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巴豆酸—醋酸乙烯酯共聚物合成及表征
The Synthesis and Characterization of Crotonic Acid-Vinyl Acetate Copolymer
【作者】 王海霞;
【导师】 苏涛;
【作者基本信息】 广西大学 , 应用化学, 2006, 硕士
【摘要】 本文采用几种不同聚合方法合成了巴豆酸—醋酸乙烯酯共聚物。 首先用乳液聚合法以辛烷基酚聚氧乙烯醚(OP—10)和羟乙基纤维素为乳化剂,过硫酸钾为引发剂合成巴豆酸-醋酸乙烯酯共聚物,通过改变单体配比,引发剂用量及引发剂加料方式研究了该共聚物乳液的性质,其乳液呈白色,pH值介于6—7之间,固含量在30%—40%之间,粘度0.02—4.3 Pa·s。 其次以马铃薯淀粉和羟乙基纤维素为分散剂,过氧化苯甲酰为引发剂,采用悬浮聚合和以丙酮为溶剂,过氧化苯甲酰为引发剂通过溶液聚合合成了巴豆酸-醋酸乙烯酯共聚物。由悬浮聚合制得的悬浮颗粒粒径在0.05—3.5mm之间,无色透明状,硬度较硬,可溶于乙醇、异丙醇、冰醋酸、乙酸乙酯、苯、氨水、碳酸钠、水溶液中。由溶液聚合所得的溶液为无色,pH值介于6—7之间,呈弱酸性,粘度小于5Pa·s.固含量可达75%。 悬浮聚合的产物经提纯后测定的IR和NMR谱支持其为巴豆酸—醋酸乙烯酯共聚物。凝胶渗透色谱(GPC)测定其数均分子量M_n为4.16*10.4,重均分子量M_w为1.19*10~5,多分散性M_w/M_n为2.85,差示扫描量热法(DSC)得知其玻璃化温度(T_g)为5℃,由热失重分析(TGA)得知它的分解温度为300℃。 所有的实验得到共聚物中巴豆酸结构单元含量为0.8-9.8 mol%,醋酸乙烯酯结构单元含量90.2-99.2 mol%,巴豆酸转化率33—87%,醋酸乙烯酯转化率45—72%,共聚物酸值5—70 mg KOH/g。
【Abstract】 The synthesis of crotonic acid - vinyl acetate copolymer is given by different polymerization techniques in this paper.Firstly, crotonic acid - vinyl acetate copolymer was synthesized by emulsion polymerization in which OP-10 and hydroxyethyl cellulose (HEC) was used as an emulsifier, and potassium persulfate as initiator. Properties of the copolymer emulsion were studied by changing monomer ratio, initiator doses, different ways of initiator, and the emulsion was white-colored, the pH value was between 6-7, and the obtained solid content was between 30%—40%, and its viscosity 0.02—4.3 Pa · s.Secondly, crotonic acid - vinyl acetate copolymer was synthesized by suspension polymerization. Potato starch and HEC were used as suspending agent and BPO as initiator. The copolymer was also synthesized by solution polymerization in which acetone was the solvent and BPO was the initiator. The granules of the suspension polymerization was between 0.05-3.5mm, was transparent, colorless, and hard. It can be dissolved in ethanol, isopropanol, acetone, glacial acetic acid、 ethyl acetate、 benzene 、 ammonia spirit, sodium carbonate, water solution. The obtained solution by solution polymerization is was transparent, colorless. Its pH value was 6-7, exhibited a weak acidity, and its viscosity was below 5Pa · s. The solid content obtained by solution polymerization reached up to 75%.The product obtained by suspension polymerization was identified to be crotonic acid - vinyl acetate copolymer by IR and NMR spectra. The number
【Key words】 crotonic acid; vinyl acetate; copolymerization; emulsion polymerization; suspension polymerization; solution polymerization;
- 【网络出版投稿人】 广西大学 【网络出版年期】2006年 12期
- 【分类号】TQ316.334
- 【被引频次】3
- 【下载频次】310