酶法催化漆蜡合成漆蜡基异丙酯工艺研究
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摘要
以脂肪酶为催化剂,催化漆蜡与异丙醇进行酯交换反应合成漆蜡基异丙酯。首先采用傅里叶红外光谱对合成产物进行结构表征,然后采用单因素试验和正交试验对酯交换反应条件进行了优化,并对最佳条件下合成的漆蜡基异丙酯的组成进行了GC-MS分析。结果表明:在脂肪酶催化下,漆蜡可与异丙醇反应生成目标产物; Novozyme 435脂肪酶催化酯交换反应的最佳工艺条件为醇蜡比4∶1、脂肪酶加量10 g/L、反应温度55℃、反应时间36 h,在此条件下酯交换率为86. 7%,漆蜡基异丙酯的酸价(KOH)为3. 28 mg/g;漆蜡基异丙酯主要由棕榈酸异丙酯(73. 64%)、油酸异丙酯(19. 39%)、硬脂酸异丙酯(6. 15%)和亚油酸异丙酯(0. 82%)组成。
Synthesis of isopropyl ester from lacquer wax by transesterification with lipase catalyst was studied. The structure of the synthesized product was characterized by FT-IR. The transesterification conditions were optimized by single factor experiment and orthogonal experiment,and the compositions of the product synthesized under the optimal conditions were analyzed by GC-MS. The results showed that the isopropyl ester could be obtained by transesterification of lacquer wax and isopropanol with lipase as catalyst. The optimal conditions were obtained as follows: ratio of isopropanol to lacquer wax 4∶ 1,Novozymes 435 lipase dosage 10 g/L,reaction temperature 55 ℃,reaction time 36 h. Under these conditions,the transesterification rate was 86. 7%,and the acid value of isopropyl ester from lacquer wax was 3. 28 mgKOH/g. The product was mainly composed of isopropyl palmitate (73. 64%), isopropyl oleate (19. 39%),isopropyl stearate (6. 15%) and isopropyl linoleate (0. 82%).
Synthesis of isopropyl ester from lacquer wax by transesterification with lipase catalyst was studied. The structure of the synthesized product was characterized by FT-IR. The transesterification conditions were optimized by single factor experiment and orthogonal experiment,and the compositions of the product synthesized under the optimal conditions were analyzed by GC-MS. The results showed that the isopropyl ester could be obtained by transesterification of lacquer wax and isopropanol with lipase as catalyst. The optimal conditions were obtained as follows: ratio of isopropanol to lacquer wax 4∶ 1,Novozymes 435 lipase dosage 10 g/L,reaction temperature 55 ℃,reaction time 36 h. Under these conditions,the transesterification rate was 86. 7%,and the acid value of isopropyl ester from lacquer wax was 3. 28 mgKOH/g. The product was mainly composed of isopropyl palmitate (73. 64%), isopropyl oleate (19. 39%),isopropyl stearate (6. 15%) and isopropyl linoleate (0. 82%).
引文
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[4]张思桂.实用精细品化学品手册[M].北京:化学工业出版社,1996.
[5]陈顺玉,田文慧,谢珍珍.生物柴油降凝剂脂肪酸异丙酯的制备及降凝效果的研究[J].福建师范大学学报,2009,25(4):62-66.
[6]LEE I,JOHNSON L A,HAMMOND E G.Use of branchedchain esters to reduce the crystallization temperature of biodiesel[J].J Am Oil Chem Soc,1995,72(10):1155-1160.
[7]姜思炜,夏凡,蔡莉,等.废弃油脂甘油酯化降酸及制备生物柴油[J].中国油脂,2016,41(12):92-95.
[8]王晓春,高甲君,张新春.棕榈酸异丙酯的性能、合成及在化妆品中的应用[J].四川日化,1993(4):18-20.
[9]卜文娟,耿全华,阮复昌.棕榈酸异丙酯的合成研究进展[J].香料香精化妆品,2010,12(6):49-52.
[10]魏盼中,曾平,张浴沂,等.棕榈酸异丙酯的合成工艺研究[J].精细与专用化妆品,2017,25(6):37-39.
[11]李静,李法社,徐娟,等.油酸异丙酯的合成及其对生物柴油低温流动性研究[J].广东化工,2011,38(6):5-6.
[12]INUI K,KURABAYASHI T,SATO S.Direct synthesis of ethylacetate from ethanol over Cu-Zn-Zr-Al-O catalyst[J].Appl Catal A-Gen,2002,237(12):53-61.
[13]井强山,王振海,王慎典.直接酯化法制备棕榈酸异丙酯工艺路线探讨[J].信阳师范学院学报(自然科学版),1998,11(3):291-293.
[14]张飞龙,张武桥,魏朔南.中国漆树资源研究及精细化应用[J].中国生漆,2007,26(2):36-51.
[15]张飞龙,郭勇智,王尚林,等.漆树资源的开发和利用[J].中国生漆,1995,14(1):42-50.
[16]张瑞琴,张飞龙.漆树果实资源开发态势分析[J].中国生漆,2000,19(3):23-30.
[17]李润兰,叶洪权.漆蜡脂肪酸的利用研究[J].中国生漆,1998,17(11):44-45.
[18]李翔宇,蒋剑春,王奎,等.生物柴油酯化反应机理和影响因素分析[J].生物质化学工程,2010,44(3):1-5.