CAJ | 학술논문

以柠檬酸和正丁醇为原料，在稀土超强酸S2O82-/ZrO2-La2O3的催化下合成柠檬酸三丁酯。通过XRD和红外光谱确定了稀土元素La的掺量对催化剂结构的影响，用正交优化实验优化了催化剂用量、酸醇摩尔比、反应时间等对酯化率的影响。实验结果表明：La掺量为0.07 mol·L-1所得催化剂性能最佳，柠檬酸三丁酯最优催化合成条件为反应温度175℃，醇酸摩尔比4.0∶1，催化剂用量为柠檬酸质量的2.0%，反应时间180 min，酯化率可达98.27%。催化剂可循环使用5次而不会明显降低活性。经折光率、红外光谱、核磁共振氢谱和碳谱测定，所合成产物为柠檬酸三丁酯。
이저몽산화정정순위원료，재희토초강산S2O82-/ZrO2-La2O3적최화하합성저몽산삼정지。통과XRD화홍외광보학정료희토원소La적참량대최화제결구적영향，용정교우화실험우화료최화제용량、산순마이비、반응시간등대지화솔적영향。실험결과표명：La참량위0.07 mol·L-1소득최화제성능최가，저몽산삼정지최우최화합성조건위반응온도175℃，순산마이비4.0∶1，최화제용량위저몽산질량적2.0%，반응시간180 min，지화솔가체98.27%。최화제가순배사용5차이불회명현강저활성。경절광솔、홍외광보、핵자공진경보화탄보측정，소합성산물위저몽산삼정지。
Tributyl citrate(TBC) was synthesized by reaction of citric acid with n-butanol using rare earth solid su?peracid S2O82-/ZrO2-La2O3 as the catalyst. Effects of La content on the catalyst structures were determined by using XRD and FT-IR. Effects of catalyst dosage, molar ratio of n-butanol to citric acid, reaction time on the esterifica?tion rates were explored by orthogonal experiment. Results show that the catalyst can present the best behavior un?der concentration of the La content of 0.07 mol·L-1. The optimum synthesis condition of TBC adds 4 times of n-bu?tanol to citric acid, under the condition of temperature 175℃for 180 min using 2.0 wt%catalyst, with the yield of ester reaching 98.27%. The catalyst can be reused for 5 times without significant decline in its behavior. The struc?ture of the product was qualitatively analyzed by refractive index, FT-IR, 1H-NMR, and 13C-NMR.