期刊文献+

合成甘脲和四羟甲基甘脲工艺条件的研究 被引量:2

Process Conditions for Synthesis of Tetramethylol Glycoluril and Glycoluril
在线阅读 下载PDF
导出
摘要 甘脲和四羟甲基甘脲是粉末涂料、水性涂料的添加剂,也是多功能材料化合物瓜环的中间体。以乙二醛和尿素为原料,首先经过酸催化缩合合成甘脲,然后甘脲和甲醛通过碱催化缩合合成四羟甲基甘脲。考察了反应物摩尔比、pH值、反应时间和温度、滴加溶液的速率等因素对甘脲和四羟甲基甘脲收率的影响规律,并确定了合成甘脲和四羟甲基甘脲的最佳条件和工艺参数。采用红外色谱(FT-IR)表征了产品的化学结构;使用高效液相色谱和紫外色谱检测了产品的纯度和产率。其中甘脲产率75%,纯度95%;四羟甲基甘脲产率70%,纯度90%。研究结果表明,采用酸碱催化缩合反应条件,可以制备出产率和纯度都比较高的产物。 Glycoluril and tetramethylol glycoluril are not only the additives of powder coatings and hydrophilic coatings,but also the intermediates of cucurbit In] urils of multifunctional mate rial compounds. In this paper,glycoluril was synthesized by the acid catalyzed condensation reac tion using glyoxal and urea as raw materials,and then tetramethylol glycoluril was synthesized by the alkali catalyzed condensation reaction with formaldehyde. The influences of the molar ratio of reactant,pH value,reaction time and temperature,the rate of adding solution in drop on the yield of glycoluril and tetramethylol glycoluril were studied and the optimum processing conditions and parameters were identified. Some physical parameters of glycoluril and tetramethylol glycoluril were determined by IR,UV and HPLC. Results indicate that the yield of glycoluril reached 75% and purity was 95% ,and the yield of tetramethylol glycoluril reached 70% and purity was 90%. This method offers several advantages including low cost, simple experimental procedure and lit tle enviroment pollution.
出处 《太原理工大学学报》 CAS 北大核心 2012年第6期665-668,682,共5页 Journal of Taiyuan University of Technology
关键词 甘脲 四羟甲基甘脲 酸催化 乙二醛 碱催化 glycoluril tetramethylol glycoluril acid catalysis, glyoxal alkali catalysis
  • 相关文献

参考文献11

二级参考文献52

  • 1赵红振,齐暑华,周文英,李国新.紫外光固化涂料的研究进展[J].化学与粘合,2006,28(5):352-356. 被引量:19
  • 2王荣耕,李立,杨晓东.高固体分涂料现状及其发展趋势[J].现代涂料与涂装,2006,9(8):13-16. 被引量:7
  • 3高桥春.涂装技术特集,1997,(11):69-69.
  • 4Jianzhang Zhao, Hee - Joon Kim, Jinho Oh, Soo - young Kim, Jae Wook Lee, Shigeru Sakamoto, Kentaro Ya maguehi,and kimoon Kim. Cueurbit[n]uril Derivatives Soluble in Water and Organic Solvents Angew. Chem. Int. Ed.2001,40,No. 22,4233--4235.
  • 5Behrend R, Meyer E, Rusche F. Ueber Liebigs. Ann.Chem, 1905,339 : 1-37.
  • 6Freeeman W A, Mock W L, Shih N Y F. Cucurbituril. J.Am. Chem. Soc., 1981,103(24) ; P7367--7368.
  • 7Kim J,Jung I S, Kim S Y, lee E,et al. New Cucurbituril Homologues: Syntheses, Isolation, Characterization, and X - ray Crystal Structures of Cucurbit [n] uril ( n = 5,7, and8). J.Am, Chem. Soc . ,2000,122(3) :540--541.
  • 8Anthony Day, Alan P. Arnold,Rodney J. Blanch,and Barry Snushall Controlling Factors in the Synthesis of Cucurbituril and Its Homologues J. Org. Chem. 2001,66,8094 - 8100.
  • 9Anthony Filnn, Gordon C. Hough, J. Fraser Stoddart and David J. Williams Decamethylcucurbit [ 5 ] uril Angew.Chem. Int. Ed. Engl. 1992,31, No. 11,1475-- 1477.
  • 10Behrend R, Meyer E, Rusehe F, Ueber Liebigs [ J ]. Ann. Chem, 1905,339 : 1-37.

共引文献122

同被引文献22

引证文献2

二级引证文献8

相关作者

内容加载中请稍等...

相关机构

内容加载中请稍等...

相关主题

内容加载中请稍等...

浏览历史

内容加载中请稍等...
;
使用帮助 返回顶部