【作者】 郭能民；

【导师】 安秋凤；

【作者基本信息】 陕西科技大学 ， 有机化学， 2012， 硕士

【摘要】 本论文应用种子乳液聚合方法，以阴离子型乳化剂A-51和非离子型乳化剂AEO-9为复合乳化剂体系，制备了阴离子型丙烯酸酯乳液。探讨了单体含量和配比、乳化剂含量和配比以及聚合反应工艺条件对乳液性能的影响。实验结果表明，当丙烯酸丁酯和苯乙烯质量比为1~3，交联单体质量为5~10%，丙烯酸和丙烯酸羟丙酯质量比为1~3时，乳化剂含量为2~5%，阴非离子质量比为1到3，制备的乳液及乳胶膜性能较优。聚合反应温度控制在80~85℃，搅拌速率控制在300r/min左右，对乳液聚合有利。以阳离子单体甲基丙烯酸二甲氨基乙酯和丙烯酸酯类单体为原料，V50为引发剂，制备出性能稳定的阳离子型丙烯酸酯硬挺剂。对该丙烯酸酯硬挺剂进行了FT–IR，Zeta电位和TEM分析表征，结果表明，丙烯酸类单体都参与了聚合反应，与目标产物基本吻合；乳胶粒表面带正电荷，乳胶粒的Zeta电位为+70.43mV，乳胶粒稳定性较好；乳胶粒粒径呈正态分布，平均粒径为85.84nm，乳胶粒分散较好；乳胶粒呈圆球核壳状，无团聚现象。探讨了乳化剂用量及配比、软硬单体配比对乳液制备及性能的影响，当苯乙烯和丙烯酸丁酯质量比为1~3，阳非离子质量比为1~3，乳化剂含量为1~4%时，乳液性能较佳。探讨出该硬挺剂整理的较佳工艺为：配制整理液（100g蒸馏水中加入10.8g乳液）→浸轧整理液（二浸二轧，轧液率约80%）→烘干（100℃，5min）→焙烘（160℃，3min）。在纯丙烯酸酯乳液制备的基础上，采用有机硅对丙烯酸酯乳液进行改性，制备得到阴离子型有机硅改性丙烯酸酯乳液。制备得到的硅丙乳液外观为乳白色泛蓝光，乳液耐钙离子相对稳定性良好，有机硅的加入明显改变了纯丙烯酸酯胶膜的发粘性能，并且增强了胶膜的柔软性能，在皮革织物表面处理、室内装潢和工业防护等领域具有巨大的应用价值。对该有机硅改性丙烯酸酯乳液进行了FT–IR，Zeta电位和TEM分析表征，结构分析表明，丙烯酸类单体和有机硅都参与了聚合反应，与目标产物基本吻合；乳胶粒表面带负电荷，乳胶粒的Zeta电位为-32.99mV，乳胶粒稳定性较好；乳胶粒粒径呈正态分布，平均粒径为96.5nm，乳胶粒分散较好；乳胶粒呈圆球状，无团聚现象。探讨了乳化剂用量及配比、单体配比、偶联剂用量和有机硅含量对乳液制备及其性能的影响，实验结果显示，使用A-51和AEO-9的复合乳化剂体系，能以较少的乳化剂用量制备凝胶率和吸水率都较低的硅丙乳液，具有较好的应用和推广价值。同时，也探讨了预乳化工艺条件对硅丙乳液制备的影响，实验结果显示，预乳化工艺条件对硅丙乳液的制备至关重要，能够有效地降低乳液凝胶率。更多还原

【Abstract】 Anionic acrylate copolymer latex were synthesized by seeding emulsionpolymerization with A-51and AEO-9as the emulsifiers. Effect of the ratio andamount of emulsifier, monomer and the synthesized process on emulsion werediscussed.The optimal synthesis conditions were the mass ratio between BA andST of1~3, the crosslinking monomer mass fraction of5~10%, the mass ratiobetween AA and HPA of1~3, A-51and AEO-9mass fraction of2~5%, the massratio between A-51and AEO-9of1~3. The emulsion and the latex film had thebest integrated performance. The polymerization temperature was controlled at80~85℃and the best stirring rate of the reaction was300r/min.The stable cationic polyacrylate stiffening agent was prepared using acrylicester and cationic methacrylic acid ethyl amide dimethyl(DM) as raw materialand α,α-azodiisobutyramidine dihydrochloride(V50) as initiator. Theperformance of cationic polyacrylate stiffening agents were characterized byinfrared spectro scopy(FT-IR), TEM and Zeta potential. The results showed thatall of the acrylic monomers were involved in the polymerization reaction andconsisted with the target product. The Zeta potential of the latex particle was+70.43mV and the emulsion was stable. The latex particle size showed a normaldistribution and dispersed very well, and the average particle size was85.84nm.The latex particle was cylindrical ball like core-shell, and non-agglomeration.Effect of the ratio and amount of emulsifier, the ratio of hard and soft monomeron emulsion were discussed. The optimal synthesis conditions were the massratio between ST and BA of1~3，1631and AEO-9mass fraction of1~4%, themass ratio between1631and AEO-9of1~3. The emulsion had the bestintegrated performance. The process for finishing was explored as follows:preparation of the finishing solution (10.8g emulsion was added in the100gdistilled water)→padding finishing agent (two dip two rolling, rolling fluid rate of about80%)→drying (100℃,5min)→baking (160℃,3min).On the basis of synthesizing acrylate copolymer latex, silicone was used tosynthesize the silicone-modified acrylate copolymer latex. The modified latexwas transparent or translucent and bright bluish. Emulsion resistant to thecalcium ion was relatively stable. The sticky and softy performance of the filmwas proved significantly because of the organic silicone. The silicone-modifiedacrylate copolymer latex had a broad foreground to apply in many fields such asfinishing coatings of leather and fabric, inner decoration and protecting coatingin industry. The performance of silicone-acrylic emulsion were characterized byinfrared spectro scopy(FT-IR), TEM and Zeta potential. The results showed thatall of the acrylic monomers and silicone was involved in the polymerizationreaction and consisted with the target product. The Zeta potential of the latexparticle was-32.99mV and the emulsion was stable. The latex particle sizeshowed a normal distribution and dispersed well, and the average particle sizewas96.5nm. The latex particle was cylindrical ball and non-agglomeration.Effect of the ratio and amount of emulsifier, the ratio of hard and soft monomer,the content of the silicone and the coupling agent on emulsion were discussed.The results showed that silicone-acrylic emulsion can be synthesized by usingvery little emulsifier. The silicone-modified acrylate copolymer latex had a broadapplication and promotion value for its low gelfraction and water absorption.Meanwhile, the impact of the pre-emulsification process conditions on thepreparation of silicone-modified acrylate latex was explored. The experimentalresults showed that pre-emulsion process conditions on the preparation of theemulsion was essential, and the process can reduce the rate of emulsion gelfraction effectively.更多还原