乌桕籽油制备环氧脂肪酸乙酯及增塑PVC研究
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摘要
选用具有高碘值的乌桕籽油为原料,通过酯交换和原位环氧化法制备脂肪酸乙酯和环氧脂肪酸乙酯,并分别采用条件法和正交实验法研究了合成工艺条件。结果表明,梓油与乙醇酯交换的反应条件为:梓油与乙醇物质的量之比为7∶1,催化剂用量为梓油质量的1.6%,在65℃下恒温搅拌回流反应2h,转化率在76.7%左右;脂肪酸乙酯环氧化的最佳工艺条件为:每百克脂肪酸乙酯需甲酸14g,双氧水113g,反应温度控制在55℃,反应时长为3h,所得产物环氧值为5.5。并通过凝胶色谱和红外光谱验证了反应产物。软质PVC薄膜性能测试表明:环氧脂肪酸乙酯(EFAEE)可有效降低PVC塑料的结晶度,并具有较好的增塑性能,其断裂伸长率优于DOP;EFAEE可有效提升PVC材料的热稳定性,其增塑的PVC薄膜的玻璃化温度也较DOP增塑薄膜低12.67℃,并可根据需要与DOP复配使用。
Choose stillingia oil which has high iodine value as raw material,through transesterification,epoxidation reaction,synthesized an Epoxidized plasticizer epoxy fatty acid ethyl ester.And study the synthetic process through condition experiment and orthogonal experiments respectively,The results show that,the best conditions for ester exchange between stillingia oil with alcohol,The ratio of the amount of substance of stillingia oil and alcohol is 7:1,the quality of catalyst is 1.6% of the stillingia oil,the reaction temperature at 65 ℃,reaction time is 2 h,percent conversion is around76.7%;the Optimum process conditions of epoxidation is use formic acid 14 g,hydrogen peroxide 113 g per hundred grams of fatty acid ethyl ester,the reaction temperature control in 55 ℃,the reaction time is 3 h,the epoxide number of product was 5.5.finally the products were validated by gel chromatography and infrared spectrum.
Choose stillingia oil which has high iodine value as raw material,through transesterification,epoxidation reaction,synthesized an Epoxidized plasticizer epoxy fatty acid ethyl ester.And study the synthetic process through condition experiment and orthogonal experiments respectively,The results show that,the best conditions for ester exchange between stillingia oil with alcohol,The ratio of the amount of substance of stillingia oil and alcohol is 7:1,the quality of catalyst is 1.6% of the stillingia oil,the reaction temperature at 65 ℃,reaction time is 2 h,percent conversion is around76.7%;the Optimum process conditions of epoxidation is use formic acid 14 g,hydrogen peroxide 113 g per hundred grams of fatty acid ethyl ester,the reaction temperature control in 55 ℃,the reaction time is 3 h,the epoxide number of product was 5.5.finally the products were validated by gel chromatography and infrared spectrum.
引文
[1]李祥庆,沈凯华,严秋钫.环氧脂肪酸甲酯的合成研究进展及应用[J].塑料助剂,2016(4):23-27.
[2]程正载,林素素,王洋,等.菜籽油非均相催化环氧化合成环氧脂肪酸甲酯[J].中国油脂,2012,37(8):49-52.
[3]刘振兴,聂小安,王义刚.白花树果油环氧脂肪酸甲酯增塑剂的制备及其应用[J].现代化工,2014,34(2):97-100.
[4]贾茂林,王芳,陈意,等.地沟油改性制备PVC用环氧脂肪酸甲酯增塑剂[J].中国塑料,2014,28(11):82-87.
[5]尹立军,陆向红,卢美贞,等.乌桕梓油中四酯的分离及鉴定[J].中国粮油学报,2012,27(8):52-56.
[6]李科,李翔宇,蒋剑春,等.质量法:一种计算油脂甲酯化转化率的新方法研究[J].林产化学与工业,2011,31(2):43-47.
[2]程正载,林素素,王洋,等.菜籽油非均相催化环氧化合成环氧脂肪酸甲酯[J].中国油脂,2012,37(8):49-52.
[3]刘振兴,聂小安,王义刚.白花树果油环氧脂肪酸甲酯增塑剂的制备及其应用[J].现代化工,2014,34(2):97-100.
[4]贾茂林,王芳,陈意,等.地沟油改性制备PVC用环氧脂肪酸甲酯增塑剂[J].中国塑料,2014,28(11):82-87.
[5]尹立军,陆向红,卢美贞,等.乌桕梓油中四酯的分离及鉴定[J].中国粮油学报,2012,27(8):52-56.
[6]李科,李翔宇,蒋剑春,等.质量法:一种计算油脂甲酯化转化率的新方法研究[J].林产化学与工业,2011,31(2):43-47.