Thioether-containing self-flame-retardant polyester and preparation method thereof
A technology of flame-retardant polyester and flame-retardant polyester, which is applied in the field of sulfide-containing self-flame-retardant polyester and its preparation, can solve the problems of molecular chain forming processing, low glass transition temperature, poor processability, etc., and achieves good stability , high purity, the effect of improving flame retardant properties
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Embodiment 1
[0038] Embodiment 1, poly 4, the preparation of 4'-diphenylsulfide dicarboxylic acid 2,2-bis(3,5-dimethyl-4-hydroxyphenyl) propane ester---TDC-TMBPA
[0039] With 2,2-bis(3,5-dimethyl-4-hydroxyphenyl) propane 28.4g, hexadecyltrimethylammonium chloride 10g, potassium carbonate 13.8g, add successively to the tank containing 200g water In the three-necked flask, stir and dissolve at room temperature; then dissolve 20 g of 4,4'-diphenylsulfide diformyl chloride into a beaker containing 300 parts of dichloromethane, and add it dropwise to the above-mentioned three-necked flask, Stir the reaction at 35°C for 10 hours to obtain high molecular weight sulfide-containing polyester poly 4,4'-diphenylsulfide dicarboxylic acid 2,2-bis(3,5-dimethyl-4-hydroxyphenyl)propane Esters---TDC-TMBPA, washed with water and ethanol, dried at 50°C for 8 hours, pulverized, extracted and purified with deionized water and acetone respectively, dried at 100°C for 5 hours to obtain 47.4g of pure resin, the ...
Embodiment 2
[0040] Embodiment 2, poly 4, the preparation of 4'-diphenylsulfide dicarboxylic acid 1,1-bis(4-hydroxyphenyl)-1-phenylethane ester---TDC-PhBPA
[0041]29g of 1,1-bis(4-hydroxyphenyl)-1-phenylethane, 5g of sodium dodecylsulfonate, and 20g of potassium bicarbonate were successively added to a three-necked flask with 100g of water, and Stir to dissolve at room temperature; then dissolve 40 g of 4,4'-diphenylsulfide diformyl chloride into a beaker containing 150 parts of chloroform, and dropwise add it to a three-necked flask, and stir and react at 25°C for 5 hours to obtain high Molecular weight thioether-containing polyester poly 4,4'-diphenylsulfide dicarboxylic acid 1,1-bis(4-hydroxyphenyl)-1-phenylethane ester---TDC-PhBPA, after water, Wash with ethanol, dry at 100°C for 5h, pulverize, extract and purify with deionized water and acetone respectively, and dry at 200°C for 1h to obtain 50.6g of pure resin with a yield of about 96%; use concentrated sulfuric acid as a solvent to...
Embodiment 3
[0042] Embodiment 3, the preparation of poly 4,4'-diphenylsulfide dicarboxylic acid 2,2-bis(3,5-dimethyl-4-hydroxyphenyl) propane ester---TDC-TMBPA
[0043] 2,2-bis(3,5-dimethyl-4-hydroxyphenyl)propane 28.5g, hexadecyltrimethylammonium bromide 0.1g, sodium hydroxide 8g, were added in turn to the In a three-necked flask, stir and dissolve at room temperature; then dissolve 30 g of 4,4'-diphenylsulfide diformyl chloride into a beaker containing 50 parts of chlorobenzene, and add it dropwise to the above-mentioned three-necked flask, Stir and react at 5°C for 3 hours to obtain high molecular weight thioether-containing polyester poly 4,4'-diphenylsulfide dicarboxylic acid 2,2-bis(3,5-dimethyl-4-hydroxyphenyl)propane Esters---TDC-TMBPA, washed with water and ethanol, dried at 200°C for 2 hours, pulverized, extracted and purified with deionized water and acetone respectively, dried at 80°C for 20 hours to obtain 46.3g of pure resin, the yield is about 93% ; Use chloroform as a sol...
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