以2,2-二羟甲基丁酸钠、1,3-丙烷磺内酯为原料,采用磺烷基化反应合成了新型的磺酸盐亲水单体2,2-二羟甲基丁酸-3＇-磺酸钠-丙酯（DMBPS-Na）。采用FT-IR、1H-NMR、13C-NMR、EIS-MS和元素分析等对DMBPS-Na进行了表征。DMBPS-Na的熔点为85...以2,2-二羟甲基丁酸钠、1,3-丙烷磺内酯为原料,采用磺烷基化反应合成了新型的磺酸盐亲水单体2,2-二羟甲基丁酸-3＇-磺酸钠-丙酯（DMBPS-Na）。采用FT-IR、1H-NMR、13C-NMR、EIS-MS和元素分析等对DMBPS-Na进行了表征。DMBPS-Na的熔点为85-90℃,易溶于水、乙醇、N,N-二甲基乙酰胺,微溶于丙酮、乙酸乙酯。以DMBPS-Na为亲水单体,聚四氢呋喃二醇、异佛尔酮二异氰酸酯和乙二胺为原料,采用丙酮法合成了固含量达50%以上的磺酸型聚氨酯分散体（PUD）。性能测试结果显示,DMBPS-Na用量为8 mmol？（100 g）？1树脂时,PUD的平均粒径为122.3 nm,黏度为475 m Pa·s,ζ电位为？66.39 m V,具有良好的稳定性;透射电镜（TEM）显示PUD胶粒呈二元分布的球状结构;PUD胶膜的拉伸强度为10.66 MPa,断裂伸长率为1160%;PUD胶膜的起始分解温度约为270℃,至490℃时基本分解完全。展开更多
研究了在对甲基苯磺酸的催化作用下,2,2-二羟甲基丙酸与苯乙酮的缩合反应,从催化剂用量,带水剂用量,物料比以及反应时间四个方面对反应条件进行了优化,实验结果表明:对甲基苯磺酸对2,2-二羟甲基丙酸缩环己酮的缩酮化反应具有较好的催化...研究了在对甲基苯磺酸的催化作用下,2,2-二羟甲基丙酸与苯乙酮的缩合反应,从催化剂用量,带水剂用量,物料比以及反应时间四个方面对反应条件进行了优化,实验结果表明:对甲基苯磺酸对2,2-二羟甲基丙酸缩环己酮的缩酮化反应具有较好的催化作用,其最佳反应为:催化剂用量为3%,n(DMPA):n(苯乙酮)=1:1.2,反应时间为7 h,反应温度105℃,带水剂(环已烷)的用量为10 m L,产率为85.18%。展开更多
A new 3D supramolecular complex,namely dimethylammonium 4,4΄-([2,2΄-bipyrimidine]-5,5΄-diyl)bis(2-hydroxybenzoate)dihydrate,has been synthesized by the reaction of 4,4΄-([2,2΄-bipyrimidine]-5,5΄-diyl)bis(2-hydroxybenz...A new 3D supramolecular complex,namely dimethylammonium 4,4΄-([2,2΄-bipyrimidine]-5,5΄-diyl)bis(2-hydroxybenzoate)dihydrate,has been synthesized by the reaction of 4,4΄-([2,2΄-bipyrimidine]-5,5΄-diyl)bis(2-hydroxybenzoic acid)with aqueous dimethylamine solution and characterized by single-crystal X-ray diffraction,^(1)H NMR spectroscopy and elemental analysis.It belongs to triclinic system,space groupP with a=6.5539(4),b=9.4977(6),c=12.1407(8)Å,α=72.299(6),β=89.160(5),γ=70.797(8)°,V=676.52(8)Å^(3),Z=1,Mr=556.57,µ=0.103 mm^(-1),Dc=1.366 g/cm^(3),F(000)=294,the final R=0.0828 and wR=0.2083 for 1934 observed reflections with I>2σ(I).The 4,4΄-([2,2΄-bipyrimidine]-5,5΄-diyl)bis(2-hydroxybenzoic acid)dianion,dimethylammonium cation,and water molecule are interconnected by O−H∙∙∙O,N−H∙∙∙N,and N−H∙∙∙O hydrogen bonds,forming a two-dimensional(2D)layer.Two adjacent 2D layers are further stacked into a three-dimensional supramolecular structure through O−H∙∙∙O hydrogen bonds.In addition,the luminescent property of this supramolecular complex has also been investigated.展开更多
