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
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[0063] The preparation method of the bishydroxy polyphenylene ether of the present invention comprises the following steps: after the oxygen-containing gas is introduced into the reaction liquid composed of a solvent, a metal salt and an amine compound to oxidize the coupled monomer product, the reaction is terminated to obtain the bishydroxy polyphenylene ether; The preparation method of the hydroxy polyphenylene ether has the advantages of simple process operation, low production cost and high production efficiency, and can meet the industrial production requirements of the low molecular weight bishydroxy polyphenylene 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, 2,6-xylenol, 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.
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Example Embodiment
[0108] Example 1
[0109] A preparation method of dihydroxy polyphenylene ether, comprising the steps:
[0110] 1. Monomer preparation: 1200g of 2,6-xylenol, 1200g of toluene and 300g of sulfonated polystyrene-divinylbenzenesulfonic acid resin were charged into 5000mL of monomer reaction kettle 1, and after stirring and heating to 70°C. , 142.6g of acetone was added to the reactor 1 with the raw material metering pump 16, the addition time was 80min, the timing started after the acetone was added, and after 480min, the reaction solution was filtered and moved to the neutralizer 2, and 100g was added to the neutralizer 2. The sodium carbonate solution with a mass fraction of 20% is stirred for 10 minutes and then moved into the phase separation tank 3. After the phase separation, the light phase enters the distillation column 5 for distillation. After cooling, the top material enters the acetone storage tank 12, and the column bottom material enters the toluene and water storag...
Example Embodiment
[0112] Example 2
[0113] The low molecular weight bishydroxy polyphenylene ether was prepared according to the method of Example 1, except that the amount of toluene in the preparation of the monomer was 4800g, the amount of acid catalyst was 1200g, the amount of acetone was 570.4g, the monomer reaction temperature was 20°C, the monomer The reaction time was 24h, the reaction temperature of the polymerization reaction was 90°C, and the reaction time of the polymerization reaction was 1h. After the reaction was terminated, the temperature was controlled to 90°C, and the stirring was continued for 30 minutes. The desolvation temperature was 100°C, and the extrusion temperature was 200°C. The experimental results are listed in Table 1.
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