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1、西安科技大学 硕士学位论文 固相剪切碾磨法制备PVC/高岭土纳米复合材料 姓名：陈建军 申请学位级别：硕士 专业：应用化学 指导教师：李侃社 论文题目：固相剪切碾磨法制备 PVC/高岭土纳米复合材料 专 业：应用化学 硕 士 生：陈建军 (签名) 指导老师：李侃社 (签名) 摘 要 聚氯乙烯(PVC)是世界上最早实现工业化生产的塑料品种之一， 但 PVC 属于一种脆 性材料，这种韧性差的缺陷大大地限制了 PVC 的进一步发展及广泛应用。因此，需要 对 PVC 进行增强、增韧改性研究，以期得到高性能的 PVC 材料。 利用磨盘形力化学反应器在室温和固相条件下制备 PVC 微粉。经碾磨处理后可使
2、PVC 固有的多层次结构和微晶结构破坏， 粒度和分子量下降。 经过 40 次碾磨处理， PVC 粒径 d(0.1)由 84.29 m 变为 12.46 m；塑化时间从 294s 降至 90s，塑化速率和熔融效率 均有所提高，平衡扭矩从 42.7Nm 降至 38.4Nm，加工性能得到明显改善；经过 30 次碾 磨处理后断裂伸长率由 57.00%提高到 202.1%；经过 15 次碾磨处理后拉伸强度由 49.50MPa提高到53.25MPa； 经过10次碾磨处理后缺口冲击强度由3.91 kJ/m2提高到4.30 kJ/m2。 利用磨盘形力化学反应器在室温和固相条件下制备了 PVC/高岭土纳米复合粉
3、体 (FT-3)和 PVC/膨胀高岭土纳米复合粉体(FT-4)。XRD 和 SEM 分析表明：固相剪切碾磨 产生的强大剪切、挤压、摩擦等作用引起 PVC 相和高岭土相的多种复杂的物理及化学 变化，表现为高岭土粒径变小，粒子比表面积增加，PVC/高岭土界面相互作用增强。 讨论了碾磨次数、高岭土含量、稀土稳定剂和增塑剂用量对 PVC/高岭土纳米复合 材料的力学性能影响。结果表明：碾磨次数为 30 次、高岭土含量为 8%、稀土稳定剂含 量为 3%、 微粉 PVC 含量为 30%时复合材料力学性能最佳。 与简单的填充复合方法相比， 固相剪切碾磨技术制备的 PVC/高岭土纳米复合材料的力学性能有较大的提
4、高实现了增 强增韧。 SEM 和 TEM 分析表明： 经碾磨后部分高岭土以直径小于 30nm 且厚径比为 10 倍左 右的纳米粒子均匀的分散在 PVC 基体中。热重分析可以看出复合材料的热稳定性要远 远优于纯 PVC 材料，纯 PVC 材料在 122时就开始失重，而复合材料在 156才开始 失重，且失重率比纯 PVC 的要低 7.12%。 关 键 词：固相剪切碾磨；自增塑；PVC；高岭土；纳米复合材料 研究类型：基础理论研究 Subject : Preparation of PVC/Kaolin Nanocomposites Through Solid State Shear Panmilli
5、ng Method Specialty : Applied Chemistry Name : Chen Jianjun (Signature) Instructor : Li Kanshe (Signature) ABSTRACT Polyvinyl-chloride(PVC) is one of the earliest industrialization production plastics in the world, but it is brittle, which defect has greatly restricted the development and the widesp
6、read application of the pvc in the further. Therefore, it is necessary to carry on the reinforcing and toughening modification research to obtain better performance pvc material. Firstly, the PVC powder was prepared through solid state panmilling method under the condition of solid phase at the room
7、 temperature. After the process of the milling, the multi-level structure and microcrystalline were destroyed; the particle size and molecular weight were decreased. After grinding through 40, the PVC particle size d(0.1) reduced from 84.29 m to 12.46 m; plasticizing time reduced from 294s to 90s; p
8、lasticizing and melting rates were increased; torque balance dropped from 42.7Nm to 38.4Nm; processing performance was significantly improved. The elongation of PVC/Kaolin nanocomposites was increased from 57.00% to 202.10% after grinding through 30. The tensile strength increased from 49.50Mpa to 5
