5-（Difluoromethoxy）-2-mercapto- 1H-benzimi- dazole （DMB） was precipitated by adding acetic acid to the DMB sodium salt solution. The spherical agglomeration of DMB during the reactive crystallization in a batch cr...5-（Difluoromethoxy）-2-mercapto- 1H-benzimi- dazole （DMB） was precipitated by adding acetic acid to the DMB sodium salt solution. The spherical agglomeration of DMB during the reactive crystallization in a batch crystallizer was monitored by real-time Particle Video Microscope （PVM）. We found that the low feeding rate of acetic acid, high crystallization temperature, low agitation rate or adding seed crystal can facilitate the formation of spherical agglomerates. By using a simple model, the mean crystal agglomerate size of DMB thus predicted is generally in agreement with the experimental data. In addition, the crystallization process of DMB was optimized by a new control strategy of supersaturation to avoid disadvantages brought by agglomeration.展开更多
The complex of[N,N,N ’ ,N ’- tetrakis(2 - benzimida zolyl methyl) - 1,4 - diethylene amino] - glycol ether(EGTB)with zinc (Ⅱ) ,[Zn 2 (EGTB)Cl 2 ](ClO 4 ) 2 · CH 3 OH · 3H 2 O was synthesized and character...The complex of[N,N,N ’ ,N ’- tetrakis(2 - benzimida zolyl methyl) - 1,4 - diethylene amino] - glycol ether(EGTB)with zinc (Ⅱ) ,[Zn 2 (EGTB)Cl 2 ](ClO 4 ) 2 · CH 3 OH · 3H 2 O was synthesized and characterized with element analysis,UV and IR spectroscopy,and X - ray diffraction method.The crystal belongs to monoclinic with space group of P2 1 /c.The cell parameters are a=1.4376(2)nm,b=2.52650(4)nm,c=1.43531(2)nm,β =101.7037(8) ° ,Z=4,F(000)=2376,D c =1.503g · cm -3 ,The final R=0.0804,wR 2 =0.2236.Biological activities of the complexe was traced by UV - Vis spectrum.The result demonstrates that the complexe has good catalytic abliliy.CCDC:180994.展开更多
以Fe3+/Cu2+为氧化剂,绿色氧化苯偶姻合成了苯偶酰,研究了铜盐、铵盐和硝酸盐的类型及其用量对反应的影响,讨论了可能的反应的机理.结果表明:以10 mmol苯偶姻为原料,2 mL 2%的Cu(OAc)2溶液为氧化剂,10 mmol硝酸铵为助剂,14 mL冰醋酸为溶...以Fe3+/Cu2+为氧化剂,绿色氧化苯偶姻合成了苯偶酰,研究了铜盐、铵盐和硝酸盐的类型及其用量对反应的影响,讨论了可能的反应的机理.结果表明:以10 mmol苯偶姻为原料,2 mL 2%的Cu(OAc)2溶液为氧化剂,10 mmol硝酸铵为助剂,14 mL冰醋酸为溶剂,添加1 g FeCl3.6H2O,回流温度下反应时间可从90 min减少至60 min,苯偶酰的收率高达98.4%,其结构经红外光谱、元素分析等进行了表征.展开更多
文摘5-（Difluoromethoxy）-2-mercapto- 1H-benzimi- dazole （DMB） was precipitated by adding acetic acid to the DMB sodium salt solution. The spherical agglomeration of DMB during the reactive crystallization in a batch crystallizer was monitored by real-time Particle Video Microscope （PVM）. We found that the low feeding rate of acetic acid, high crystallization temperature, low agitation rate or adding seed crystal can facilitate the formation of spherical agglomerates. By using a simple model, the mean crystal agglomerate size of DMB thus predicted is generally in agreement with the experimental data. In addition, the crystallization process of DMB was optimized by a new control strategy of supersaturation to avoid disadvantages brought by agglomeration.
文摘The complex of[N,N,N ’ ,N ’- tetrakis(2 - benzimida zolyl methyl) - 1,4 - diethylene amino] - glycol ether(EGTB)with zinc (Ⅱ) ,[Zn 2 (EGTB)Cl 2 ](ClO 4 ) 2 · CH 3 OH · 3H 2 O was synthesized and characterized with element analysis,UV and IR spectroscopy,and X - ray diffraction method.The crystal belongs to monoclinic with space group of P2 1 /c.The cell parameters are a=1.4376(2)nm,b=2.52650(4)nm,c=1.43531(2)nm,β =101.7037(8) ° ,Z=4,F(000)=2376,D c =1.503g · cm -3 ,The final R=0.0804,wR 2 =0.2236.Biological activities of the complexe was traced by UV - Vis spectrum.The result demonstrates that the complexe has good catalytic abliliy.CCDC:180994.
文摘以Fe3+/Cu2+为氧化剂,绿色氧化苯偶姻合成了苯偶酰,研究了铜盐、铵盐和硝酸盐的类型及其用量对反应的影响,讨论了可能的反应的机理.结果表明:以10 mmol苯偶姻为原料,2 mL 2%的Cu(OAc)2溶液为氧化剂,10 mmol硝酸铵为助剂,14 mL冰醋酸为溶剂,添加1 g FeCl3.6H2O,回流温度下反应时间可从90 min减少至60 min,苯偶酰的收率高达98.4%,其结构经红外光谱、元素分析等进行了表征.
