The title compound has been synthesized by the reaction of 3,3-dimethyl-1-（1H-1,2,4-triazol-1-yl）butan-2-one oxime with 2-chlorobenzyl chloride, and then treated with 65～68% HNO3. Its crystal structure was determin...The title compound has been synthesized by the reaction of 3,3-dimethyl-1-（1H-1,2,4-triazol-1-yl）butan-2-one oxime with 2-chlorobenzyl chloride, and then treated with 65～68% HNO3. Its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 14.5481（8）, b = 9.3351（5）, c = 13.1911（7） , β = 98.9450（10）°, Z = 4, V = 1769.67（17） 3, Mr = 369.81, Dc = 1.388 g/cm3, S = 1.06, μ = 0.247 mm-1, F（000） = 776, the final R = 0.0352 and wR = 0.0960 for 3069 observed reflections （I 2σ（I））. X-ray crystal structure presents the intramolecular N–H…O hydrogen bond. The packing is nearly parallel without π-π stacking interactions between two adjacent phenyl rings and stabilized by Van der Waals force. The preliminary bioassay shows that the title compound possesses fungicidal activity against Gibberella zeae at the dosage of 25 mg/L.展开更多
The chemoselectivities of PdCl2 and CuCl2-catalyzed oligomerization of 3, 3-dimethyl-butyne: 1, 3, 5-tri-tert-butylbenzene, 2, 2, 7, 7-tetramethyl-3, 6-dichloro-3, 5-octadiene and 2, 2, 7, 7- tetramethyl-3, 5-octadiyn...The chemoselectivities of PdCl2 and CuCl2-catalyzed oligomerization of 3, 3-dimethyl-butyne: 1, 3, 5-tri-tert-butylbenzene, 2, 2, 7, 7-tetramethyl-3, 6-dichloro-3, 5-octadiene and 2, 2, 7, 7- tetramethyl-3, 5-octadiyne were obtained, respectively, by regulating the polarity of the solvent.展开更多
The title compound 1-（3-amino-[1,2,4]triazol-1-yl）-3,3-dimethyl-butan-2-one（3） was synthesized by Hofmann-alkylation reaction of 1-chloro-3,3-dimethyl-butan-2-one（1） and ~1H-[1,2,4]triazol-3-ylamine（2） with eq...The title compound 1-（3-amino-[1,2,4]triazol-1-yl）-3,3-dimethyl-butan-2-one（3） was synthesized by Hofmann-alkylation reaction of 1-chloro-3,3-dimethyl-butan-2-one（1） and ~1H-[1,2,4]triazol-3-ylamine（2） with equal amount of K_2CO_3 as acid acceptor. The structure of compound 3 was characterized by ~1H NMR, 13 C NMR, HRMS and single-crystal X-ray diffraction. The compound crystallizes in the monoclinic system, space group P21/n with a = 5.7227（8）, b = 27.924（4）, c = 6.2282（7） ？, β = 101.892（11）°, V = 973.9（2） ？~3, Z = 4, T = 180.00（10） K, μ（MoKα） = 0.087 mm^（-1）, Dc = 1.243 g/cm^3, 3832 reflections measured（3.648≤θ≤26.022°）, 1916 unique reflections（Rint = 0.0359, Rsigma = 0.0572） used in all calculations. The final R = 0.0557（I 〉 2σ（I）） and w R = 0.1276（all data）. Bioassay showed that 3 displayed excellent activity as plant growth regulator with inducing lateral root formation and enhancing primary root elongation at 0.27 mmol/L（50 ppm） in soybeen（He Feng-50）. Good water solubility was found with 50 mg in 1 m L of water. Therefore, application of 3 in agriculture is more environmentally friendly due to cosolvent-free condition, and results in improved abiotic-stress tolerance by affecting the root growth. And furthermore, it can be used as a precursor to investigate the function of regulating plant root growth.展开更多
1, 3-Dimethyluracil （DMU） in phosphate buffered-saline （PBS, pH=8） was irradiated by a medium pressure mercury lamp （MPML） and produced a novel compound C6H9N2O6P. The composition and structure of the compound h...1, 3-Dimethyluracil （DMU） in phosphate buffered-saline （PBS, pH=8） was irradiated by a medium pressure mercury lamp （MPML） and produced a novel compound C6H9N2O6P. The composition and structure of the compound has been identified by elemental analysis, EIMS, UV, IR, ^1H and ^31P-NMR.展开更多
