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Dihydroxyl polyphenyl ether and preparation method thereof

A technology of bishydroxy polyphenylene ether and toluene, which is applied in the field of bishydroxy polyphenylene ether and its preparation, can solve the problems of reducing the market competitiveness of products, long process cycle, difficult separation, etc., and can meet the requirements of industrial production and have uniform molecular weight distribution. , The effect of molecular weight control and stability

Active Publication Date: 2017-11-17
宋立旺
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Problems solved by technology

[0005] In the related art, the redistribution method is used to prepare low-molecular-weight dihydroxypolyphenylene ether, which is to use high-molecular-weight polyphenylene ether to break the chain under the action of a peroxide initiator to form a small-molecule polyphenylene ether with free radicals, and then combine with polyphenylene ether. Phenolic compounds are combined to form low-molecular-weight dihydroxypolyphenylene ether. There are many by-products in this method, and a large amount of initiator is added during the preparation process. It is easy to have a certain amount of residue in the final product, which is difficult to handle and difficult to prepare high-purity products. ; and the method has a long process cycle and a large amount of waste discharge, which is difficult to meet industrial production
In the related art, low-molecular-weight dihydroxypolyphenylene ether is prepared by oxidative coupling method, and the raw materials tetramethylbisphenol F, tetrabromobisphenol A, bisphenol A and bisphenol B used are not high in solubility in the reaction system, and The reactivity between 2,6-dimethylphenols is low, and there are many residual bisphenol monomers in the obtained product and it is not easy to separate, resulting in low purity of the product, which is difficult to meet the use requirements
In addition, in related technologies, tetramethylbisphenol A monomer is directly used as a raw material to prepare bishydroxypolyphenylene ether through oxidative coupling. Due to the low degree of commercialization and high price of tetramethylbisphenol A monomer, the production cost is relatively high. Reduce the market competitiveness of the product, so it is not suitable for mass commercial production

Method used

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[0063] The preparation method of the bishydroxy polyphenylene ether of the present invention comprises passing through a reaction liquid composed of a solvent, a metal salt and an amine compound to oxidatively couple monomer products with an oxygen-containing gas, and then terminating the reaction to obtain bishydroxy polyphenylene ether; the bishydroxy polyphenylene ether of the present invention The preparation method of the hydroxypolyphenylene ether has simple process operation, low production cost and high production efficiency, and can meet the industrial production requirements of the low-molecular-weight dihydroxypolyphenylene ether.

[0064] In a preferred embodiment of the present invention, the monophenol is selected from one or more of phenol and alkylphenol, preferably selected from 2,6-xylenol, 2,3-xylenol, 2 , one of 5-xylenol, 3,5-xylenol phenol, o-cresol, m-cresol, 2,3,6-trimethylphenol, 2,3,5-trimethylphenol and phenol One or more, more preferably 2,6-xylenol...

Embodiment 1

[0109] A preparation method of bishydroxy polyphenylene ether, comprising the steps of:

[0110] 1. Monomer preparation: put 1200g 2,6-xylenol, 1200g toluene and 300g sulfonated polystyrene-divinylbenzenesulfonic acid resin into 5000mL monomer reactor 1, start stirring and heat up to 70°C 142.6g of acetone is added to the reaction kettle 1 with the raw material metering pump 16, and the addition time is 80min. After the acetone is added, the timing starts. After 480min, the reaction solution is filtered and moved to the neutralization kettle 2, and 100g of the acetone is added to the neutralization kettle 2. The sodium carbonate solution with a mass fraction of 20% is stirred for 10 min and then moved into the phase separation tank 3. After the phase separation, the light phase enters the distillation tower 5 for distillation. The tank 13 is used for further processing; the heavy phase in the phase separation tank 3 enters the dehydration tower 4 for dehydration and then enter...

Embodiment 2

[0113] The low molecular weight dihydroxy polyphenylene ether was prepared according to the method of Example 1, except that the amount of toluene used in the monomer preparation was 4800g, the amount of acid catalyst was 1200g, the amount of acetone was 570.4g, and the monomer reaction temperature was 20°C. The reaction time is 24 hours, the reaction temperature of the polymerization reaction is 90°C, and the reaction time of the polymerization reaction is 1h. After the reaction is terminated, the temperature is controlled to 90°C, and the stirring is continued for 30 minutes. The precipitation temperature is 100°C, and the extrusion temperature is 200°C. The experimental results are listed in Table 1.

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Abstract

The invention provides dihydroxyl polyphenyl ether and a preparation method thereof. The preparation method of the dihydroxyl polyphenyl ether provided by the invention comprises the following steps of introducing an oxygen-containing gas into a reaction solution prepared from a solvent, a metallic salt and an amine compound to carry out oxidative coupling to obtain a monomer product, and then terminating a reaction, so as to obtain the dihydroxyl polyphenyl ether. The preparation method of the dihydroxyl polyphenyl ether provided by the invention is simple in technical operation, low in production cost and high in production efficiency, and can be used for meeting the industrialized production requirement of the dihydroxyl polyphenyl ether with a low molecular weight. A product of the dihydroxyl polyphenyl ether provided by the invention is low in molecular weight, stable in molecular weight control and uniform in molecular weight distribution, good in compatibility with other matrix resin such as PCB (Printed Circuit Board) and excellent in reaction performance, and is ideal matrix resin for preparing a high-frequency copper-clad board.

Description

technical field [0001] The invention relates to the technical field of polyphenylene ether preparation, in particular to a dihydroxy polyphenylene ether and a preparation method thereof. Background technique [0002] With the rapid development of the information industry, higher requirements have been put forward for the matrix resin for copper clad laminates, which are required to have low dielectric constant, low dielectric loss, high glass transition temperature, high heat resistance and low water absorption. The most widely used matrix resin in the CCL manufacturing industry is epoxy resin, which cannot meet the needs of technological development due to poor dimensional stability when used at high temperatures and high dielectric constant in the high frequency range. Polyphenylene ether resin has good comprehensive properties, especially high glass transition temperature and excellent dielectric properties. It is an ideal substitute material for high-performance copper-c...

Claims

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Application Information

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IPC IPC(8): C08G65/44C07C41/09C07C43/295
CPCC07C41/09C07C43/295C08G65/44C08G2650/56
Inventor 宋立旺
Owner 宋立旺
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