Purpose

Initiator for Acrylate Polymerization

(1) Synthesis of p-tert-butyl cyclohexyl chloroformate The toluene solution of p-tert-butyl cyclohexanol was dropped into the reactor equipped with phosgene toluene solution, and the reaction temperature was controlled at about 5°C. After the dropwise addition, the stirring was continued for 2 hours. . Then the temperature was raised to 60° C. to remove excess phosgene and by-product hydrogen sulfide until there was no phosgene in the exhausted gas, and the reaction solution was determined to be nearly neutral with test paper. Finally, toluene is distilled off under reduced pressure to obtain p-tert-butylcyclohexyl chloroformate. (CH3)3COH+CChemicalbookOCl2(CH3)3COCOCl+HCl↑(2) Synthesis of TBCP Water, sodium hydroxide, hydrogen peroxide and emulsifier sodium lauryl sulfate were added to the reactor, and the reaction was carried out at about 10 ℃ under stirring to prepare Get sodium peroxide. Then, the above-prepared p-tert-butylcyclohexyl chloroformate was added dropwise, and the reaction temperature was controlled at about 40°C. After adding the ester, a small amount of hydrogen peroxide was added, and the reaction was continued for 1 h. The product is filtered, washed with ice water until neutral, and the finished product is obtained after drying.

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