[Objectives] To establish the high performance liquid chromatography( HPLC) determination method for oxysophocarpine and optimize the extraction and purification technology of oxysophocarpine from Sophora alopecuroide...[Objectives] To establish the high performance liquid chromatography( HPLC) determination method for oxysophocarpine and optimize the extraction and purification technology of oxysophocarpine from Sophora alopecuroides by inverse three-phase membrane cycle.[Methods]Based on the single-factor experiment,the effects of aqueous phase and organic phase volume ratio,the concentration of sodium hydroxide,concentration of hydrochloric acid and extraction cycle time on extraction process of oxysophocarpine were investigated using orthogonal design method,to determine the optimal extraction process. [Results]The oxysophocarpine was determined by Shim-pack VP-ODS chromatographic column( 4. 6 mm × 250 mm,5 μm),mobile phase was methanol-0. 2% phosphoric acid aqueous solution( 7∶ 93),gradient elution,flow rate was 1 m L/min,the sample size was 5 μm,column temperature was 30℃,detection wavelength was 221 nm. Aqueous phase and organic phase volume ratio was 1∶ 1,hydrochloric acid concentration was 0. 3 mol/L,sodium hydroxide concentration was 0. 75 mol/L,water pump flow rate was 6 m L/min,60 min cycle time. The extraction rate of oxysophocarpine 98. 21 % within 60 min under the best experimental conditions. Oxysophocarpine has good linearity relationship within the range of 0. 01-0. 7 mg/m L( r^2= 0. 9978,n = 6),the respective average recovery rate was 97. 47%( RSD = 1. 95%). [Conclusions] This extraction process is simple in operation,the organic solvent has low consumption,and can be used for extraction of alkaloid.展开更多
Helium(He)is commercially produced from natural gas by low-temperature condensation.The process is energy extensive because of the extremely low He concentration(<0.3%)and the operation at cryogenic temperature.Her...Helium(He)is commercially produced from natural gas by low-temperature condensation.The process is energy extensive because of the extremely low He concentration(<0.3%)and the operation at cryogenic temperature.Herein we demonstrated DD3R zeolite membrane was efficient to extract He from natural gas at atmosphere temperature.The membrane performance was evaluated in terms of temperature,pressure and molar fractions.The overall membrane performance was dominated by the diffusivity selectivity.The single He permeance and ideal He/CH_(4) selectivity were 5.8×10^(-9)mol·m^(-2)·s^(-1)·Pa^(-1)and 79 under a feed pressure of 1.3 MPa.Even though He concentration was as low as 0.22%,the He permeance and He/CH_(4) mixture selectivity were 3.0×10^(-9)mol·m^(-2)·s^(-1)·Pa^(-1)and 44 at 0.7 MPa.During the longterm operation(~130 h)the membrane performance was stable even the feed mixture containing3.6%ethane as contaminations.The results approved the feasibility of DD3R zeolite membranes for He extraction from natural gas.展开更多
The based membrane extraction of TI(IV) and Yb(III) was studied with HBTMPP in heptane. The separation process of Th(IV) and Yb(III) was proposed to be a kinetics competition one. The separation of mixture Th(IV) and ...The based membrane extraction of TI(IV) and Yb(III) was studied with HBTMPP in heptane. The separation process of Th(IV) and Yb(III) was proposed to be a kinetics competition one. The separation of mixture Th(IV) and Yb(III) was carried out by two successive extraction and stripping simultaneously. The concentration ratio of TI(IV) and Yb(III) is 16.74 in the stripping solution. The recovery of Th(IV) is 71.6%. The purity of Th(IV) is 95.74%. The separation factor of Th(IV) and Yb(III) is 2.52×106, which was obtained by interfacial kinetics.展开更多