Synthesis of ketals and acetals from 2,2bis(hydroxymethyl)propane1,3diol with aldehydes and ketones was catalysed by phosphotungstic acid supported on active carbon(HPW/C),and the factors influencing the yield w...Synthesis of ketals and acetals from 2,2bis(hydroxymethyl)propane1,3diol with aldehydes and ketones was catalysed by phosphotungstic acid supported on active carbon(HPW/C),and the factors influencing the yield were investigated.It is show that HPW/C was an excellent catalyst,and it was stabtilitive and reusable.The products were characterized by 1H NMR,IR and elemental analysis.展开更多
文摘以2,2-二羟甲基丁酸钠、1,3-丙烷磺内酯为原料,采用磺烷基化反应合成了新型的磺酸盐亲水单体2,2-二羟甲基丁酸-3＇-磺酸钠-丙酯（DMBPS-Na）。采用FT-IR、1H-NMR、13C-NMR、EIS-MS和元素分析等对DMBPS-Na进行了表征。DMBPS-Na的熔点为85-90℃,易溶于水、乙醇、N,N-二甲基乙酰胺,微溶于丙酮、乙酸乙酯。以DMBPS-Na为亲水单体,聚四氢呋喃二醇、异佛尔酮二异氰酸酯和乙二胺为原料,采用丙酮法合成了固含量达50%以上的磺酸型聚氨酯分散体（PUD）。性能测试结果显示,DMBPS-Na用量为8 mmol？（100 g）？1树脂时,PUD的平均粒径为122.3 nm,黏度为475 m Pa·s,ζ电位为？66.39 m V,具有良好的稳定性;透射电镜（TEM）显示PUD胶粒呈二元分布的球状结构;PUD胶膜的拉伸强度为10.66 MPa,断裂伸长率为1160%;PUD胶膜的起始分解温度约为270℃,至490℃时基本分解完全。
文摘研究了在对甲基苯磺酸的催化作用下,2,2-二羟甲基丙酸与苯乙酮的缩合反应,从催化剂用量,带水剂用量,物料比以及反应时间四个方面对反应条件进行了优化,实验结果表明:对甲基苯磺酸对2,2-二羟甲基丙酸缩环己酮的缩酮化反应具有较好的催化作用,其最佳反应为:催化剂用量为3%,n(DMPA):n(苯乙酮)=1:1.2,反应时间为7 h,反应温度105℃,带水剂(环已烷)的用量为10 m L,产率为85.18%。
基金the National Natural Science Foundation of China(21372112)。
文摘A new 3D supramolecular complex,namely dimethylammonium 4,4΄-([2,2΄-bipyrimidine]-5,5΄-diyl)bis(2-hydroxybenzoate)dihydrate,has been synthesized by the reaction of 4,4΄-([2,2΄-bipyrimidine]-5,5΄-diyl)bis(2-hydroxybenzoic acid)with aqueous dimethylamine solution and characterized by single-crystal X-ray diffraction,^(1)H NMR spectroscopy and elemental analysis.It belongs to triclinic system,space groupP with a=6.5539(4),b=9.4977(6),c=12.1407(8)Å,α=72.299(6),β=89.160(5),γ=70.797(8)°,V=676.52(8)Å^(3),Z=1,Mr=556.57,µ=0.103 mm^(-1),Dc=1.366 g/cm^(3),F(000)=294,the final R=0.0828 and wR=0.2083 for 1934 observed reflections with I>2σ(I).The 4,4΄-([2,2΄-bipyrimidine]-5,5΄-diyl)bis(2-hydroxybenzoic acid)dianion,dimethylammonium cation,and water molecule are interconnected by O−H∙∙∙O,N−H∙∙∙N,and N−H∙∙∙O hydrogen bonds,forming a two-dimensional(2D)layer.Two adjacent 2D layers are further stacked into a three-dimensional supramolecular structure through O−H∙∙∙O hydrogen bonds.In addition,the luminescent property of this supramolecular complex has also been investigated.
文摘Synthesis of ketals and acetals from 2,2bis(hydroxymethyl)propane1,3diol with aldehydes and ketones was catalysed by phosphotungstic acid supported on active carbon(HPW/C),and the factors influencing the yield were investigated.It is show that HPW/C was an excellent catalyst,and it was stabtilitive and reusable.The products were characterized by 1H NMR,IR and elemental analysis.
