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腰果酚甜菜碱型两性离子表面活性剂的合成与性能研究

发布时间:2018-04-16 20:03

  本文选题:腰果酚 + 氯醇醚 ; 参考:《东北石油大学》2015年硕士论文


【摘要】:本文以腰果酚、环氧氯丙烷为原料,四丁基溴化铵为催化剂合成中间体腰果酚氯醇醚,继而与二甲胺经胺化合成腰果酚叔胺,产物再与3-氯-2-羟基丙磺酸钠进行最终反应,获得产品--腰果酚甜菜碱,对合成的产品进行了红外表征并对表/界面张力、乳化性、热稳定性、与聚合物的复配性等进行了一系列的展开研究。本实验是在实验室前人基础上对合成该表面活性剂的工艺进行了改进,将缩水甘油醚中间体法改为氯醇醚中间体法,该方法具有反应条件低、操作简单、催化剂使用量少、中间产物处理方便、叔胺转化率高等优点。最终产品及中间体的红外谱图显示,合成的物质均具有目标产物的特征吸收峰可初步判断为目标产品。对中间产物腰果酚叔胺设计4因素3水平的正交试验,以确定最佳反应条件,实验结果为:n(腰果酚氯醇醚):n(二甲胺):n(氢氧化钠)=1:2.5:1.4;反应时间为6h;反应温度为40℃。在此条件下进行3次平行试验,腰果酚叔胺产率较为理想,达到90%。通过旋滴法测试表面活性剂降低油-水界面张力的性能,实验表明实验室自制的腰果酚甜菜碱可以高效地降低油水界面张力,当浓度为0.5~3.0g/L时仍能保持良好的性能,界面张力均可达到10-4~10-3mN/m,而且在高温(55~95℃)、高盐(32308~64616mg/L)条件下均能满足驱油过程中达到超低界面张力(10-3mN/m)的要求。采用滴体积法测定该表面活性剂的表面张力,实验表明低浓度表面活性剂溶液即可达到临界胶束浓度,其中cmc=3.17×10-4mol/L,此时表面张力γcmc=32.86mN/m。通过分水时间法来反映表面活性剂的乳化性能,实验表明单一的该表面活性剂乳化性能较差,在0.5~3.0g/L浓度范围内,分水时间短,约为35s左右,该性能仍亟待提高。通过测试表面活性剂在42天模拟地层温度(85℃)的条件下界面张力的变化来反映该表面活性剂热稳定,实验表明,该表面活性剂的表面活性会随着时间的推移有所降低,导致油-水界面张力的增长,但仍能保持10-3mN/m,可以满足采油需要。与聚丙烯酰胺的复配使用使其性能更为优越:加入一定量(0.5~1.5g/L)的聚合物可使界面张力达到10-6~10-4mN/m;cmc有所降低,对γcmc无太大影响:聚合物浓度为0.5g/L时cmc=2.75×10-4mol/L,γcmc=34.96mN/m;聚合物浓度为1.5g/L时cmc=1.38×10-4mol/L,γcmc=35.72m N/m;聚合物浓度为1.0~1.5g/L时,分水时间大幅度提高(约为200~1200s),乳化性能得到改善;聚合物的加入使体系热稳定性更佳,基本呈稳定状态,且在一定程度上降低界面张力至10-5~10-4mN/m。
[Abstract]:In this paper, cashew fruit phenol and epichlorohydrin were used as raw materials, and tetra ammonium bromide was used as catalyst to synthesize the intermediate cashew fruit phenol chlorol ether, which was then aminated with dimethylamine to synthesize cashew phenol tertiary amine, and the final reaction was carried out with sodium 3-chloro-2-hydroxypropyl sulfonate.The synthesized product was characterized by IR and a series of studies were carried out on the surface / interfacial tension, emulsification, thermal stability and the compatibility with polymer.In this experiment, the synthetic process of the surfactant was improved on the basis of laboratory predecessors. The method was changed from the intermediate of glycidyl ether to the intermediate of chloroalcohol ether. The method has the advantages of low reaction conditions, simple operation and less catalyst usage.The intermediate product is easy to deal with and the conversion rate of tertiary amine is high.The infrared spectra of the final product and the intermediate show that the synthesized substance has the characteristic absorption peak of the target product and can be preliminarily judged as the target product.The orthogonal design of 4 factors and 3 levels of the intermediate product cashew fruit phenol tertiary amine was carried out to determine the optimum reaction conditions. The experimental results showed that the reaction temperature was 40 鈩,

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