Background:The 2-amino-5-chloro-N,3-dimethylbenzamide is a key intermediate in the synthesis of pesticides and pharmaceuticals.However,no literature currently exists on 2-amino-5-chloro-N,3-dimethylbenzamide poisoning...Background:The 2-amino-5-chloro-N,3-dimethylbenzamide is a key intermediate in the synthesis of pesticides and pharmaceuticals.However,no literature currently exists on 2-amino-5-chloro-N,3-dimethylbenzamide poisoning in humans.This study aimed to reveal the health hazard of this chemical for humans and summarize the clinical characteristics of patients with occupational 2-amino-5-chloro-N,3-dimethylbenzamide poisoning.Methods:This observational study included four patients with 2-amino-5-chloro-N,3-dimethylbenzamide poisoning from June 2022 to July 2022.The entire course of the incidents was described in detail.Blood 2-amino-5-chloro-N,3-dimethylbenzamide concentrations were detected by a mass spectrometer.Hema-toxylin and eosin staining was performed to assess liver injury,and immunofluorescence was used to evaluate hepatic mitophagy.Results:The 2-amino-5-chloro-N,3-dimethylbenzamide powder(99%purity)entered the human body mainly via the skin and respiratory tract due to poor personal protective measures.The typical course of 2-amino-5-chloro-N,3-dimethylbenzamide poisoning was divided into latency,rash,fever,organic dam-age,and recovery phases in accordance with the clinical evolution.Rash and fever may be the important premonitory symptoms for further organ injuries.The chemical was detected in the blood of all patients and caused multiple organ injuries,predominantly liver injury,including kidney,myocardium,and micro-circulation.Three patients recovered smoothly after comprehensive treatments,including artificial liver therapy,continuous renal replacement therapy,glucocorticoids,and other symptomatic and supportive treatments.One patient survived by liver transplantation.The postoperative pathological findings of the removed liver showed acute liver failure,and immunofluorescence staining confirmed the abundance of mitophagy in residual hepatocytes.Conclusions:This study is the first to elaborate the clinical characteristics of patients with 2-amino-5-chloro-N,3-dimethylbenzamide poisoning.The chemical enters the body through the respiratory tract and skin during industrial production.The 2-amino-5-chloro-N,3-dimethylbenzamide poisoning causes multiple-organ dysfunction with a predominance of liver injury.Liver transplantation may be an effective option for patients with severe liver failure.The mechanisms of liver injury induced by 2-amino-5-chloro-N,3-dimethylbenzamide might involve abnormal mitochondrial function and mitophagy.展开更多
（2,3-Dimethylbutyl）（2,4,40-trimethylpentyl）phosphinic acid（INET-3） was impregnated onto dry macroporous resins XAD-16 and pretreated XAD-16 with ethyl alcohol and HCl（Pre-XAD-16） to prepare the solvent impregn...（2,3-Dimethylbutyl）（2,4,40-trimethylpentyl）phosphinic acid（INET-3） was impregnated onto dry macroporous resins XAD-16 and pretreated XAD-16 with ethyl alcohol and HCl（Pre-XAD-16） to prepare the solvent impregnated resins SIRs-INET-3/XAD-16 and SIRs-INET-3/Pre-XAD-16. The molecular weight distribution of the low molecular weight（LMW） polymers washed off by ethyl alcohol during XAD-16 pretreatment was determined by gel permeation chromatography（GPC）. The macroporous resins（XAD-16 ＆ Pre-XAD-16）, the corresponding solvent impregnated resins（SIRs-INET-3/XAD-16 ＆SIRs-INET-3/Pre-XAD-16） and the PVA coated SIRs-INET-3/Pre-XAD-16 with boric acid as cross-linking agent were characterized by FT-IR, SEM-EDS and TGA. The effects of XAD-16 pretreatment and PVA coating technology on RE（III） adsorption equilibrium time, INET-3 losses during extraction and adsorption capacity were investigated. The adsorption kinetics, selectivity