| 斯志昆，范明明，张萍波，等.α-磷酸锆@磺酸基固体酸催化剂的表征及其催化酯化反应的研究[J].中国油脂,2019,44(4):.[SI Zhikun, FAN Mingming, ZHANG Pingbo，etc.Characterization of α-ZrP@SO3H solid acid catalyst and its catalytic performance in esterification[J].China Oils and Fats,2019,44(4):.] |
| α-磷酸锆@磺酸基固体酸催化剂的表征及其催化酯化反应的研究 |
| Characterization of α-ZrP@SO3H solid acid catalyst and its catalytic performance in esterification |
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| DOI： |
| 中文关键词: α-磷酸锆 KH-580 固体酸催化剂 酯化反应 |
| 英文关键词:α-ZrP KH-580 solid acid catalyst esterification |
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| 中文摘要: |
| 以层状结构的α-磷酸锆为载体，用四正丁基氢氧化铵对其剥离改性，再连接上γ-巯丙基三乙氧基硅烷（KH-580），通过氧化和酸化两步，制备出一种新型的固体酸催化剂α-磷酸锆@磺酸基。通过XRD、SEM、BET、TGA、FT-IR等手段对该催化剂进行表征。结果表明：制备的催化剂比表面积增大，结晶度降低，酸强为2.43 mmol/g；FT-IR表征显示—SO3H的存在，证明α-磷酸锆被成功磺化。将该催化剂应用于月桂酸与甲醇的催化酯化反应中，对反应条件进行优化，发现在反应温度90?℃、反应时间5 h、酸醇摩尔比1∶?30、催化剂用量3%(以月桂酸质量计)时，酯化率达到97%以上。该催化剂使用3次后，仍然保持着较高的催化活性，酯化率为87.48%。 |
| 英文摘要: |
| The layered α-ZrP was exfoliated by tetra-n-butylammonium hydroxide, masked as E-ZrP, then KH-580 was gifted on the surface of it, after oxidation and acidification, α-ZrP@SO3H was successfully prepared. The catalyst was characterized by XRD, SEM, BET, TGA and FT-IR. The results showed that the prepared catalyst had a larger specific surface area and a lower crystallinity, and its acid strength was 2.43 mmol/g. FT-IR analysis indicated that —SO3H was successfully gifted on α-ZrP. The catalyst was used in the esterification of lauric acid and methanol, and the esterification conditions were optimized as follows: temperature 90?℃, time 5 h, molar ratio of acid to methanol 1∶?30, catalyst dosage 3%(on the basis of lauric acid mass). Under the optimal conditions, the esterification rate was more than 97%. After used for three times, the catalyst still maintained high catalytic activity, and the esterification rate was 87.48%. |
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