9、3.25Mpa after 15 milling treatment. The notched impact strength increased from 3.91kJ/m2 to 4.30 kJ/m2 after 10 milling treatment. Pvc/kaolin composite powder (FT-3) and PVC/expantion kaolin composite powder (FT-4) were prepared through solid state shear panmilling method. The structures were charac
10、terized by XRD and SEM. The results showed that solid-phase shear milling produces a strong shear, compressionm, friction and other effects , it was cause the physical and chemical changes betweenPVCand Kaolin, kaolin particle size change into samll, the surface area of particles was increased and t
11、he interaction between pvc and kaolin was increased. Packed with simple methods, solid phase shear milling Preparation of PVC/Kaolin nanocomposites have greatly improved mechanical properties to achieve the strengthening and toughening. The number of milling, content of kaolin, the rare earth stabil
12、izers and plasticizer content on PVC/Kaolin composite to the mechanical properties were discussed. The results showed that the composite has best mechanical properties when the number of milling is 30, kaolin is 8%, rare earth stabilizer is 3% and the pvc powder is 30%. The results of the SEM and TE
13、M showed that kaolin with a diameter less than 30nm and the aspect ratio of 10 times the nano-particles uniformly dispersed in pvc matrix after the milling. Thermogravimetric analysis showed that the thermal stability of composites is much better than pure PVC material, the pure PVC began to loss we
14、igth at the 122, but the composite began to loss weigth at he 156, and the weigth of loss is lower than that of pure PVC about 7.12%. Keywords: PVC Kaolin Solid State Shear Milling Self-plasticizer Nanocomposites Thesis : Basic Theory Research 1 绪论 1 1 绪论 聚氯乙烯(Polyvinyl Chloride，简称 PVC)是氯乙烯的均聚物，它是由氯
15、乙烯单体在 过氧化物、偶氮二异丁腈等引发剂作用下，在光、热的条件下发生聚合反应而生成的热 塑性高聚物，其数均分子量约为 512 万。PVC 为无定形聚合物，含结晶度 5%10%的 微晶体，熔点为 175。 聚氯乙烯(PVC)是世界上最早实现工业化的塑料品种之一。 自 20 世纪 30 年代以来， PVC 以其优良的综合性能和较低的价格而备受各工业化国家的重视， 保持着长盛不衰的 发展势头。由于其具有难燃、抗化学腐蚀、耐磨、电绝缘性优良和机械强度较高等优点， 广泛地应用于工业、农业、建筑、日用品、包装以及电力等方面。但 PVC 属于一种脆 性材料，这种缺陷大大地限制了 PVC 的进一步发展及广泛
16、应用。随着人们生活水平的 提高，品种更多的零部件及制品需由塑料树脂来制作，对其性能也提出了更高的要求。 要开发新品种的塑料树脂，塑料合金及共混填充改性塑料已成为目前最切实的要求，也 是当前国内外高分子材料加工领域中重要的研究与开发内容。因此，对 PVC 进行增韧、 增强改性研究，从而得到高强、高韧的 PVC 材料，一直是众多研究者和商家追求的目 标。 1.1PVC 的生产现状 我国 PVC 树脂的消费主要分为 2 大类，一是软制品，约占总消费量的 37%，主要 包括电线电缆、各种用途的膜、铺地材料、织物涂层、人造革、各类软管、手套、玩具、 塑料鞋以及一些专用涂料和密封部件等。二是硬制品，约占总消费量的 63%，主要包括 各种型材、管材、板材、硬片和瓶等。 随着国民经济持续高速发展， 以及建筑业和 PVC 加工工业对 PVC 消费的强烈需求， 国内 PVC 工业发展十分迅速。特别是近几年来
