论文总字数：17472字

摘 要

羧基功能化聚甲基丙烯酸甲酯微球是指以聚甲基丙烯酸甲酯（ PMMA）为原料制备的高分子微球，经过优化反应条件、改良实验方法进行表面改性，得到具有一定羧基含量的聚合物微球。以 PMMA为材料，结合微球表面羧酸酯基皂化水解，制备出了单分散性好，表面羧基含量高、粒径可控且粒径大小均一且合适的微米级羧基功能化聚甲基丙烯酸甲酯微球。将其作为填料填充色谱柱，装配在美国伯乐公司的全自动血红蛋白分析仪上，用于糖化血红蛋白指标检测，具有临床应用价值^[1]。

本文利用电导率的变化测定微球表面的羧基含量，研究皂化时间、皂化反应过程中碱浓度、皂化反应温度以及乙醇或水的反应相对微球表面羧基含量的影响，得到最经济最有效环境最友好的制备方法制备羧基功能化聚甲基丙烯酸甲酯。 结果表明： 1 mol/ L NaOH、80℃、40 h、乙醇相的反应条件下， PMMA微球的羧基含量可达0.096 mmol/ g。 经红外光谱以及返电导滴定分析，在3445.17 cm-1处有明显变化，该峰说明了产物中有羟基， 且含量高。 所以本课题设置的皂化条件制备羧基功能化聚甲基丙烯酸甲酯微球可用于糖化血红蛋白的检测。

关键词：羧基功能化 聚甲基丙烯酸甲酯 高分子微球 皂化 糖化血红蛋白

Preparation and Characterization of Carboxyl-functionalized Poly(methyl methacrylate) Microspheres

Abstract

The carboxyl functionalized poly(methyl methacrylate) microspheres contains a certain amount of carboxyl groups, which are polymeric microspheres prepared from poly(methyl methacrylate) (PMMA). PMMA was treated in optimized reaction conditions and modified microspheres surface. The carboxylic ester groups on the surface of PMMA microspheres were saponified and hydrolysed. The carboxyl functionalized PMMA microspheres were prepared with a good monodispersity, high surface carboxyl group content, controllable and uniform particle size. The chromatographic column filled with the carboxyl functionalized PMMA microspheres and was assembled on the Automatic Hemoglobin Analyzer of Bio-Rad company(USA) applied in the Glycated hemoglobin (HbA1c) assay. It was valuable for clinical application.

In this paper, the change of conductivity was used to determine the content of carboxyl groups on the surface of microspheres. We studied the influences on the carboxyl content of saponification time, alkali concentration during saponification reaction, saponification reaction temperature, and the reaction of ethanol or water. An effective and friendly-environment method was obtained on preparing the carboxyl functional PMMA microspheres. The results showed that the carboxyl group content of PMMA microspheres was high to 0.096 mmol/g under the reaction conditions of 1 mol/L NaOH, 80°C, 40 h and ethanol phase. According to a significant change at 3445.17 cm^-1 on the Infrared Spectroscopy and the result of Conductance Titration Assay, it was indicated that the hydroxyl groups content of the product was very high. Therefore, it was feasible to prepare carboxyl functionalized PMMA microspheres by saponification treatments, which could apply in the detection of glycosylated hemoglobin.

Key Words: Functionalization of carboxyl groups; Polymethylmethacrylate; Polymer microspheres; Saponification; Glycated hemoglobin

目 录

摘 要 I

Abstract II

第一章 文献综述 1

1.1高分子微球 1

1.1.1 高分子微球概述： 1

1.1.2 高分子微球的功能基化： 1

1.2聚甲基丙烯酸甲酯 1

1.2.1 聚甲基丙烯酸甲酯概述: 1

1.2.2 聚甲基丙烯酸甲酯的皂化: 1

1.2.3 羧基功能化聚甲基丙烯酸甲酯作分析柱填料测血糖原理： 2

1.3聚甲基丙烯酸甲酯微球的羧基功能化 2

1.4本课题的研究内容和意义 2

第二章 材料与方法 3

2.1实验材料与设备 3

2.1.1 实验材料与试剂 3

2.1.2 实验设备与仪器 3

2.2试验方法 4

2.2.1 PMMA微球的皂化反应 4

2.2.2 微球羧基含量的测定 4

2.3测试与表征 4

2.4羧基含量计算依据 5

第三章 结果与讨论 7

3.1聚甲基丙烯酸甲酯微球皂化反应条件的研究 8

3.1.1NaOH浓度对微球皂化反应的影响 8

3.1.2皂化时间对微球皂化反应的影响 8

3.1.3皂化温度对微球皂化反应的影响 9

3.2水相皂化反应结果分析: 9

3.3醇作为反应相对微球皂化反应的影响 12

3.4皂化后微球表征分析 15

第四章 结论与展望 20

4.1结论 20

4.2展望 20

参考文献 21

致谢 23

第一章 文献综述

1.1高分子微球

1.1.1 高分子微球概述：

高分子微球多指球型或者其他几何体的微球，直径范围在微米级至纳米级的高分子材料或复合材料。纳米微球一般是高分子聚合而成，多是树脂， 乳液聚合，聚苯乙烯，聚丙烯酸等。不同形状和直径的微球有着不同的作用效果。“结构决定功能”，高分子微球性能于结构的可人为设计的特性使得其作为功能材料有着巨大的应用前景，例如在医药工程、建筑涂料、化学化工等领域都有重要作用和广泛应用^[2]。

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