and stripping behaviors of SIRs-INET-3/XAD-16 were further studied. The washed off LMW polymers had the Mn of 36,656, Mw of 40,310 and polydispersity coefficient of 1.10. The SIRs-INET-3/XAD-16 had shorter equilibrium time,less INET-3 loss and more Tm（III） adsorption capacity than the SIRs-INET-3/Pre-XAD-16. The PVA coated SIRs-INET-3/Pre-XAD-16 had less INET-3 loss and more Tm（III） adsorption capacity but longer equilibrium time than the uncoated SIRs-INET-3/Pre-XAD-16. The adsorption of RE（III） on the SIRsINET-3/XAD-16 followed the pseudo-second-order kinetic model. The Tm（III） accumulative adsorption amounts onto SIRs-INET-3/XAD-16 after eight extraction stages was 23.6 mg/g. The separation factors of adjacent heavy RE（III） β（Er/Ho）, β（Tm/Er）, β（Yb/Tm） and β（Lu/Yb） values were 1.76, 2.59, 2.56 and 1.19,respectively. The adsorbed Lu（III） onto the SIRs-INET-3/XAD-16 can be stripped completely by 1.0 mol/L H2SO4.展开更多
In absorption cycles,ionic liquid(IL)1,3-dimethylimidazolium tetrafluoroborate([Dmim]BF4)may be a promising absorbent of working pair using water as refrigerant.The vapor pressures of[Dmim]BF4 aqueous solution were me...In absorption cycles,ionic liquid(IL)1,3-dimethylimidazolium tetrafluoroborate([Dmim]BF4)may be a promising absorbent of working pair using water as refrigerant.The vapor pressures of[Dmim]BF4 aqueous solution were measured with the boiling-point method in the temperature range from 312.25 to 403.60 K and in the mass concentration range of 65%to 90%of[Dmim]BF4.The experimental data were correlated with an Antoine-type equation and the Non-Random Two-Liquid(NRTL)model,and the average absolute deviations between the experimental and calculated values were 1.06%and 1.15%,respectively.For the[Dmim]BF4 aqueous solution,the experimental vapor pressures show negative deviations from the calculated data with Raoult's law.For higher mass concentration of the IL,the deviation is more negative.In addition,the vapor pressures,the hydrophilicity and the solubility of[Dmim]BF4 aqueous solutions were compared with those of[Dmim]Cl aqueous solutions and [Bmim]BF4 aqueous solutions at IL-mole fraction of 0.20.展开更多
Carbon-coated Fe3O4（ Fe3O4/C） microspheres activated with 1-ethyl-3-（3-dimethylaminopropyl）-carbodiimide hydrochloride（EDC） were prepared, characterized and applied to adsorb bovine serum albumin（BSA）. The pre...Carbon-coated Fe3O4（ Fe3O4/C） microspheres activated with 1-ethyl-3-（3-dimethylaminopropyl）-carbodiimide hydrochloride（EDC） were prepared, characterized and applied to adsorb bovine serum albumin（BSA）. The prepared magnetic microspheres had spherical core-shell structure with a uniform and continuous carbon coating coupled with activation by EDC, and possessed superparamagnetic characteristics. The experimental results showed that the adsorption amount of BSA on the EDC-activated Fe3O4/C（Fe3O4/C-EDC） microspheres was higher than that on the Fe3O4/C microspheres. The maximum adsorption of BSA on Fe3O4/C-EDC microspheres occurred at pH 4.7, which was the isoelectric point of BSA. At low concentrations（below 1.0 M）, salt had no noticeable effect on BSA adsorption. The BSA adsorption of Fe3O4/C-EDC microspheres had a better fit to the Langmuir model than the Freundlich isotherm and Temkin isotherm model, and the kinetic data were well described by the pseudo-second-order model. The adsorption equilibrium could be reached within 20 min. High desorption efficiency（97.6%） of BSA from Fe3O4/C-EDC microspheres was obtained with 0.5 M Na2HPO4（pH 9.4） as the desorbent.展开更多