The present research work examines extraction mechanism of zinc by D2 EHPA(Di-2-ethyl hexyl phosphoric acid) and comprehensively studies the main effective parameters on the process. Results of thermodynamic experimen...The present research work examines extraction mechanism of zinc by D2 EHPA(Di-2-ethyl hexyl phosphoric acid) and comprehensively studies the main effective parameters on the process. Results of thermodynamic experiments showed that zinc extraction by D2 EHPA was endothermic and spontaneous, and thermodynamic parameters including entropy and enthalpy were + 27.37 J·mol^(-1)·K^(-1) and 25.21 kJ·mol^(-1), respectively.Gibbs free energy was varied between-7.21 kJ·mol^(-1) and-8.41 kJ·mol^(-1) with the variation of temperature from 20 °C to 70 °C. Solution ionic strength was increased by addition of potassium and lithium sulfate solution while addition of calcium sulfate decreased ionic strength whereby zinc extraction efficiency was also decreased.TBP showed positive synergism at concentration of 5%(v/v) and negative synergism effect at concentrations of2% and 10%. Simultaneous addition of both TBP and salt caused extraction efficiency to drop significantly and lower both TBP and ionic strength efficiency. Results showed that a continuous addition of TBP tends to effectively improve the zinc extraction efficiency. Experiments in the presence of catalyst Ni-Raney demonstrated that zinc extraction kinetic increases remarkably and due to easy recycling of the catalyst, we can propose a novel idea in solvent extraction field.展开更多
针对煤炭地下气化(UCG)技术制备的合成气具有温度高(>200℃)、压力大(3.35 MPa)、饱和含水量大及组分复杂(含CH_(4)、H_(2)、CO_(2)和CO等)的特点,设计并采用膜分离+溶剂吸收耦合的处理方法以实现地下煤合成气中CO_(2)的脱除和H_(2)...针对煤炭地下气化(UCG)技术制备的合成气具有温度高(>200℃)、压力大(3.35 MPa)、饱和含水量大及组分复杂(含CH_(4)、H_(2)、CO_(2)和CO等)的特点,设计并采用膜分离+溶剂吸收耦合的处理方法以实现地下煤合成气中CO_(2)的脱除和H_(2)的提纯。地下煤合成气经过二级膜分离单元的处理,实现了CO_(2)/H_(2)与CH_(4)的分离并得到了脱碳净化气,其中CO_(2)含量(物质的量分数)≤3%,该膜分离工艺所需能耗为0.297 k W·h/m^(3)。使用醇胺吸收法处理CO_(2)/H_(2)混合气,并通过配方溶液筛选、工艺流程优化和校验分析等方法开展了研究,最终得到了H_(2)纯度(物质的量分数)≥99%的产品,该醇胺吸收法的能耗为0.341 k W·h/m^(3)。使用膜分离+溶剂吸收耦合处理复杂工况的地下煤合成气,可得到脱碳净化气、纯CO_(2)和工业级H_(2),提高了项目的经济价值,具有较大的应用潜力。展开更多
基金Supported by Project of National Natural Science Foundation(21162030)
文摘[Objectives] To establish the high performance liquid chromatography( HPLC) determination method for oxysophocarpine and optimize the extraction and purification technology of oxysophocarpine from Sophora alopecuroides by inverse three-phase membrane cycle.[Methods]Based on the single-factor experiment,the effects of aqueous phase and organic phase volume ratio,the concentration of sodium hydroxide,concentration of hydrochloric acid and extraction cycle time on extraction process of oxysophocarpine were investigated using orthogonal design method,to determine the optimal extraction process. [Results]The oxysophocarpine was determined by Shim-pack VP-ODS chromatographic column( 4. 6 mm × 250 mm,5 μm),mobile phase was methanol-0. 2% phosphoric acid aqueous solution( 7∶ 93),gradient elution,flow rate was 1 m L/min,the sample size was 5 μm,column temperature was 30℃,detection wavelength was 221 nm. Aqueous phase and organic phase volume ratio was 1∶ 1,hydrochloric acid concentration was 0. 3 mol/L,sodium hydroxide concentration was 0. 75 mol/L,water pump flow rate was 6 m L/min,60 min cycle time. The extraction rate of oxysophocarpine 98. 21 % within 60 min under the best experimental conditions. Oxysophocarpine has good linearity relationship within the range of 0. 01-0. 7 mg/m L( r^2= 0. 9978,n = 6),the respective average recovery rate was 97. 47%( RSD = 1. 95%). [Conclusions] This extraction process is simple in operation,the organic solvent has low consumption,and can be used for extraction of alkaloid.
