Preparation method of polyacrylic acid pentabromobenzyl ester with controllable molecular weight
A technology of poly(pentabromobenzyl acrylate and molecular weight) is applied in the field of preparation of controllable molecular weight poly(pentabromobenzyl acrylate), which can solve the problems of imperfect purification process, uneven molecular weight distribution, low heat resistance and the like, and achieves the The effect of low cost, stable product quality and easy control
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Embodiment 1
[0029] (1) Electrophilic substitution reaction: add 640g of anhydrous bromine, 0.5g of catalyst aluminum trichloride, and 250g of dichloroethane into the reactor, cool down to 10°C, slowly drop 100g of benzyl chloride into the reactor, drop During the addition process, the temperature in the reaction kettle was controlled to 10°C, the tail gas was absorbed by water, and after the dropwise addition was completed, the temperature was kept for 1 hour, and an electrophilic substitution reaction occurred to prepare pentabromobenzyl chloride with a yield of 98.2% and a purity of more than 99%.
[0030] (2) Nucleophilic substitution reaction: react 75g acrylic acid and 550g 20% sodium carbonate solution at room temperature to obtain sodium acrylate solution, adjust the pH value to 7-9; make pentabromobenzyl chloride in step (1) Heat up the solution, distill off excess bromine and residual hydrobromic acid, then cool down to below 50°C, add 1g of tetrabutylammonium bromide to the rea...
Embodiment 2
[0034] (1) Electrophilic substitution reaction: add 640g of anhydrous bromine, 0.5g of catalyst aluminum trichloride, and 250g of dichloroethane into the reactor, cool down to 10°C, slowly drop 100g of benzyl chloride into the reactor, drop During the addition process, the temperature in the reaction kettle was controlled at 20°C, the tail gas was absorbed with water, and after the dropwise addition was completed, the temperature was kept for 1.5 hours, and an electrophilic substitution reaction occurred to prepare pentabromobenzyl chloride with a yield of 98.79%.
[0035] (2) Nucleophilic substitution reaction: react 75g acrylic acid and 565g 20% sodium carbonate solution at room temperature to obtain sodium acrylate solution, adjust the pH value to 7-9; make pentabromobenzyl chloride in step (1) Warm up the solution, distill off excess bromine and residual hydrobromic acid, then cool down to below 50°C, add 1g of tetrabutylammonium bromide to the reaction kettle, raise the ...
Embodiment 3
[0039] (1) Electrophilic substitution reaction: Add 700g of anhydrous bromine, 5g of catalyst aluminum trichloride, and 550g of dichloroethane into the reactor, cool down to 10°C, slowly drop 100g of benzyl chloride into the reactor, and drop The temperature in the reaction kettle was controlled at 30°C during the process, and the tail gas was absorbed by water. After the dropwise addition, the temperature was kept for 2 hours, and an electrophilic substitution reaction occurred to prepare pentabromobenzyl chloride with a yield of 98.12%.
[0040](2) Nucleophilic substitution reaction: react 75g acrylic acid and 580g 20% sodium carbonate solution at room temperature to obtain sodium acrylate solution, adjust the pH value to 7-9; make pentabromobenzyl chloride in step (1) Heat up the solution, distill off excess bromine and residual hydrobromic acid, then cool down to below 50°C, add 1g of tetrabutylammonium bromide to the reaction kettle, raise the temperature to 110°C, keep ...
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