氨基硅油论文：氨基硅油的合成及其乳化

氨基硅油论文：氨基硅油的合成及其乳化 氨基硅油论文:氨基硅油的合成及其乳化 【中文摘要】氨基硅油可以赋予织物柔软、滑爽和丰满的效果,广泛应用于纺织、制革及日化行业。近年来,国内有机硅纺织印染助剂发展迅速,但国内有机硅产品不稳定,部分高档产品仍依赖进口。开发具有自主知识产权的有机硅柔软剂,提高纺织品质量,已成为国内纺织行业的迫切需求。目前国内外对氨基改性硅油的研究主要是针对传统的N-(β-氨乙基)氨丙基侧链改性硅油,对其它类型氨基硅油的研究则较少。考虑到硅氢加成反应的优点及含氢硅油价格适中,实验室合成也很方便,因此,本研究选用含氢硅油与不饱和氨催化加成反应来制取氨基硅油。通过对反应温度、加料时间、催化剂用量、投料比等影响因素的考察,得到最优化的氨基硅油合成条件,并采用红外光谱、核磁共振光谱等仪器手段对所制备的加成产物氨基硅油的结构进行了表征。通过化学滴定法确定了含氢硅油的Si-H键含量以及氨基硅油的氨值。实验结果表明,氨值会随着反应温度的升高、反应时间的延长呈上升趋势,最终趋于缓和。实验确定最佳反应条件为:反应温度为100?、反应时间为4h、催化剂用量为0.02%、烯丙基氨与含氢硅油的物质的量比为:1.2:1。在此条件下,所合成的氨基硅油氨值最高可达1.2mmol/g。以含氢硅油和实验室合成的氨基硅油为原料,进行了微乳化实验研究。考察了乳化剂类型和用量、乳化剂复配比例、助乳化剂种类、有机酸种类和用量以及温度等因素对硅油微乳化效果的影响,归纳出了各种因素的影响关系图,总结得到含氢硅油 和氨基硅油微乳化的工艺参数。 【英文摘要】The microemulsion of amino-silicon oil is extensive used in the industry of chemical engineering, textile, leather and cosmetic industries, and so on. In recent years, silicone textile printing and dyeing auxiliaries developed rapidly, but the domestic organic silicon products were instable, some high-end products still need import. Develop our own independent intellectual property of silicone softeners, improve the quality of textiles has become the urgent needs of the domestic textile industry.The studies of amino-modified silicone oil modified upon the traditional N-(β-aminoethyl) aminopropyl side chain is familiar, but other types of amino silicone oil’s research are less. For the hydrogen silicone easy to get, laboratory synthesis is also very convenient, so the amino-silicone was prepared by hydrosilylation of hydrogen-silicone and allyl amimo over the catalyst of PHB. Through the study of reaction temperature, dropping time, amount of catalyst, the feed ratio and other factors for amino silicone oil preparation, the structure amino silicone oil were characterized by the use of infrared spectrum and 1H-NMR spectrograms and other equipment. The amino-value of the amino-silicone and the content of the Si-H bond were determined by chemical titration.The results show that the amino-value rising with the reaction temperature rising and the reaction time extending, The optimal reactive condition was the toluene as solvent, reaction temperature 100?, reaction time 4h, the allyl amine molar ratio of hydrogen-silicone was 1.2:1, catalyst content of PHB was 0.02%. Under this condition, the amino-value is 1.2. And then in this condition using the hydrogen silicone oil and synthesis of amino silicone as raw materials, the experimental study of emulsion were conducted, suitable emulsifiers were chosen, together with the complex obtained amino silicone oil emulsion, the type and amount of emulsifier, emulsifier compound, emulsifier type, type and amount of organic acids and temperature on the effect of silicone oil emulsion were examined. The impact parameters of factors which were got from hydrogen silicone oil and amino-silicone oil emulsion process were summed up. On the basis of the experiments, a suitable emulsifier compound was prepared, and the micro-emulsion of amino-silicon oil and hydrogen silicone were obtained. 【关键词】氨基硅油 含氢硅油 烯丙基氨 硅氢加成 微乳化 【英文关键词】amino-silicon oil hydrogen-silicone ally amine hydrosililation reaction microemulsion 【备注】索购全文在线加好友:1.3.9.9.3.8848 同时提供论文写作一对一指导和论文发表委托服务 【目录】氨基硅油的合成及其乳化 摘要 5-6 Abstract 6 第1章 绪论 9-22 1.1 前言 9 1.2 硅油及其分类 9-11 1.3 氨基硅油 11-13 1.4 氨基硅油的合成 13-16 1.5 合成路线的确定 16 1.6 硅氢加成反应催化机理 16-19 1.6.1 离子加成机理 16-17 1.6.2 自由基加成机理 17 1.6.3 配位加成机理 17-19 1.7 硅油的乳化及其研究进展 19-21 1.7.1 普通乳液与微乳液的比较 20 1.7.2 微乳液的结构 20-21 1.8 课题的研究意义及内容 21-22 第2章 实验部分 22-29 2.1 实验试剂及仪器 22 2.2 实验原理 22-23 2.3 催化剂的选择 23-24 2.4 溶剂的选择 24-25 2.5 实验步骤 25 2.6 实验 分析 定性数据统计分析pdf销售业绩分析模板建筑结构震害分析销售进度分析表京东商城竞争战略分析 方法 25-29 2.6.1 摩尔质量的测定 26 2.6.2 氨值的测定 26-27 2.6.3 Si-H键含量的测定 27 2.6.4 产物的结构表征 27-29 第3章 氨基硅油的合成 29-45 3.1 产品表征 29-31 3.1.1 产品的IR分析 29-30 3.1.2 产物的~1H-NMR分析 30-31 3.2 正交实验 31-37 3.2.1 水平分析及正交实验表 32-33 3.2.2 正交实验结果 33-37 3.3 单因素实验 37-43 3.3.1 反应温度对产品氨值的影响 37-38 3.3.2 反应时间对产品氨值的影响 38-39 3.3.3 催化剂用量对产品氨值的影响 39-40 3.3.4 投料比对产品氨值的影响 40-41 3.3.5 保温时间对产品氨值的影响 41-43 3.4 重复性实验 43 3.5 本章小结 43-45 第4章 含氢硅油及氨基硅油的乳化 45-62 4.1 乳化剂的选择与复配 45-46 4.2 微乳化实验 46-48 4.2.1 微乳化主要实验试剂 46-47 4.2.2 微乳液的制备实验 47 4.2.3 硅油乳液的性能测试 47-48 4.3 含氢硅油的乳化 48-55 4.3.1 乳化剂种类对微乳化的影响 49-50 4.3.2 复合乳化剂用量对微乳液的影响 50-52 4.3.3 乳化温度对微乳液稳定性的影响 52 4.3.4 搅拌强度对微乳液的影响 52-53 4.3.5 助乳化剂的影响 53-54 4.3.6 有机酸的影响 54-55 4.4 氨基硅油的乳化 55-61 4.4.1 乳化剂种类对微乳化的影响 55-56 4.4.2 复合乳化剂用量对微乳液的影响 56-57 4.4.3 搅拌强度对微乳液的影响 57-58 4.4.4 乳化温度对微乳液稳定性的影响 58-59 4.4.5 助乳化剂的影响 59-60 4.4.6 有机酸对微乳液的影响 60 4.4.7 其他因素对微乳化的影响 60-61 4.5 小结 61-62 第5章 结论 62-64 参考文献 64-67 致谢 67-68 硕士期间发表的论文 68