三烯丙基异氰尿酸酯的合成与表征

以异氰尿酸和氯丙烯为原料,N,N-二甲基甲酰胺(DMF)为溶剂,季铵盐为催化剂,合成三烯丙基异氰尿酸酯(TAIC),并考察了合成工艺参数对收率的影响,采用高效液相色谱(HPLC)、红外光谱(FTIR)、核磁共振碳谱(13CNMR)对目标产物进行表征。结果表明,在n(异氰尿酸)∶n(氯丙烯)=1∶4,氯丙烯滴加温度100℃,滴加时间2 h,反应温度120℃,反应时间1.5 h,四甲基氯化铵作催化剂的条件下,收率可达93.3%(以异氰尿酸计),纯度为97.9%(HPLC)。     

异氰尿酸三苄基酯的合成研究

采用Ｎ，Ｎ－二甲基甲酰胺作溶剂，异氰尿酸、苄氯为原料合成了异氰尿酸三苄基酯。通过正交实验得最佳反应条件为原料摩尔比异氰尿酸∶苄氯∶三乙胺＝１∶３．１∶３．２，反应温度１６０℃，反应时间４ｈ，溶剂ＤＭＦ６．５ｍｌ／ｇ异氰尿酸。该条件下产率达８５％以上     

高效液相色谱法测定三烯丙基异氰尿酸酯的含量

建立了高效液相色谱测定三烯丙基异氰尿酸酯含量的分析方法。通过实验确定了最佳色谱条件,色谱柱:Ultmate-C18柱(250 mm×4.6 mm,5μm);柱温:25℃;流动相:V(甲醇)∶V(0.1 mol/L磷酸-磷酸二氢钠缓冲溶液(pH为3.0))=60∶40;检测波长:210 nm;流速:1.0 mL/min。结果表明,三烯丙基异氰尿酸酯的浓度在1.0～200.0 mg/L范围内线性良好,相关系数为0.999 9,平均回收率为99.33%,相对标准偏差为1.81%,最低检出限为0.2 mg/L,最低定量限为1.2mg/L。本法简便、快速、准确,重复性好,可有效测定三烯丙基异氰尿酸酯的含量。     

一锅法合成异氰尿酸三苄基酯

对尿素为原料一锅法制备异氰尿酸三苄基酯的合成反应进行了研究。首先由尿素通过液相法合成异氰尿酸,不经分离继续与苄氯和三乙胺反应生成异氰尿酸三苄基酯,对反应条件及影响产率的各种因素进行了讨论。     

三(2-羟乙基)异氰尿酸酯的合成研究

研究了用环氧乙烷在常压下合成三(2-羟乙基)异氰尿酸酯的方法。探讨了原料配比、反应温度、溶剂、催化剂等对反应的影响,并对溶剂的回收利用做了研究。讨论了产品的后处理工艺。通过红外光谱和核磁共振谱分析表征了化合物的结构。     

三(环氧丙基)异氰尿酸丙烯酸酯的合成及应用

以三(环氧丙基)异氰尿酸酯作为树脂基体,经丙烯酸加成酯化,得到了三官能团环氧丙基异氰尿酸丙烯酸酯(TGICA)。研究了催化剂种类、原料配比、阻聚剂种类、酯化温度及反应时间对产物性能的影响。结果表明,合成TGICA的最优化条件为:n(TGIC)/n(AA)=1∶2 79;催化剂为N,N-二甲基苯胺;阻聚剂为2,6-二叔丁基对甲酚;反应温度(105±2)℃;反应时间3h。丙烯酸的转化率可达到99 7%。应用研究表明TGI CA是一种性能优异,价格低廉且合成方法简单的紫外光固化涂料成膜树脂。     

SYNTHESIS OF POLY(METHYL METHACRYLATE)—CLAY NANOCOMPOSITES

Poly(methyl methacrylate)/clay nanocomposites were synthesized via in situ free radical polymerization of methyl methacrylate (MMA) in the presence of functionalized clay. Montmoril-lonite (MMT), a smectic type of clay, was treated with a commercial cationic surfactant, benzalkonium chloride (BAC), and a synthesized zwitterionic surfactant, octadecyldimethyl betaine (CI8DMB) Functionalized MMT was prepared via an ion exchange between Na,ions in the clay and the surfactant cations in aqueous medium. The intercalation of the surfactant in the clay galleries was determined using X-ray diffraction (XRD). The interlayer spacing for C18DMB was 2.03nm, higher than 1.86nm observed for BAC. This is due to longer chain length of C18DMB. Both organophilic clays formed a viscous gel when dispersed in the monomer, MMA. Poly(methyl methacrylate) (PMMA) nanocomposites were obtained by polymerizing the dispersions. XRD and transmission electron microscopy (TEM) indicate predominant exfoliation of the silicate layers in the polymer matrix for MMT treated with C18DMB, and partial exfoliation for MMT treated with BAC     