The title compound 7-amino-2,3,4,5-tetrahydro-1,3-dimethyl-5-（2-nitrophenyl）- 2,4- dioxo-1H-pyrano[2,3-d] pyrirnidine-6-carbonitrile DMF solvate 1 （C19H20N6O6, Mr = 428.41） was synthesized and crystallized. The cr...The title compound 7-amino-2,3,4,5-tetrahydro-1,3-dimethyl-5-（2-nitrophenyl）- 2,4- dioxo-1H-pyrano[2,3-d] pyrirnidine-6-carbonitrile DMF solvate 1 （C19H20N6O6, Mr = 428.41） was synthesized and crystallized. The crystal belongs to the monoclinic system, space group P2 1/c with a = 11.383（2）, b = 13.372（2）, c = 13.673（2）A, β = 97.380（4）°, Z = 4, V = 2063.8（6）A^3, Dc = 1.379 g/cm^3,μ（MoKα） = 0.105 mm^-1, F（000） = 896, the final R = 0.0738 and wR = 0.1647 for 2964 observed reflections （I〉 2σ（I））. X-ray analysis reveals that the new pyran ring is coplanar, which is obviously different from those of other similar compounds. In addition, the unclassical hydrogen bonds of C-H…O and C-H…N are presented in the crystals except for the normal hydrogen bonds of N-H…O.展开更多
The solid-liquid equilibria of musk ketone + musk xylene, musk xylene +l,3-dimethyl-2,4-dinitro-5-tert-butyl benzene are measured by differential scanning calorimeter (DSC), these systems are proved to be simple eutec...The solid-liquid equilibria of musk ketone + musk xylene, musk xylene +l,3-dimethyl-2,4-dinitro-5-tert-butyl benzene are measured by differential scanning calorimeter (DSC), these systems are proved to be simple eutectics. Moreover the melting points and the fusion enthalpies of musk ketone, musk xylene and 1,3-dimethyl-2,4-dinitro-5-tert-butyl benzene are also measured by the DSC. These solid-liquid equilibrium data and the heats of fusion are reported for the first time. Then UNIFAC model is used to correlate the sofid-liquid equilibrium data. It is shown that the solid-liquid equilibria of musk systems can be predicted by the UNIFAC model.展开更多
The formaidehyde-free finishing agent 4,5-di-hydroxy-1,3-dimethy1-2-imidazolidinone(DMeDHEU)was prepared by the reaction of 1,3-dimethylurea and glyoxal.The reaction rate and equilib-rium conversion in relation to pH ...The formaidehyde-free finishing agent 4,5-di-hydroxy-1,3-dimethy1-2-imidazolidinone(DMeDHEU)was prepared by the reaction of 1,3-dimethylurea and glyoxal.The reaction rate and equilib-rium conversion in relation to pH value,molar ratio,temperature and catalyst were studied.The conversionto DMeDHEU,catalyzed with citric acid/anhydrousNaAc,reached 95% in 6 hours at 40℃, pH 5.5 andmolar ratio 1.2.展开更多
The photophysics of 3-dimethylamino-2-methyl-propenal （DMAMP） after excitation to the S2 （ππ^＊） electronic state was studied using the resonance Raman spectroscopy and complete active space self-consistent fiel...The photophysics of 3-dimethylamino-2-methyl-propenal （DMAMP） after excitation to the S2 （ππ^＊） electronic state was studied using the resonance Raman spectroscopy and complete active space self-consistent field method calculations. The transition barriers of the ground state tautomerization reactions between DMAMP and its three isomers were determined at B3LYP/6-311＋＋G（d,p） level of theory. The vibrational spectra were assigned. The A- band resonance Raman spectra were obtained in acetonitrile with excitation wavelengths in resonance with the first intense absorption band to probe the structural dynamics of DMAMP. The B3LYP-TD computation was carried out to determine the relative A-band resonance Raman intensities of the fundamental modes, and the result indicated that the vibronic-coupling existed in Franck-Condon region. Complete active space self-consistent field （CASSCF） calculations were carried out to determine the excitation energies of the lower-lying singlet and triplet excited states, the conical intersection points and the intersystem crossing points. The A-band short-time structural dynamics and the corresponding decay dynamics of DMAMP were