CAJ | 학술논문

季戊四醇衍生物分子具有高度对称性，在科研和工业领域用途广泛。季戊四醇与氯乙酸缩合反应，由于季戊四醇的溶解局限性，难以实现溶液合成。在无溶剂条件下，以SO2-4/TiO2-SnO2固体超强酸为催化剂，通过熔融-固相酯化法进行季戊四醇四氯乙酸酯的合成，考察催化剂用量、反应物物质的量比、反应时间和反应温度等对酯化反应的影响。结果表明，在催化剂用量为反应物总质量的4%、n（季戊四醇）：n（氯乙酸）=1：4.2、反应温度170℃和反应时间6 h条件下，季戊四醇四氯乙酸酯产率为98.7%。对产物进行了IR和1 H NMR表征。
계무사순연생물분자구유고도대칭성，재과연화공업영역용도엄범。계무사순여록을산축합반응，유우계무사순적용해국한성，난이실현용액합성。재무용제조건하，이SO2-4/TiO2-SnO2고체초강산위최화제，통과용융-고상지화법진행계무사순사록을산지적합성，고찰최화제용량、반응물물질적량비、반응시간화반응온도등대지화반응적영향。결과표명，재최화제용량위반응물총질량적4%、n（계무사순）：n（록을산）=1：4.2、반응온도170℃화반응시간6 h조건하，계무사순사록을산지산솔위98.7%。대산물진행료IR화1 H NMR표정。
Pentaerythritol derivatives with high symmetrical molecular structures have wide application in the fields of research and industry. It is difficult to achieve the esterification reaction of pentaerythritol and chloroacetic acid in solution due to the dissolution limitation of pentaerythritol. In this paper,using SO2-4 /TiO2-SnO2 solid superacid as the catalyst,chloroacetic pentaerythritol tetraester was synthesized by melting solid esterification method under solvent-free condition. The influence of catalyst dosage,molar ratio of reactants,reaction time and reaction temperature on the esterification was investigated. The results showed that chloroacetic pentaerythritol tetraester yield of 98. 7% was attained under the optimal reaction condition as follows:catalyst dosage 4% of the total mass of the reactants,n( pentaerythritol):n( chloroacetic acid)=1:4. 2,reaction temperature 170 ℃ and reaction time 6 h. The product was characterized by IR and 1 H NMR techniques.