Journal of Liaoning Petrochemical University

Journal of Liaoning Petrochemical University ›› 2015, Vol. 35 ›› Issue (6): 1-5.DOI: 10.3696/j.issn.1672-6952.2015.06.001

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Tungstate Phosphorus Compounds Catalytic Synthesis of Acetals

Yang Xing, Wang Xin, Chen Ping   

  1. Liaoning Shihua University, Fushun Liaoning 113001, China)
  • Published:2015-12-25 Online:2015-12-10

磷钨酸盐催化苯甲醛的缩醛化反应

杨 星,王 欣,陈 平   

  1.     
    ( 辽宁石油化工大学, 辽宁抚顺1 1 3 0 0 1)
  • 通讯作者: 王欣( 1 9 8 1 - ) , 女, 博士, 讲师, 从事有机催化方面的研究; E - m a i l : z i p p l e 5@1 6 3. c o m。
  • 作者简介:杨星( 1 9 8 9 - ) , 女, 硕士研究生, 从事有机合成及催化方面的研究; E - m a i l : 8 6 2 6 2 1 7 9 8@q q. c o m。
  • 基金资助:
    辽宁省自然科学基金项目( 2 0 1 2 0 2 1 2 8) 。

Abstract: A l PW1 2O4 0 was prepared by phosphotungstic acid and Al(NO3)3•9H2O and used as catalyst to catalyze the condensation of benzaldehyde with 1,2propylene glycol using cyclohexane as water trapping reagent. The reaction condition including catalyst pretreatment temperature, amount of cyclohexane, molar ratio of starting materials, reaction time, dosage of catalyst and oil bath temperature were investigated. The results show that A l PW1 2O4 0 is a good catalyst for the condensation of benzaldehyde with 1, 2propylene glycol. The optimal reaction condition were as followed:n (alcohol)∶n(aldehyde)=2.0∶1, catalyst pretreatment at 150 ℃, 0.7 g of catalyst, 7 mL of cyclohexane and 2.6% total mass of starting material at 130 ℃ for 3 h. The conversion of benzaldehyde can reach up to 98.83% under optimal condition.

Key words: Phosphotungstic acid, Benzaldehyde 1,2propylene glycol acetal, 1,2propylene glycol, Benzaldehyde, Catalysi

摘要: 利用磷钨酸( HPW) 和 A l ( NO3) 3·9H2O合成 A l PW1 2O4 0, 以其为催化剂、 苯甲醛和1, 2 - 丙二醇为原料、 环己烷为带水剂, 进行缩合反应, 考察了催化剂的预处理温度、 带水剂体积、 原料的物质的量比、 反应时间、 催化剂质量及油浴温度等因素对苯甲醛转化率的影响。结果表明, 最佳反应条件为: 催化剂预处理温度为1 5 0℃, 带水剂体积为7mL, n( 醇) ∶n( 醛) =2. 0∶1, 反应时间为3h, 催化剂质量为0. 7g, 油浴温度为1 3 0℃。在最佳反应条件下进行反应, 苯甲醛的转化率达到9 8. 8 3%。

关键词: 磷钨酸, 苯甲醛1, 2 - 丙二醇缩醛, 1, 2 - 丙二醇, 苯甲醛, 催化

Cite this article

Yang Xing, Wang Xin, Chen Ping. Tungstate Phosphorus Compounds Catalytic Synthesis of Acetals[J]. Journal of Liaoning Petrochemical University, 2015, 35(6): 1-5.

杨 星,王 欣,陈 平. 磷钨酸盐催化苯甲醛的缩醛化反应[J]. 辽宁石油化工大学学报, 2015, 35(6): 1-5.