obtained by analysis of the resonance Raman intensity pattern and CASSCF computations. It was found that a sudden de-conjugation between C1=O6 and C2=C3 occurred at the Franck-Condon region of the S2（ππ^＊） state, while the enhancement of the conjugation interaction between C3 and N（CH3）2, and between C1 and C2 evolutions shortly after the wavepacket leaves away the Pranck-Condon region via the excited state charge redistribution. The de-conjugation interaction between C1=O6 and C2=C3 made the rotation of C3=N（CH3）2 group around the C2-C3 bond much easier, while the enhanced conjugation between C1 and C2, and between C3 and N（CH3）2 made the rotation around the C1-C2 bond and C3-N5 more difficult. It was revealed that the initial structural dynamics of DMAMP was predominantly towards the CI-I（S2/S0） point, while the opportunities towards either CI-2（S2/S0） or CI-3（S2/S0） point were negligible. Two decay channels of DMAMP from S2,FC（ππ^＊） to So or Tl,min via various CIs and ISCs were proposed.展开更多
基金Supported by the Central University Basic Scientific Research Fund of Hunan University (2009)the Key Scientific and Technological Project of Changsha, Hunan Province (No. 0901077-31)
文摘The title compound has been synthesized by the reaction of 3,3-dimethyl-1-（1H-1,2,4-triazol-1-yl）butan-2-one oxime with 2-chlorobenzyl chloride, and then treated with 65～68% HNO3. Its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 14.5481（8）, b = 9.3351（5）, c = 13.1911（7） , β = 98.9450（10）°, Z = 4, V = 1769.67（17） 3, Mr = 369.81, Dc = 1.388 g/cm3, S = 1.06, μ = 0.247 mm-1, F（000） = 776, the final R = 0.0352 and wR = 0.0960 for 3069 observed reflections （I 2σ（I））. X-ray crystal structure presents the intramolecular N–H…O hydrogen bond. The packing is nearly parallel without π-π stacking interactions between two adjacent phenyl rings and stabilized by Van der Waals force. The preliminary bioassay shows that the title compound possesses fungicidal activity against Gibberella zeae at the dosage of 25 mg/L.
文摘The chemoselectivities of PdCl2 and CuCl2-catalyzed oligomerization of 3, 3-dimethyl-butyne: 1, 3, 5-tri-tert-butylbenzene, 2, 2, 7, 7-tetramethyl-3, 6-dichloro-3, 5-octadiene and 2, 2, 7, 7- tetramethyl-3, 5-octadiyne were obtained, respectively, by regulating the polarity of the solvent.
基金supported by the National Natural Science Foundation of China(No.2012BAD20B04)
文摘The title compound 1-（3-amino-[1,2,4]triazol-1-yl）-3,3-dimethyl-butan-2-one（3） was synthesized by Hofmann-alkylation reaction of 1-chloro-3,3-dimethyl-butan-2-one（1） and ~1H-[1,2,4]triazol-3-ylamine（2） with equal amount of K_2CO_3 as acid acceptor. The structure of compound 3 was characterized by ~1H NMR, 13 C NMR, HRMS and single-crystal X-ray diffraction. The compound crystallizes in the monoclinic system, space group P21/n with a = 5.7227（8）, b = 27.924（4）, c = 6.2282（7） ？, β = 101.892（11）°, V = 973.9（2） ？~3, Z = 4, T = 180.00（10） K, μ（MoKα） = 0.087 mm^（-1）, Dc = 1.243 g/cm^3, 3832 reflections measured（3.648≤θ≤26.022°）, 1916 unique reflections（Rint = 0.0359, Rsigma = 0.0572） used in all calculations. The final R = 0.0557（I 〉 2σ（I）） and w R = 0.1276（all data）. Bioassay showed that 3 displayed excellent activity as plant growth regulator with inducing lateral root formation and enhancing primary root elongation at 0.27 mmol/L（50 ppm） in soybeen（He Feng-50）. Good water solubility was found with 50 mg in 1 m L of water. Therefore, application of 3 in agriculture is more environmentally friendly due to cosolvent-free condition, and results in improved abiotic-stress tolerance by affecting the root growth. And furthermore, it can be used as a precursor to investigate the function of regulating plant root growth.
