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1、浙 江 理 工 大 学 材 料 与 纺 织 学 院毕业设计(论文)诚信声明我谨在此保证：本人所写的毕业设计(论文)，凡引用他人的研究成果均已在参考文献或注释中列出。设计(论文)主体均由本人独立完成，没有抄袭、剽窃他人已经发表或未发表的研究成果行为。如出现以上违反知识产权的情况，本人愿意承担相应的责任。声明人(签名)：年 月 日摘 要聚丙烯酸酯因成膜性好，粘结性强，耐热等优点而被广泛应用于涂料印花粘合剂，但其存在胶膜硬度大，耐水性差，冷脆热黏等缺点而影响了印花产品的质量。聚硅氧烷疏水性强，链段柔顺，将含有乙烯基的聚硅氧烷对聚丙烯酸进行改性，能有效改善聚丙烯酸酯粘合剂的缺点，提高涂料印花的色牢度与
2、手感。因此本文合成出双端乙烯基聚二甲基硅氧烷（diVi-PDMS） ，并将其用于改性聚丙烯酸酯，制得一种新型涂料印花粘合剂，使得涂料印花织物兼具良好的耐摩擦牢度和手感。主要研究内容分为两部分：第一部分：双端乙烯基聚二甲基硅氧烷的合成及表征。采用 1,3-二乙烯基-1,1,3,3-四甲基二硅氧烷和八甲基环四硅氧烷为原料，以三氟甲基磺酸为催化剂，通过阳离子开环聚合合成双端乙烯基聚硅氧烷（diVi-PDMS） 。研究了催化剂用量，反应温度和反应时间对产物转化率和封端率的影响，优化了合成工艺条件并采用红外光谱（FTIR）和核磁共振（1H-NMR）对产物结构进行表征。结果表明：双端乙烯基聚硅氧烷（diV
3、i-PDMS）的优化工艺条件为催化剂用量 0.15%，反应温度 70，反应时间 6h，产物转化率达到 91%,FTIR 和1H-NMR 谱图分析表明了产物为双端乙烯基聚硅氧烷（diVi-PDMS)。第二部分：diVi-PDMS 改性聚丙烯酸酯细乳液的合成及其性能研究。采用自制的双端乙烯基聚硅氧烷（diVi-PDMS）改性聚丙烯酸酯，通过细乳液聚合制得有机硅改性聚丙烯酸酯乳液。研究了传统乳化剂（SDS:O-10）/可聚合乳化剂（V-20S）配比及用量，有机硅单体分子量对聚合稳定性、乳液性能、胶膜性能及涂料印花性能的影响，并用红外光谱仪（FTIR） 、热重分析仪（TG） 、差示扫描量热仪（DSC）
4、等对聚合物的结构和性能进行测定和表征。结果表明：乳化剂配比为 1.5:1:1、用量为 6%时，聚合稳定性及乳液稳定性良好，乳液粒径小，分布窄，且相比传统乳化剂，复配可聚合乳化剂明显提升胶膜的力学性能；随着 diVi-PDMS 分子量的增大，胶膜交联度降低，耐水性降低，力学性能变差，涂料印花织物耐摩擦牢度变差，当 diVi-PDMS 分子量为约为 1600 时，胶膜水接触角为 94.9，吸水率为 7.39%，印花织物干、湿摩擦牢度可达 4 级，手感柔软。红外分析表明产物为有机硅改性聚丙烯酸酯，DSC 和 TG 分析表明经改性后聚合物的玻璃化温度降低，热分解温度提高，耐热稳定性增强。i论文研究表明
5、，以双端乙烯基聚硅氧烷（diVi-PDMS）为改性单体，采用细乳液聚合，制备有机硅改性聚丙烯酸酯乳液粘合剂，应用于印花涂料，其印花织物耐干、湿摩擦牢度均达到 4 级，手感柔软，印花织物具有良好的耐摩擦牢度，又具有柔软的手感。关键词：聚丙烯酸酯；双端乙烯基聚硅氧烷；细乳液聚合；涂料印花iiAbstractPolyacrylate has been widely used as pigment printing binder because of its advantages, such as good film-forming ability, strong adhesion, good hea
6、t resistance, etc. However, the polyacrylate generally exists many defects which affect the quality of the printing products, such as high hardness, poor property of waterproof, hot sticky-cool brittle performance of the latex film. There are many advantages in polydimethylsiloxane (PDMS), such as g
7、ood hydrophobicity and flexibility. PDMS which contains vinyl group was applied in the modification of polyacrylate, in order to improve the color fastness and handle of pigment printing fabric. In this paper, a double Vinyl-terminated polydimethylsiloxane (diVi-PDMS) was synthesized and applied in
8、the preparation of silicone-modified polyacrylate emulsion for pigment printing binder, so as to be good color fastness and softer handle of pigment printed fabric. There are two parts in this paper.Part 1: Synthesis and characterization of diVi-PDMSIn this part, diVi-PDMS was synthesized by ring-op
9、ening polymerization reaction of cationic with 1,3-divinyl-1,1,3,3-tetramethyldisiloxane and Octamethyl cyclotetrasiloxane, using trifluoromethanesulfonic acid as a catalyst. The influences of reaction factors such as amount of catalyst, reaction temperature and time on the conversion rate and yield
10、 of termination were investigated, then the synthesis conditions were optimized and the structure of product was characterized by FTIR and 1H-NMR. The results showed that the optimal condition for the preparation of diVi-PDMS was that the amounts of catalyst were 0.2%, reaction temperature was 70 an
11、d reaction time was 6h. In the optimal condition, the conversion rate can reach 91%. The results of FTIR and 1H-NMR analysis indicated that the structure of product was diVi-PDMS.Part 2: Synthesis and characterization of diVi-PDMS modified polyacrylate miniemulsion In this part, the diVi-PDMS modifi
12、ed polyacrylate miniemulsion was prepared with diVi-PDMS and polyacrylate via miniemulsion polymerization. The ratio and iiidosage of traditional emulsifier(SDS:O-10)/polymeric emulsifier(V-20S), the molecular weight of organic silicon monomer on the polymerization stability and the properties of si
13、licone-modified polyacrylate emulsion, latex film and pigment printing were studied. The polymer structure and properties were characterized by FTIR, TGA and DSC. The results showed that when the mass ratio of polymerizable emulsifier was 1.5:1:1 and the amount of compound emulsifier was 6%, the pol
14、ymerization and latex had good stability, the latex had small particle size and narrow distribution. Compared to conventional emulsifier, complex polymeric emulsifier can significantly improve the mechanical properties of the film. With the increase of molecular weight of diVi-PDMS, the crosslinking
15、 degree of the film, the water resistance, the mechanical properties and the rubbing fastness of pigment printing fabric became worse. It was found that the molecular weight of diVi-PDMS was about 1600, the water contact angle of the film was 94.9 , the water absorption was 7.39%, the dry and wet ru
16、bbing fastness of pigment printing fabric reached 4 grade, and the printed fabrics handle became softer. The results of FTIR analysis indicated that the product was silicone-modified polyacrylate miniemulsion, DSC and TG analysis displayed that the glass transition temperatures of silicone-modified polymer was reduced, thermal decomposition temperature and heat-resistant stability was increased. The results of project showed that the diVi-PDMS modified polyacrylate adhesiv
