Preparation,characterization of AlH3P2W18O62·nH2O and its catalytic performance in synthesis of adipic acid

doi:10.16085/j.issn.1000-6613.2015.04.019

Chemical Industry and Engineering Progree ›› 2015, Vol. 34 ›› Issue (04): 1014-1018.DOI: 10.16085/j.issn.1000-6613.2015.04.019

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Preparation,characterization of AlH₃P₂W₁₈O₆₂·nH₂O and its catalytic performance in synthesis of adipic acid

CAO Xiaohua¹, LI Shuigen², ZHOU Dezhi¹, LEI Yanhong¹, ZHAN Changchao¹

1. School of Chemistry and Chemical Engineering, Jiujiang College, Jiujiang 332005, Jiangxi, China;
2. School of New Energy Science and Engineering, Xinyu College, Xinyu 338000, Jiangxi, China

Received:2014-09-01 Revised:2014-11-02 Online:2015-04-05 Published:2015-04-05

Dawson结构磷钨酸铝催化剂的制备、表征及其催化合成己二酸

曹小华¹, 李水根², 周德志¹, 雷艳虹¹, 占昌朝¹

1. 九江学院化学与环境工程学院, 江西九江 332005;
2. 新余学院新能源科学与工程学院, 江西新余 338000

通讯作者: 曹小华(1978—),男,博士,副教授,从事多酸化学与石油化工方面的研究.E-mail caojimmy@126.com.
作者简介:曹小华(1978—),男,博士,副教授,从事多酸化学与石油化工方面的研究.E-mail caojimmy@126.com.
基金资助:
国家自然科学基金(21161009)、江西省自然科学基金(20132BAB203004、20122BAB213001)、江西省教育厅科技项目(GJJ10626、GJJ11613) 及九江学院科技项目(2013KJ005).

Abstract

Abstract: Dawson-type aluminum phosphotungstate(AlH₃P₂W₁₈O₆₂·nH₂O)was prepared by the double decomposition method,and characterized by FT-IR,SEM,XRD and EDS. The catalyst was used to catalyze synthesis of adipic acid from oxidation of cyclohexanone by 30% hydrogen peroxide. Orthogonal experiments were used to optimize reaction conditions. The optimum reaction conditions were:mass ratio of catalyst to cyclohexanon 7.6%,molar ratio of cyclohexanone to 30 percent hydrogen peroxide 100:450,reaction time 6.0h,reaction temperature 105℃,and isolated yield of adipic acid could reach 91.4%. The filtrate containing the catalyst could be concentrated by rotary evaporation and be reused five times by easy separation of the product after reaction,and isolated yield of adipic acid was still above 72.3%.

Key words: AlH₃P₂W₁₈O₆₂·nH₂O, 30%H₂O₂, adipic acid, preparation, catalysis, oxidation

摘要： 利用复分解法制备出Dawson结构磷钨酸铝AlH₃P₂W₁₈O₆₂·nH₂O催化剂,以30% H₂O₂为氧源,催化氧化环己酮合成了己二酸.采用FT-IR、SEM、XRD、EDS对催化剂进行表征.用正交实验法优化反应工艺条件,考察了反应时间、催化剂用量、反应温度和催化剂重复套用次数等因素对己二酸收率的影响.确定较优工艺条件为:w(催化剂)= 7.6%(基于环己酮质量),n(环己酮):n(30%H₂O₂)=100:450,反应时间6.0h,反应温度105℃.通过3次平行实验,己二酸平均收率为91.4%.催化剂重复使用5次,己二酸收率仍可达72.3%.

关键词: AlH₃P₂W₁₈O₆₂·nH₂O, 30%H₂O₂, 己二酸, 制备, 催化, 氧化

CLC Number:

CAO Xiaohua, LI Shuigen, ZHOU Dezhi, LEI Yanhong, ZHAN Changchao. Preparation,characterization of AlH₃P₂W₁₈O₆₂·nH₂O and its catalytic performance in synthesis of adipic acid[J]. Chemical Industry and Engineering Progree, 2015, 34(04): 1014-1018.

曹小华, 李水根, 周德志, 雷艳虹, 占昌朝. Dawson结构磷钨酸铝催化剂的制备、表征及其催化合成己二酸[J]. 化工进展, 2015, 34(04): 1014-1018.

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Preparation,characterization of AlH₃P₂W₁₈O₆₂·nH₂O and its catalytic performance in synthesis of adipic acid

Dawson结构磷钨酸铝催化剂的制备、表征及其催化合成己二酸

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