基金The project was supported by the National Natural Science Foundation of China(No:20171038).
文摘1, 3-Dimethyluracil （DMU） in phosphate buffered-saline （PBS, pH=8） was irradiated by a medium pressure mercury lamp （MPML） and produced a novel compound C6H9N2O6P. The composition and structure of the compound has been identified by elemental analysis, EIMS, UV, IR, ^1H and ^31P-NMR.
基金This work was supported by grants from the Key Research and Development Program of Zhejiang Province(2019C03076)the Fundamental Research Funds for the Central Universities(226-2022-00088).
文摘Background:The 2-amino-5-chloro-N,3-dimethylbenzamide is a key intermediate in the synthesis of pesticides and pharmaceuticals.However,no literature currently exists on 2-amino-5-chloro-N,3-dimethylbenzamide poisoning in humans.This study aimed to reveal the health hazard of this chemical for humans and summarize the clinical characteristics of patients with occupational 2-amino-5-chloro-N,3-dimethylbenzamide poisoning.Methods:This observational study included four patients with 2-amino-5-chloro-N,3-dimethylbenzamide poisoning from June 2022 to July 2022.The entire course of the incidents was described in detail.Blood 2-amino-5-chloro-N,3-dimethylbenzamide concentrations were detected by a mass spectrometer.Hema-toxylin and eosin staining was performed to assess liver injury,and immunofluorescence was used to evaluate hepatic mitophagy.Results:The 2-amino-5-chloro-N,3-dimethylbenzamide powder(99%purity)entered the human body mainly via the skin and respiratory tract due to poor personal protective measures.The typical course of 2-amino-5-chloro-N,3-dimethylbenzamide poisoning was divided into latency,rash,fever,organic dam-age,and recovery phases in accordance with the clinical evolution.Rash and fever may be the important premonitory symptoms for further organ injuries.The chemical was detected in the blood of all patients and caused multiple organ injuries,predominantly liver injury,including kidney,myocardium,and micro-circulation.Three patients recovered smoothly after comprehensive treatments,including artificial liver therapy,continuous renal replacement therapy,glucocorticoids,and other symptomatic and supportive treatments.One patient survived by liver transplantation.The postoperative pathological findings of the removed liver showed acute liver failure,and immunofluorescence staining confirmed the abundance of mitophagy in residual hepatocytes.Conclusions:This study is the first to elaborate the clinical characteristics of patients with 2-amino-5-chloro-N,3-dimethylbenzamide poisoning.The chemical enters the body through the respiratory tract and skin during industrial production.The 2-amino-5-chloro-N,3-dimethylbenzamide poisoning causes multiple-organ dysfunction with a predominance of liver injury.Liver transplantation may be an effective option for patients with severe liver failure.The mechanisms of liver injury induced by 2-amino-5-chloro-N,3-dimethylbenzamide might involve abnormal mitochondrial function and mitophagy.
基金Project supported by the National Natural Science Foundation of China(21301104)the State Key Laboratory of Chemical Engineering(SKLCh E-14A04)the Fundamental Research Funds for the Central Universities(FRFTP-16-019A3)
文摘（2,3-Dimethylbutyl）（2,4,40-trimethylpentyl）phosphinic acid（INET-3） was impregnated onto dry macroporous resins XAD-16 and pretreated XAD-16 with ethyl alcohol and HCl（Pre-XAD-16） to prepare the solvent impregnated resins SIRs-INET-3/XAD-16 and SIRs-INET-3/Pre-XAD-16. The molecular weight distribution of the low molecular weight（LMW） polymers washed off by ethyl alcohol during XAD-16 pretreatment was determined by gel permeation chromatography（GPC）. The macroporous resins（XAD-16 ＆ Pre-XAD-16）, the corresponding solvent impregnated resins（SIRs-INET-3/XAD-16 ＆SIRs-INET-3/Pre-XAD-16） and the PVA coated SIRs-INET-3/Pre-XAD-16 with boric acid as cross-linking agent were characterized by FT-IR, SEM-EDS and TGA. The effects of XAD-16 pretreatment and PVA coating technology on RE（III） adsorption equilibrium time, INET-3 losses during extraction and adsorption capacity were investigated. The adsorption kinetics, selectivity and stripping behaviors of SIRs-INET-3/XAD-16 were further studied. The washed off LMW polymers had the Mn of 36,656, Mw of 40,310 and polydispersity coefficient of 1.10. The SIRs-INET-3/XAD-16 had shorter equilibrium time,less INET-3 loss and more Tm（III） adsorption capacity than the SIRs-INET-3/Pre-XAD-16. The PVA coated SIRs-INET-3/Pre-XAD-16 had less INET-3 loss and more Tm（III） adsorption capacity but longer equilibrium time than the uncoated SIRs-INET-3/Pre-XAD-16. The adsorption of RE（III） on the SIRsINET-3/XAD-16 followed the pseudo-second-order kinetic model. The Tm（III） accumulative adsorption amounts onto SIRs-INET-3/XAD-16 after eight extraction stages was 23.6 mg/g. The separation factors of adjacent heavy RE（III） β（Er/Ho）, β（Tm/Er）, β（Yb/Tm） and β（Lu/Yb） values were 1.76, 2.59, 2.56 and 1.19,respectively. The adsorbed Lu（III） onto the SIRs-INET-3/XAD-16 can be stripped completely by 1.0 mol/L H2SO4.
