Ammonium thiocyanate was prepared in 2 steps from aqueous ammonia and carbon disulfied by phase transfer catalysis in yield of 72 7%, when catalysts consisted of OP 4 and OP 21 in mole ratio of 4∶6. The effects of re...Ammonium thiocyanate was prepared in 2 steps from aqueous ammonia and carbon disulfied by phase transfer catalysis in yield of 72 7%, when catalysts consisted of OP 4 and OP 21 in mole ratio of 4∶6. The effects of reaction temperature, time, mole ratio of OP 4 to OP 21 and conparison with other catalysts on the reaction were descurved.展开更多
Copper-tetra-4-(butyloxycarbonyl) phthalocyanine, copper-tetra-4-(octyloxycarbonyl) phthalocyanine and copper-tetra-4-(dodecoxycarboxyl) phthalocyanine were synthesized by the phase transfer catalysis reaction. The re...Copper-tetra-4-(butyloxycarbonyl) phthalocyanine, copper-tetra-4-(octyloxycarbonyl) phthalocyanine and copper-tetra-4-(dodecoxycarboxyl) phthalocyanine were synthesized by the phase transfer catalysis reaction. The reaction has several advantages in comparison with the previous carboxyl-esterified method, such as the milder conditions, the shorter reaction time(3—6 h), the higher yield(>95%), and so on. Because of the difference in the substituent group length of these compounds, the morphology and the congregation of the molecules in their casting films is different, leading to the different photoconductivities of them.展开更多
本文以NaH_(2)PO_(2)·H_(2)O和L-抗坏血酸为还原剂,以不同脱乙酰度壳聚糖(CHS)为稳定剂,制备氧化石墨烯(GO)负载纳米铜(CuNPs)复合物(GO-CuNPs-CHS)。利用紫外-可见光谱(UV-vis)研究了壳聚糖脱乙酰度对GO-CuNPs-CHS中CuNPs尺寸形...本文以NaH_(2)PO_(2)·H_(2)O和L-抗坏血酸为还原剂,以不同脱乙酰度壳聚糖(CHS)为稳定剂,制备氧化石墨烯(GO)负载纳米铜(CuNPs)复合物(GO-CuNPs-CHS)。利用紫外-可见光谱(UV-vis)研究了壳聚糖脱乙酰度对GO-CuNPs-CHS中CuNPs尺寸形貌的影响。利用傅里叶变换红外光谱(FT-IR)、透射电子显微镜(TEM)和X射线衍射(XRD)对GO-CuNPs-CHS进行了表征,探究了其对4-硝基苯酚(4-NP)的氢转移催化性能。结果表明,使用低脱乙酰度壳聚糖为稳定剂有利于制备小粒径、近球形的CuNPs。以脱乙酰度为52.3%的壳聚糖为稳定剂制备的GO-CuNPs-N3中CuNPs的平均粒径为(9.0±1.3)nm。GO-CuNPs-CHS的氢转移催化性能随着壳聚糖脱乙酰度的降低而逐渐增强,以GO-CuNPs-N3为催化剂时仅需8 min 4-NP转化率可达到98.4%,反应速率常数可达0.6868 min^(-1),反应活化能Ea为40.5 kJ·mol^(-1)。展开更多
系统地研究了无溶剂条件下,H2O2为氧源,反应控制相转移催化剂[(C16H33(70%)+C18H37(30%))N(CH3)3]3[PW4O16]催化氯丙烯环氧化制环氧氯丙烷反应.结果表明,在氯丙烯/H2O2/催化剂(摩尔比)=400∶100∶1条件下,50～55℃反应3 h,环氧氯丙烷的...系统地研究了无溶剂条件下,H2O2为氧源,反应控制相转移催化剂[(C16H33(70%)+C18H37(30%))N(CH3)3]3[PW4O16]催化氯丙烯环氧化制环氧氯丙烷反应.结果表明,在氯丙烯/H2O2/催化剂(摩尔比)=400∶100∶1条件下,50～55℃反应3 h,环氧氯丙烷的收率为85～87%.在NaH2PO4存在下,催化剂循环使用5次,活性无明显降低,新鲜催化剂和回收催化剂的31P MAS NMR谱分析结果表明NaH2PO4对催化剂结构和组成具有稳定作用.展开更多
以3-溴丙炔、异氰尿酸为原料,利用相转移催化剂合成了三炔丙基异氰尿酸酯(TPIC),并用FT-IR、1 H NMR对其结构进行了表征。用TGA表征了热固化后的TPIC的热性能。结果表明:热固化后的树脂在375℃开始分解,800℃的残炭率达75%。根据DSC曲线...以3-溴丙炔、异氰尿酸为原料,利用相转移催化剂合成了三炔丙基异氰尿酸酯(TPIC),并用FT-IR、1 H NMR对其结构进行了表征。用TGA表征了热固化后的TPIC的热性能。结果表明:热固化后的树脂在375℃开始分解,800℃的残炭率达75%。根据DSC曲线,TPIC的熔点为167℃左右,并用Kissinger、Flynn-Wall-Ozawa和Friedman-Reich-Levi法分别计算了热固化反应活化能,它们分别为46.81、48.70和40.92kJ.mol-1,热固化反应级数都接近1,并探讨了固化反应过程与机理。通过对比分析表明,这3种方法均适用于TPIC体系。展开更多
乌拉地尔是一种新型的多靶点降压药物,现对其已有的合成方法进行改进。讨论了相转移催化条件和逆向相转移催化条件下,以6-（3-氯丙基）氨基-1,3-二甲基尿嘧啶和1-（2-甲氧基苯基）哌嗪盐酸盐为原料,进行乌拉地尔合成的反应结果。逆向相...乌拉地尔是一种新型的多靶点降压药物,现对其已有的合成方法进行改进。讨论了相转移催化条件和逆向相转移催化条件下,以6-（3-氯丙基）氨基-1,3-二甲基尿嘧啶和1-（2-甲氧基苯基）哌嗪盐酸盐为原料,进行乌拉地尔合成的反应结果。逆向相转移催化条件下所获收率高于相转移催化条件。当选择β-CD为逆向相转移催化剂,水为溶剂,反应温度为95℃,在1500 r min 1转速下经2~3 h反应,可以大于80%的收率获得含量为96.6%~98.0%乌拉地尔粗品。乌拉地尔粗品精制采用反溶剂重结晶法,其适宜条件是7℃时,二氯甲烷为溶剂,丙酮为反溶剂,所获得乌拉地尔成品含量〉98.5%,收率〉95%。乌拉地尔结构经1H-NMR、MS、IR和元素分析确证。与已有工艺比较,改进的合成方法具有显著缩短反应时间,产物分离简单易行,合成工艺简单、易于工业化生产等优点。展开更多
文摘Ammonium thiocyanate was prepared in 2 steps from aqueous ammonia and carbon disulfied by phase transfer catalysis in yield of 72 7%, when catalysts consisted of OP 4 and OP 21 in mole ratio of 4∶6. The effects of reaction temperature, time, mole ratio of OP 4 to OP 21 and conparison with other catalysts on the reaction were descurved.
