磷钨酸铵铝复合盐催化合成柠檬酸三丁酯
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湖南省自然科学基金(2018JJ3475),湖南省知识产权战略实施专项(2017Z4013G)


Synthesis of Tributyl Citrate Catalyzed by Mixed Salt of Ammonium and Aluminum Phosphotungstate
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Hunan Provincial Natural Science Foundation of China (2018JJ3475); Hunan Provincial Intellectual Property Strategy Implementation Project of China (2017Z4013G).

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    摘要:

    制备了系列金属离子与NH4+复合掺杂磷钨酸盐催化剂,并将其应用于酯化合成柠檬酸三丁酯的反应中。其中,(NH4)0.5Al2/3H0.5PW12O40(I)的催化活性较高,且成本相对较低。在正丁醇与柠檬酸的物质的量之比为4:1,催化剂I用量1.5%,温度150℃,时间3h的反应条件下,柠檬酸三丁酯的收率达到97.1%。对催化剂I的元素组成、结构、表面酸强度与酸密度进行了表征。I的表面酸强度(H0)为-14.52~-13.75,表面酸密度为2.57 mmol/g,高于传统的单一掺杂磷钨酸盐。此外,经3次使用后,催化剂I的活性没有明显下降。

    Abstract:

    Metal ion and ammonium co-doped phosphotungstate were prepared and used as catalyst for the synthesis of tributyl citrate. Among them, (NH4)0.5Al2/3H0.5PW12O40 (I) showed relatively high catalytic activity and low cost. And the yield of tributyl citrate reached 97.1% with 4: 1 molar ratio of n-butanol to citric acid using 1.5% I as catalyst at 150oC in 3 h. The element composition, structure, surface acid strength and acid density of I were also characterized. The surface acid strength of I was in the range of -14.52 to -13.75, and the acid density of I reached 2.57 mmol/g, which was higher than that of traditional single cation doped phosphotungstate. In addition, the catalytic activity of I had no viewable change after 3 runs.

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周喜,李泽贤,张超.磷钨酸铵铝复合盐催化合成柠檬酸三丁酯[J].精细化工,2019,36(5):

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  • 收稿日期:2018-08-20
  • 最后修改日期:2018-12-24
  • 录用日期:2018-12-25
  • 在线发布日期: 2019-03-28
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