目前2-羟基对苯二甲酸(2-HTA)的生产主要以间羟基苯甲酸、甲酸钾、二氧化碳为原料实验室制备,未见放大生产的报导。为满足市场需求,以间羟基苯甲酸、碳酸氢钾、碳酸钾和氢氧化钾为原料,加入一定量高沸点溶剂,用改进的Koble-Schmi t t法...目前2-羟基对苯二甲酸(2-HTA)的生产主要以间羟基苯甲酸、甲酸钾、二氧化碳为原料实验室制备,未见放大生产的报导。为满足市场需求,以间羟基苯甲酸、碳酸氢钾、碳酸钾和氢氧化钾为原料,加入一定量高沸点溶剂,用改进的Koble-Schmi t t法放大生产制备2-羟基对苯二甲酸。考察原料配比、反应温度、反应压力和反应时间对产物收率的影响,用高效液相色谱法(HPLC)分析产物纯度,用DSC测定产物的熔点,用FTIR和1H NMR对产物的结构进行表征。在间羟基苯甲酸与碳酸氢钾、碳酸钾和氢氧化钾物质的量比为2.67∶3.77∶1.3∶1,反应温度180℃,反应压力2.0 MPa,反应时间8 h时,粗产品经混合溶剂一次精制,2-羟基对苯二甲酸的收率达74.87%,纯度99.7%,钾金属离子含量19 mg/kg。结果表明改进的Koble-Schmi t t法放大工艺,成本低、步骤少、环境污染小,适合放大生产。展开更多
A new kind of second order nonlinear optical(NLO) material m hydroxybenzoic acid(HBA) was reported in this paper. Primary study results revealed that it had a relatively strong nonlinearity, its powder SHG effect was ...A new kind of second order nonlinear optical(NLO) material m hydroxybenzoic acid(HBA) was reported in this paper. Primary study results revealed that it had a relatively strong nonlinearity, its powder SHG effect was 12 times that of KDP. The solid cut off wavelength λ cut off (350 nm) is very short compared to other organic second order NLO materials. The experimental results also showed that HBA had a high laser damage threshold and good characteristic thermal stability. Furthermore, We calculated its second order nonlinear hyperpolarizability β and analyzed the microscopic nonlinear properties, and found that the hydroxyl group could improve β obviously while the hydroxyl multisubstitution could hardly contribute to β values. [WT5HZ]展开更多
文摘目前2-羟基对苯二甲酸(2-HTA)的生产主要以间羟基苯甲酸、甲酸钾、二氧化碳为原料实验室制备,未见放大生产的报导。为满足市场需求,以间羟基苯甲酸、碳酸氢钾、碳酸钾和氢氧化钾为原料,加入一定量高沸点溶剂,用改进的Koble-Schmi t t法放大生产制备2-羟基对苯二甲酸。考察原料配比、反应温度、反应压力和反应时间对产物收率的影响,用高效液相色谱法(HPLC)分析产物纯度,用DSC测定产物的熔点,用FTIR和1H NMR对产物的结构进行表征。在间羟基苯甲酸与碳酸氢钾、碳酸钾和氢氧化钾物质的量比为2.67∶3.77∶1.3∶1,反应温度180℃,反应压力2.0 MPa,反应时间8 h时,粗产品经混合溶剂一次精制,2-羟基对苯二甲酸的收率达74.87%,纯度99.7%,钾金属离子含量19 mg/kg。结果表明改进的Koble-Schmi t t法放大工艺,成本低、步骤少、环境污染小,适合放大生产。
文摘A new kind of second order nonlinear optical(NLO) material m hydroxybenzoic acid(HBA) was reported in this paper. Primary study results revealed that it had a relatively strong nonlinearity, its powder SHG effect was 12 times that of KDP. The solid cut off wavelength λ cut off (350 nm) is very short compared to other organic second order NLO materials. The experimental results also showed that HBA had a high laser damage threshold and good characteristic thermal stability. Furthermore, We calculated its second order nonlinear hyperpolarizability β and analyzed the microscopic nonlinear properties, and found that the hydroxyl group could improve β obviously while the hydroxyl multisubstitution could hardly contribute to β values. [WT5HZ]