SWELLING PROPERTIES OF POLY(N-VINYLIMIDAZOLE) HYDROGELS

The swelling capacity of poly(N-vinylimidazole) hydrogels in aqueous solutions and organic solvents was measured as a function of polymer network structure. In pure water, the swelling capacity decreases monotonously upon increasing the crosslinker ratio and the total comonomers concentration in the polymerization feed mixture. In methanol a similar behaviour was observed while in ethanol, the swelling capacity shows an abrupt change from large values to 0.01 grams of water per gram of dry gel, that is to say, PVI experience swollen-collapsed transitions with small changes of the gel crosslinking degree. Molecular weight of chains between crosslinks, determined from swelling measurements in methanol, scales with the product of the crosslinker and total comonomers concentrations in the feed mixture to m1.14-0.05. The dependence of the polymer solvent interaction parameter on the polymer concentration inside the swollen gel was also determined for water and ethanol.     

杂环取代联苯聚醚酮的流变行为

用日本岛津ＡＧ－２０００Ａ毛细管流变仪，研究了自制的杂环取代联苯型聚醚酮的流变行为。求出了表观流动活化能，考察了巴氏效庆和非牛顿行为，对其加工行为进行了分析。     

改性蒙脱土对PET吹塑瓶阻隔性的影响

在水分散液中使蒙脱土与6－氨基已酸或对氨基苯甲酸进行插层反应制得有机改性蒙脱土。X射线衍射、热重分析和红外光谱测试结果表明，6－氨基已酸或对氨基本甲酸被插层到蒙脱土的晶格片层之间，使层间距增大在双螺杆挤出机中使聚对苯二甲酸乙二酯（PET）与改性蒙脱土进行熔融插层复合得到PET／改性蒙脱土复合材料，并用注－拉－吹工艺成型得到PET／改性蒙脱土复合瓶。阻隔性测试结果显示，PET／改性蒙脱土复合瓶对氧气的阻隔性比纯有明显提高。     

聚脲甲醛包覆双环戊二烯微胶囊的热稳定性研究

采用原位聚合法,以聚脲甲醛为壁材、以双环戊二烯(DCPD)为囊芯合成聚脲甲醛包覆DCPD微胶囊。采用傅立叶变换红外光谱对其化学结构进行表征,利用热失重分析法和差示扫描量热法表征微胶囊的热稳定性。研究结果表明,聚脲甲醛包覆DCPD微胶囊在温度低于50℃时具有很好的热稳定性并能保持微胶囊的完整性,适合于制备低温或室温成型自修复复合材料。     

聚乙烯醇硫酸钾（PVSK）的制备及其结构分析

研制了胶体滴定法所需的标准阴离子型聚电解质试剂ＰＶＳＫ，探讨了合成条件的影响，并对ＰＶＳＫ的结构进行了分析。为阳离子聚电解质测试中应用胶体滴定法提供了物质条件。     

聚乳酸立构嵌段共聚物的合成与表征

以左旋和右旋丙交酯为原料,通过开环聚合制备了含有左旋和右旋乳酸链段的聚乳酸立构嵌段共聚物.采用红外光谱对其分子结构进行表征,表明共聚物已成功合成;并采用差示扫描量热仪和X射线衍射仪对共聚物的熔点和晶型进行研究,表明所得嵌段共聚物具有立构复合结构;采用乌氏粘度计对共聚物的分子量进行研究,表明共聚物的粘均分子量为25600...     

PHASE SEPARATION OF POLY(AMIC ACID-CO-IMIDE) SOLUTION

Poly(amic acid-co-imide) (PA-I) is an intermediate for preparation of polyimide from polyamic acid (PAA). Phase separation does not appear for the solution until a certain imidization degree. The experimental results of a rotation viscometer and FT-IR analysis showed that the critical point of phase separation (CPPS) was related to the imidization methods (thermal or chemical imidization) and the backbone structures (flexible ODPA-ODA or semi-rigid PMDA-ODA). Phase separation time is shorted with the increase of the initial PAA concentration, acetic anhydride amount, or temperature. When phase separation occurs, the solution viscosity increases, while the imidization degree is almost constant as the initial PAA concentration rises. The greater the chain mobility, the higher the imidization degree at phase separation point. At CPPS, higher imidization degree and lower solution viscosity are obtained in the thermal imidization than in the chemical imidization; ODPA-ODA system exhibits higher imidization degree and better solubility than that of PMDA-ODA system.     

对苯二甲酸直接酯化法合成PBT树脂的研究

讨论了酯化温度、催化剂种类和催化剂用量对酯化速度、酯化率、四氢呋喃生成量以及缩聚反应速度和树脂质量的影响。研究表明，钛锡复合催化剂能有效地提高酯化反应和缩聚反应速度，减少四氢呋喃生成量。采用钛锡复合催化剂，可使四氢呋喃生成量降到４６．２ｇ／ｋｇ树脂所得树脂特性粘数０．８９～１．０９ｄＬ／ｇ，羧基含量１２．３～１６．８μｅｑ／ｇ，熔点２２８～２３０℃。