the solution containing the aromatic hydrocarbon and the fatty alcohol, the polyphenyl ether provided with the repeated units expressed by the formula 1 and the formula 2, and provided with the phenolic hydroxyl group on the end and the reaction process having the vinylbenzyl reactor reaction expressed by the formula 3 are provided. Under the existence of the phase transfer catalyst, the reaction liquid acquired by the reaction process can be treated by the alkali metal hydroxides water solution, and the removing process of the un-reacted vinyl benzylhalide can be provided. The preparation method of the vinylbenzyl-polyphenyl ether composition can be used to greatly reduce the residuals of the halide group composition and the halide ions.

Description

technical field [0001] The invention relates to a preparation method of vinylbenzyl-polyphenylene ether compound. Background technique [0002] Vinylbenzyl-polyphenylene ether compounds are used as materials for high-frequency electronic devices because they are excellent in dielectric properties, moisture absorption resistance, and heat resistance. [0003] Usually when used as electronic materials, starting from the durability and reliability of the product, it is necessary to reduce the residual amount of halogen compounds and halide ions as much as possible. From the aspects of preparation process and preparation cost, it is preferred to use a simple method to remove halogen compounds, halide ion. [0004] The current method for the preparation of vinylbenzyl-polyphenylene ether compounds, as known, is to combine polyphenylene ether compounds with halogenated methylstyrene (vinylbenzyl halides) in toluene in the presence of alkali metal hydroxides After the reaction, t...

Claims

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Application Information

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IPC IPC(8): C08G65/48
Inventor 村上贤志门胁利治菊田学
Owner DAI ICHI KOGYO SEIYAKU CO LTD
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