通过设计正交试验,以1,4-二乙氧基苯为原材料,碘为催化剂,二氯甲烷、冰醋酸为溶剂,制备得到1,4-二溴-2,5-二乙氧基苯并优化试验条件。以1,4-二乙氧基苯1.66 g(0.01 mol),二氯甲烷15 m L为不变量,得到最佳试验条件:反应时间10 h,V(CH3CO...通过设计正交试验,以1,4-二乙氧基苯为原材料,碘为催化剂,二氯甲烷、冰醋酸为溶剂,制备得到1,4-二溴-2,5-二乙氧基苯并优化试验条件。以1,4-二乙氧基苯1.66 g(0.01 mol),二氯甲烷15 m L为不变量,得到最佳试验条件:反应时间10 h,V(CH3COOH)∶V(CH2Cl2)=1∶3,0.7 m L溴,0.03 g碘。并通过红外、核磁共振氢谱和碳谱进行表征。展开更多
Diethylene glycol was selected as sovlent of extraction separation for DEM and Ethanol aqueous.The effects of the the theory plate numbers and the ratio of raw material/solvent to extraction separation were researcheh...Diethylene glycol was selected as sovlent of extraction separation for DEM and Ethanol aqueous.The effects of the the theory plate numbers and the ratio of raw material/solvent to extraction separation were researcheh.The results show that recovery ratio of DEM reach 99%.The pure component of DEM reachs 995%.The simulation results were provided for middle test.展开更多
The synthesis of diethoxy methane was studied using ethanol and formaldehyde as the raw materials and toluene-p-sulfonic acid as the catalyst.It was found that when the mole ratio of ethanol to formaldehyde was 3.97∶...The synthesis of diethoxy methane was studied using ethanol and formaldehyde as the raw materials and toluene-p-sulfonic acid as the catalyst.It was found that when the mole ratio of ethanol to formaldehyde was 3.97∶[KG-*3/5]1,the mole ratio of toluene-p-sulfonic acid to the total raw materials 7%,the reaction temperature 25 ℃,the stirring speed 70 r/min and the reaction time 10 min,the yield of DEM was about 90.4%.Under the above reaction conditions,the yield was about 62.3% using HCl as the catalyst,and the amount of water in the product was higher and the waste acid in the continuous reaction would pollute the environment.In(addition) toluene-p-sulfonic acid can be used repeatedly.Therefore,this synthesis method is useful the practical production of diethoxy methane.展开更多
以1,5-二乙氧基-2,4-二硝基苯为原料,乙醇为溶剂,经铁粉还原得4,6-二乙氧基间苯二胺,较佳工艺条件为:V(水)∶V(乙醇)=1∶4.5,反应温度80℃,反应时间2h,滤液在氯化亚锡保护下加入盐酸后制得盐酸盐,旋蒸浓缩,-20℃下静置16h析出产物,氮气...以1,5-二乙氧基-2,4-二硝基苯为原料,乙醇为溶剂,经铁粉还原得4,6-二乙氧基间苯二胺,较佳工艺条件为:V(水)∶V(乙醇)=1∶4.5,反应温度80℃,反应时间2h,滤液在氯化亚锡保护下加入盐酸后制得盐酸盐,旋蒸浓缩,-20℃下静置16h析出产物,氮气吹干,收率88%,纯度大于99%。又以4,6-二乙氧基间苯二胺为原料合成衍生物Ⅰ—Ⅴ,结构经FT-IR、13 C NMR和1 H NMR表征确认,并对其在大分子、染料以及材料方面的应用进行了分析.展开更多
文摘通过设计正交试验,以1,4-二乙氧基苯为原材料,碘为催化剂,二氯甲烷、冰醋酸为溶剂,制备得到1,4-二溴-2,5-二乙氧基苯并优化试验条件。以1,4-二乙氧基苯1.66 g(0.01 mol),二氯甲烷15 m L为不变量,得到最佳试验条件:反应时间10 h,V(CH3COOH)∶V(CH2Cl2)=1∶3,0.7 m L溴,0.03 g碘。并通过红外、核磁共振氢谱和碳谱进行表征。
文摘Diethylene glycol was selected as sovlent of extraction separation for DEM and Ethanol aqueous.The effects of the the theory plate numbers and the ratio of raw material/solvent to extraction separation were researcheh.The results show that recovery ratio of DEM reach 99%.The pure component of DEM reachs 995%.The simulation results were provided for middle test.
文摘The synthesis of diethoxy methane was studied using ethanol and formaldehyde as the raw materials and toluene-p-sulfonic acid as the catalyst.It was found that when the mole ratio of ethanol to formaldehyde was 3.97∶[KG-*3/5]1,the mole ratio of toluene-p-sulfonic acid to the total raw materials 7%,the reaction temperature 25 ℃,the stirring speed 70 r/min and the reaction time 10 min,the yield of DEM was about 90.4%.Under the above reaction conditions,the yield was about 62.3% using HCl as the catalyst,and the amount of water in the product was higher and the waste acid in the continuous reaction would pollute the environment.In(addition) toluene-p-sulfonic acid can be used repeatedly.Therefore,this synthesis method is useful the practical production of diethoxy methane.
文摘以1,5-二乙氧基-2,4-二硝基苯为原料,乙醇为溶剂,经铁粉还原得4,6-二乙氧基间苯二胺,较佳工艺条件为:V(水)∶V(乙醇)=1∶4.5,反应温度80℃,反应时间2h,滤液在氯化亚锡保护下加入盐酸后制得盐酸盐,旋蒸浓缩,-20℃下静置16h析出产物,氮气吹干,收率88%,纯度大于99%。又以4,6-二乙氧基间苯二胺为原料合成衍生物Ⅰ—Ⅴ,结构经FT-IR、13 C NMR和1 H NMR表征确认,并对其在大分子、染料以及材料方面的应用进行了分析.