基金sponsored by the National Natural Science Foundation of China(21908097,22035002)the National Key Research and Development Program of China(2021YFC2101203)+1 种基金Jiangsu Specially-Appointed Professors Program and"333 Talent Project"of Jiangsu ProvinceState Key Laboratory of Materials-Oriented Chemical Engineering(ZK202002)。
文摘Helium(He)is commercially produced from natural gas by low-temperature condensation.The process is energy extensive because of the extremely low He concentration(<0.3%)and the operation at cryogenic temperature.Herein we demonstrated DD3R zeolite membrane was efficient to extract He from natural gas at atmosphere temperature.The membrane performance was evaluated in terms of temperature,pressure and molar fractions.The overall membrane performance was dominated by the diffusivity selectivity.The single He permeance and ideal He/CH_(4) selectivity were 5.8×10^(-9)mol·m^(-2)·s^(-1)·Pa^(-1)and 79 under a feed pressure of 1.3 MPa.Even though He concentration was as low as 0.22%,the He permeance and He/CH_(4) mixture selectivity were 3.0×10^(-9)mol·m^(-2)·s^(-1)·Pa^(-1)and 44 at 0.7 MPa.During the longterm operation(~130 h)the membrane performance was stable even the feed mixture containing3.6%ethane as contaminations.The results approved the feasibility of DD3R zeolite membranes for He extraction from natural gas.
基金Acknowledgements- This project supported by State Key Project of Fundamental Research (GrantNo.1998061302) and the National Na
文摘The based membrane extraction of TI(IV) and Yb(III) was studied with HBTMPP in heptane. The separation process of Th(IV) and Yb(III) was proposed to be a kinetics competition one. The separation of mixture Th(IV) and Yb(III) was carried out by two successive extraction and stripping simultaneously. The concentration ratio of TI(IV) and Yb(III) is 16.74 in the stripping solution. The recovery of Th(IV) is 71.6%. The purity of Th(IV) is 95.74%. The separation factor of Th(IV) and Yb(III) is 2.52×106, which was obtained by interfacial kinetics.
基金This work was supported by the National Basic Research Program of China （973 program, Grant Nos. 2013CB733600 and 2012CB72520）, the National Natural Science Foundation of China （Grant Nos. 21390202 and 21436002）.
文摘The present research work examines extraction mechanism of zinc by D2 EHPA(Di-2-ethyl hexyl phosphoric acid) and comprehensively studies the main effective parameters on the process. Results of thermodynamic experiments showed that zinc extraction by D2 EHPA was endothermic and spontaneous, and thermodynamic parameters including entropy and enthalpy were + 27.37 J·mol^(-1)·K^(-1) and 25.21 kJ·mol^(-1), respectively.Gibbs free energy was varied between-7.21 kJ·mol^(-1) and-8.41 kJ·mol^(-1) with the variation of temperature from 20 °C to 70 °C. Solution ionic strength was increased by addition of potassium and lithium sulfate solution while addition of calcium sulfate decreased ionic strength whereby zinc extraction efficiency was also decreased.TBP showed positive synergism at concentration of 5%(v/v) and negative synergism effect at concentrations of2% and 10%. Simultaneous addition of both TBP and salt caused extraction efficiency to drop significantly and lower both TBP and ionic strength efficiency. Results showed that a continuous addition of TBP tends to effectively improve the zinc extraction efficiency. Experiments in the presence of catalyst Ni-Raney demonstrated that zinc extraction kinetic increases remarkably and due to easy recycling of the catalyst, we can propose a novel idea in solvent extraction field.
文摘针对煤炭地下气化(UCG)技术制备的合成气具有温度高(>200℃)、压力大(3.35 MPa)、饱和含水量大及组分复杂(含CH_(4)、H_(2)、CO_(2)和CO等)的特点,设计并采用膜分离+溶剂吸收耦合的处理方法以实现地下煤合成气中CO_(2)的脱除和H_(2)的提纯。地下煤合成气经过二级膜分离单元的处理,实现了CO_(2)/H_(2)与CH_(4)的分离并得到了脱碳净化气,其中CO_(2)含量(物质的量分数)≤3%,该膜分离工艺所需能耗为0.297 k W·h/m^(3)。使用醇胺吸收法处理CO_(2)/H_(2)混合气,并通过配方溶液筛选、工艺流程优化和校验分析等方法开展了研究,最终得到了H_(2)纯度(物质的量分数)≥99%的产品,该醇胺吸收法的能耗为0.341 k W·h/m^(3)。使用膜分离+溶剂吸收耦合处理复杂工况的地下煤合成气,可得到脱碳净化气、纯CO_(2)和工业级H_(2),提高了项目的经济价值,具有较大的应用潜力。
