【摘要】：利用磷鎢酸(PTA)與1,2,3-三氮唑-4,5-二羧酸(TDA)在水溶液中的反應(yīng),合成了一種新的固體酸TDA-PTA,采用X射線粉末衍射(XRD)、掃描電鏡(SEM)、紅外光譜(FT-IR)、熱重(TG)以及電位滴定等方法對其進行了表征,并以油酸與甲醇的酯化反應(yīng)為探針反應(yīng),考察了其催化性能,探討了催化劑用量、醇酸物質(zhì)的量比、反應(yīng)時間、反應(yīng)溫度以及催化劑重復(fù)利用次數(shù)等對產(chǎn)物收率的影響。結(jié)果表明,TDA-PTA不僅保留有磷鎢酸典型的Keggin結(jié)構(gòu),而且具有較強的酸強度;經(jīng)修飾后,催化劑具有規(guī)整的球形形貌,比表面積明顯大于磷鎢酸;TDA-PTA在油酸與甲醇的酯化反應(yīng)中表現(xiàn)出了優(yōu)良的催化活性,尤其顯示出好的重復(fù)利用性,六次使用后,仍得到86.8%的油酸甲酯產(chǎn)率,催化劑的物相以及Keggin結(jié)構(gòu)沒有明顯變化。
[Abstract]:A new solid acid TDA-PTA, was synthesized by the reaction of phosphotungstate TDA-PTA, with 1, 2, 3-triazole-4, 5-dicarboxylic acid (TDA) in aqueous solution. X-ray powder diffraction (XRD), scanning electron microscope (SEM),) was used to synthesize a new solid acid TDA-PTA,. It was characterized by infrared spectroscopy (FT-IR), thermogravimetric (TG) and potentiometric titration. The catalytic performance of oleic acid and methanol was investigated by esterification of oleic acid with methanol as probe reaction. The amount of catalyst and the ratio of alcohol to acid were discussed. The effects of reaction time, reaction temperature and catalyst reuse times on the yield of the product. The results show that TDA-PTA not only retains the typical Keggin structure of phosphotungstic acid, but also has strong acid strength. After modification, the catalyst has a regular spherical morphology, and the specific surface area of the catalyst is obviously larger than that of phosphotungstic acid. TDA-PTA showed excellent catalytic activity in the esterification of oleic acid with methanol, especially showed good reusability. After six times of use, the yield of methyl oleate was 86.8%. The phase of the catalyst and the structure of Keggin did not change obviously.
【作者單位】： 聊城大學(xué)化學(xué)化工學(xué)院;
【基金】：supported by the National Natural Science Foundation of China(21101086) the Doctor Foundation of Shandong Province(BS2010CL011) the Foundation of Liaocheng University
【分類號】：TE667

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