文摘Copper-tetra-4-(butyloxycarbonyl) phthalocyanine, copper-tetra-4-(octyloxycarbonyl) phthalocyanine and copper-tetra-4-(dodecoxycarboxyl) phthalocyanine were synthesized by the phase transfer catalysis reaction. The reaction has several advantages in comparison with the previous carboxyl-esterified method, such as the milder conditions, the shorter reaction time(3—6 h), the higher yield(>95%), and so on. Because of the difference in the substituent group length of these compounds, the morphology and the congregation of the molecules in their casting films is different, leading to the different photoconductivities of them.
文摘本文以NaH_(2)PO_(2)·H_(2)O和L-抗坏血酸为还原剂,以不同脱乙酰度壳聚糖(CHS)为稳定剂,制备氧化石墨烯(GO)负载纳米铜(CuNPs)复合物(GO-CuNPs-CHS)。利用紫外-可见光谱(UV-vis)研究了壳聚糖脱乙酰度对GO-CuNPs-CHS中CuNPs尺寸形貌的影响。利用傅里叶变换红外光谱(FT-IR)、透射电子显微镜(TEM)和X射线衍射(XRD)对GO-CuNPs-CHS进行了表征,探究了其对4-硝基苯酚(4-NP)的氢转移催化性能。结果表明,使用低脱乙酰度壳聚糖为稳定剂有利于制备小粒径、近球形的CuNPs。以脱乙酰度为52.3%的壳聚糖为稳定剂制备的GO-CuNPs-N3中CuNPs的平均粒径为(9.0±1.3)nm。GO-CuNPs-CHS的氢转移催化性能随着壳聚糖脱乙酰度的降低而逐渐增强,以GO-CuNPs-N3为催化剂时仅需8 min 4-NP转化率可达到98.4%,反应速率常数可达0.6868 min^(-1),反应活化能Ea为40.5 kJ·mol^(-1)。
文摘系统地研究了无溶剂条件下,H2O2为氧源,反应控制相转移催化剂[(C16H33(70%)+C18H37(30%))N(CH3)3]3[PW4O16]催化氯丙烯环氧化制环氧氯丙烷反应.结果表明,在氯丙烯/H2O2/催化剂(摩尔比)=400∶100∶1条件下,50～55℃反应3 h,环氧氯丙烷的收率为85～87%.在NaH2PO4存在下,催化剂循环使用5次,活性无明显降低,新鲜催化剂和回收催化剂的31P MAS NMR谱分析结果表明NaH2PO4对催化剂结构和组成具有稳定作用.
文摘以3-溴丙炔、异氰尿酸为原料,利用相转移催化剂合成了三炔丙基异氰尿酸酯(TPIC),并用FT-IR、1 H NMR对其结构进行了表征。用TGA表征了热固化后的TPIC的热性能。结果表明:热固化后的树脂在375℃开始分解,800℃的残炭率达75%。根据DSC曲线,TPIC的熔点为167℃左右,并用Kissinger、Flynn-Wall-Ozawa和Friedman-Reich-Levi法分别计算了热固化反应活化能,它们分别为46.81、48.70和40.92kJ.mol-1,热固化反应级数都接近1,并探讨了固化反应过程与机理。通过对比分析表明,这3种方法均适用于TPIC体系。
文摘乌拉地尔是一种新型的多靶点降压药物,现对其已有的合成方法进行改进。讨论了相转移催化条件和逆向相转移催化条件下,以6-（3-氯丙基）氨基-1,3-二甲基尿嘧啶和1-（2-甲氧基苯基）哌嗪盐酸盐为原料,进行乌拉地尔合成的反应结果。逆向相转移催化条件下所获收率高于相转移催化条件。当选择β-CD为逆向相转移催化剂,水为溶剂,反应温度为95℃,在1500 r min 1转速下经2~3 h反应,可以大于80%的收率获得含量为96.6%~98.0%乌拉地尔粗品。乌拉地尔粗品精制采用反溶剂重结晶法,其适宜条件是7℃时,二氯甲烷为溶剂,丙酮为反溶剂,所获得乌拉地尔成品含量〉98.5%,收率〉95%。乌拉地尔结构经1H-NMR、MS、IR和元素分析确证。与已有工艺比较,改进的合成方法具有显著缩短反应时间,产物分离简单易行,合成工艺简单、易于工业化生产等优点。
