TiO_2/SO_4^(2-)型固体酸催化合成丙酮缩二甲醇

Catalytic Synthesis of Acetone Dimehtyl Ketal with TiO_2/SO_4^(2-) Solid Acid

原甲酸三甲酯和丙酮在TiO2 /SO4 2 - 型固体酸的催化作用下合成了丙酮缩二甲醇 ,并对诸影响因素进行了考察。在反应温度 0～ 5℃ ,反应时间 1h ,原料配比原甲酸三甲酯∶丙酮∶催化剂 (m /m) =10 6∶5 8∶4的优惠工艺条件下 ,此反应可定量完成 ,精馏分离后收率94 .2 % ,纯度 98.1%。催化剂可重复使用多次。用红外。

Acetone dimethyl acetal was synthesized from trimethyl orthoformate and acetone, the reaction was characterized by the catalysis of TiO 2/SO 4 2- solid acid and quantitative conversion. The influence factors were investigated, the results showed that the optimum conditions were as follows: reaction temperature 0～5℃, reaction time 1h, m(trimethyl orthoformate)∶m(acetone)∶m(solid acid)=106∶58∶4. The solid acid can be used repeatedly. The yield was 94.2% after rectification and the purity was 98.1%. The structure of the product was identified with IR and 1HNMR