基金Supported by the National Natural Science Foundation of China(50890184)the National Basic Research Program of China(2010CB227304)
文摘In absorption cycles,ionic liquid(IL)1,3-dimethylimidazolium tetrafluoroborate([Dmim]BF4)may be a promising absorbent of working pair using water as refrigerant.The vapor pressures of[Dmim]BF4 aqueous solution were measured with the boiling-point method in the temperature range from 312.25 to 403.60 K and in the mass concentration range of 65%to 90%of[Dmim]BF4.The experimental data were correlated with an Antoine-type equation and the Non-Random Two-Liquid(NRTL)model,and the average absolute deviations between the experimental and calculated values were 1.06%and 1.15%,respectively.For the[Dmim]BF4 aqueous solution,the experimental vapor pressures show negative deviations from the calculated data with Raoult's law.For higher mass concentration of the IL,the deviation is more negative.In addition,the vapor pressures,the hydrophilicity and the solubility of[Dmim]BF4 aqueous solutions were compared with those of[Dmim]Cl aqueous solutions and [Bmim]BF4 aqueous solutions at IL-mole fraction of 0.20.
基金Funded by the Major Science and Technology Program for Water Pollution Control and Treatment(No.2013ZX07202-010)
文摘Carbon-coated Fe3O4（ Fe3O4/C） microspheres activated with 1-ethyl-3-（3-dimethylaminopropyl）-carbodiimide hydrochloride（EDC） were prepared, characterized and applied to adsorb bovine serum albumin（BSA）. The prepared magnetic microspheres had spherical core-shell structure with a uniform and continuous carbon coating coupled with activation by EDC, and possessed superparamagnetic characteristics. The experimental results showed that the adsorption amount of BSA on the EDC-activated Fe3O4/C（Fe3O4/C-EDC） microspheres was higher than that on the Fe3O4/C microspheres. The maximum adsorption of BSA on Fe3O4/C-EDC microspheres occurred at pH 4.7, which was the isoelectric point of BSA. At low concentrations（below 1.0 M）, salt had no noticeable effect on BSA adsorption. The BSA adsorption of Fe3O4/C-EDC microspheres had a better fit to the Langmuir model than the Freundlich isotherm and Temkin isotherm model, and the kinetic data were well described by the pseudo-second-order model. The adsorption equilibrium could be reached within 20 min. High desorption efficiency（97.6%） of BSA from Fe3O4/C-EDC microspheres was obtained with 0.5 M Na2HPO4（pH 9.4） as the desorbent.
