Preparation method for synthesizing brominated polycarbonate
A brominated polycarbonate and dual catalyst technology, applied in the field of fine chemicals, can solve problems such as low catalytic efficiency of a single catalyst, and achieve the effects of controlling production cost, simple process and safe operation
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Embodiment 1
[0036] (1) catalyzer triethylamine 0.84ml (0.006mol) is dissolved in 40ml dichloroethane, standby;
[0037] (2) Add 100g (0.184mol) of tetrabromobisphenol A, 150ml of water, 15g (0.375mol) of sodium hydroxide, 140ml of dichloroethane, 22.9g (0.077mol) of triphosgene into the reaction vessel, stir for 35min, and dissolve. Keep at 20-25°C;
[0038] (3) Add the solution prepared in step (1) dropwise to the reaction system, 5.44ml (0.009mol) of dibutyltin dilaurate, and stir for 60min;
[0039] (4) Dissolve 8g (0.2mol) of sodium hydroxide and 8.64g (0.092mol) of phenol in 142ml of water, slowly add the dissolved mixed solution into the reaction system, and stir and react at 30-35°C for 150min;
[0040] (5) Wash with 50 ml of 1% sodium hydroxide, let stand to separate layers, and separate the organic layer;
[0041] (6) wash with 50ml of 1% hydrochloric acid, leave to stand for stratification, and separate the organic layer;
[0042] (7) Wash with 150ml of deionized water three ...
Embodiment 2
[0048] (1) catalyzer triethylamine 0.84ml (0.006mol) is dissolved in 40ml dichloroethane, standby;
[0049] (2) Add 100g (0.184mol) of tetrabromobisphenol A, 150ml of water, 15.2g (0.38mol) of sodium hydroxide, 140ml of dichloroethane, 24.04g (0.081mol) of triphosgene into the reaction vessel, stir for 35min, and dissolve , keep at 20-25°C;
[0050] (3) Add the solution prepared in step (1) dropwise to the reaction system, 5.44ml (0.009mol) of dibutyltin dilaurate, and stir for 60min;
[0051] (4) Dissolve 8.8g (0.22mol) of sodium hydroxide and 9.504g (0.101mol) of phenol in 142ml of water, slowly add the dissolved mixture dropwise into the reaction system, and stir and react at 30-35°C for 150min;
[0052] (5) Wash with 50 ml of 1% sodium hydroxide, let stand to separate layers, and separate the organic layer;
[0053] (6) Wash with 50ml of 1% hydrochloric acid, leave to stand for stratification, and separate the organic phase;
[0054] (7) Wash with 150ml of deionized wat...
Embodiment 3
[0059] (1) catalyzer triethylamine 0.84ml (0.006mol) is dissolved in 40ml dichloroethane, standby;
[0060] (2) Add 100g (0.184mol) of tetrabromobisphenol A, 150ml of water, 14.72g (0.368mol) of sodium hydroxide, 140ml of dichloroethane, 22.4g (0.075mol) of triphosgene into the reaction vessel, stir for 35min, dissolve , keep at 20-25°C;
[0061] (3) Add the solution prepared in step (1) dropwise to the reaction system, 5.44ml (0.009mol) of dibutyltin dilaurate, and stir for 60min;
[0062] (4) Dissolve 7.0g (0.175mol) of sodium hydroxide and 7.52g (0.08mol) of phenol in 142ml of water, slowly add the dissolved mixture dropwise into the reaction system, and stir and react at 30-35°C for 150min;
[0063] (5) Wash with 50 ml of 1% sodium hydroxide, let stand to separate layers, and separate the organic layer;
[0064] (6) Wash with 50ml of 1% hydrochloric acid, leave to stand for stratification, and separate the organic phase;
[0065] (7) Wash with 150ml of deionized water f...
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