基金the Foundation of the Youth (OH060099) of China University of Mining and Technologythe Foundation of Natural Science Foundation (06AXL010) of Xuzhou Normal UniversityNatural Science Foundation (04KJB150139) of Education Committee of Jiangsu Province
文摘The title compound 7-amino-2,3,4,5-tetrahydro-1,3-dimethyl-5-（2-nitrophenyl）- 2,4- dioxo-1H-pyrano[2,3-d] pyrirnidine-6-carbonitrile DMF solvate 1 （C19H20N6O6, Mr = 428.41） was synthesized and crystallized. The crystal belongs to the monoclinic system, space group P2 1/c with a = 11.383（2）, b = 13.372（2）, c = 13.673（2）A, β = 97.380（4）°, Z = 4, V = 2063.8（6）A^3, Dc = 1.379 g/cm^3,μ（MoKα） = 0.105 mm^-1, F（000） = 896, the final R = 0.0738 and wR = 0.1647 for 2964 observed reflections （I〉 2σ（I））. X-ray analysis reveals that the new pyran ring is coplanar, which is obviously different from those of other similar compounds. In addition, the unclassical hydrogen bonds of C-H…O and C-H…N are presented in the crystals except for the normal hydrogen bonds of N-H…O.
文摘The solid-liquid equilibria of musk ketone + musk xylene, musk xylene +l,3-dimethyl-2,4-dinitro-5-tert-butyl benzene are measured by differential scanning calorimeter (DSC), these systems are proved to be simple eutectics. Moreover the melting points and the fusion enthalpies of musk ketone, musk xylene and 1,3-dimethyl-2,4-dinitro-5-tert-butyl benzene are also measured by the DSC. These solid-liquid equilibrium data and the heats of fusion are reported for the first time. Then UNIFAC model is used to correlate the sofid-liquid equilibrium data. It is shown that the solid-liquid equilibria of musk systems can be predicted by the UNIFAC model.
文摘The formaidehyde-free finishing agent 4,5-di-hydroxy-1,3-dimethy1-2-imidazolidinone(DMeDHEU)was prepared by the reaction of 1,3-dimethylurea and glyoxal.The reaction rate and equilib-rium conversion in relation to pH value,molar ratio,temperature and catalyst were studied.The conversionto DMeDHEU,catalyzed with citric acid/anhydrousNaAc,reached 95% in 6 hours at 40℃, pH 5.5 andmolar ratio 1.2.
基金ACKNOWLEDGMENTS This work was supported by the National Natural Science Foundation of China （No.21033002 and No.21202032） and the National Basic Research Program of China （No.2013CB834604）.
文摘The photophysics of 3-dimethylamino-2-methyl-propenal （DMAMP） after excitation to the S2 （ππ^＊） electronic state was studied using the resonance Raman spectroscopy and complete active space self-consistent field method calculations. The transition barriers of the ground state tautomerization reactions between DMAMP and its three isomers were determined at B3LYP/6-311＋＋G（d,p） level of theory. The vibrational spectra were assigned. The A- band resonance Raman spectra were obtained in acetonitrile with excitation wavelengths in resonance with the first intense absorption band to probe the structural dynamics of DMAMP. The B3LYP-TD computation was carried out to determine the relative A-band resonance Raman intensities of the fundamental modes, and the result indicated that the vibronic-coupling existed in Franck-Condon region. Complete active space self-consistent field （CASSCF） calculations were carried out to determine the excitation energies of the lower-lying singlet and triplet excited states, the conical intersection points and the intersystem crossing points. The A-band short-time structural dynamics and the corresponding decay dynamics of DMAMP were obtained by analysis of the resonance Raman intensity pattern and CASSCF computations. It was found that a sudden de-conjugation between C1=O6 and C2=C3 occurred at the Franck-Condon region of the S2（ππ^＊） state, while the enhancement of the conjugation interaction between C3 and N（CH3）2, and between C1 and C2 evolutions shortly after the wavepacket leaves away the Pranck-Condon region via the excited state charge redistribution. The de-conjugation interaction between C1=O6 and C2=C3 made the rotation of C3=N（CH3）2 group around the C2-C3 bond much easier, while the enhanced conjugation between C1 and C2, and between C3 and N（CH3）2 made the rotation around the C1-C2 bond and C3-N5 more difficult. It was revealed that the initial structural dynamics of DMAMP was predominantly towards the CI-I（S2/S0） point, while the opportunities towards either CI-2（S2/S0） or CI-3（S2/S0） point were negligible. Two decay channels of DMAMP from S2,FC（ππ^＊） to So or Tl,min via various CIs and ISCs were proposed.
