The unsaturated quaternary ammonium salt diethyldiallylammonium chloride(DEDAAC) was synthesized in a two-step synthetic method. The influences of the adding method of raw materials and temperature on the yields of di...The unsaturated quaternary ammonium salt diethyldiallylammonium chloride(DEDAAC) was synthesized in a two-step synthetic method. The influences of the adding method of raw materials and temperature on the yields of diethylallylamine (DEAA), and drying and temperature on the synthesis of DEDAAC were investigated. The content of in-process product DEAA was determined by non-aqueous titration. The structure of product DEDAAC was identified with IR, 1 H NMR and elemental analysis. The results show that adding allyl chloride and sodium hydroxide alternately can increase the yield of DEAA and decrease by-products. In further synthesizing of DEDAAC from DEAA, the step of drying DEAA is very necessary. When DEAA is dried by solid sodium hydroxide, good columnar crystals with a high purity(mp 199.5-201.0 ℃) are obtained; when DEAA is undried or the content of water in DEAA is above 20%, only platelets with bad quality are obtained even without crystals. The suitable synthesis conditions for DEAA and DEDAAC are 35 ℃, 6 h and 40 ℃, 36 h, respectively, and their yields are 69.7% and 67.3%, respectively.展开更多
The hydrogen-bonded organic framework(PFC-32),constructed by tetrahydroxyquinone(THQN)and diethylamine(DEA),was readily prepared via hydrothermal synthesis in DEF(N,N-diethylformamide).PFC-32 was characterized by PXRD...The hydrogen-bonded organic framework(PFC-32),constructed by tetrahydroxyquinone(THQN)and diethylamine(DEA),was readily prepared via hydrothermal synthesis in DEF(N,N-diethylformamide).PFC-32 was characterized by PXRD,IR,UV-Vis,TGA and photoluminescence(PL).Single crystal analysis reveals that PFC-32 shows a three-dimensional(3 D)framework,where the THQN anions are coplanar and separated by DEA cations.PFC-32 displays intrinsic photoluminescence property owing to the alleviation of the aggregation-caused quenching(ACQ)effect caused byπ-πstacking.展开更多
The phase of AlPO-21 was hydrothermally synthesized in the reactant system of diethylamine-RB-Al_2O_3-P_2O_5-H_2O-C_2H_5OH. The crystals of AlPO-21 growing in this system crystallizes in monoclinic system,space group ...The phase of AlPO-21 was hydrothermally synthesized in the reactant system of diethylamine-RB-Al_2O_3-P_2O_5-H_2O-C_2H_5OH. The crystals of AlPO-21 growing in this system crystallizes in monoclinic system,space group P2_1/n with a=0.8542(4) nm,b=1.7635(8) nm,c=0.9082(4) nm,β=108.234(5)°,V=1.2993(10) nm 3,Z=4,and the formula is [C_4H_ 10 NH_2] +~[Al_3P_3O_ 12 (OH)] -. The structure is resolved by the direct method and refined to R_1=0.0767 and wR_2=0.1627 based on 1719 observed reflections with I>2.0σ(I). An asymmetric unit consists of three PO_4 tetrahedra,one AlO_4 tetrahedron and two AlO_5 trigonal bipyramids. The framework is composed of 3-D uniform channels along [100],[001] and [101] with eight-membered oxygen ring windows. The powder sample of the MS was investigated with powder XRD,TG/DTG/DTA and the adsorption of water,methanol,n-hexane,ethylene,and ethane. The specific property for sieving molecules was observed on the adsorption isotherms,and proves the result of the single crystal structural analysis.展开更多
The kinetics of SN2 reaction between phenacyl bromide and various amines in 12 different solvents were studied. Solvent effects on the rate of this reaction and free energy of activation, ΔG#, were interpreted by app...The kinetics of SN2 reaction between phenacyl bromide and various amines in 12 different solvents were studied. Solvent effects on the rate of this reaction and free energy of activation, ΔG#, were interpreted by applying the Abraham-Kamlet-Taft (AKT) equation. The solvent polarity (π1*), solvent hydrogen-bond basicity (β1) and Hildebrand cohesive density energy (δ2H) are those parameters which increase the rate constant and decrease ΔG#, while solvent hydrogen-bond acidity (α1) will have the compensatory effect. A comparison among obtained values of second rate constants, k2 for different amines in a given solvent indicates that the amine reactivities are highly dependent on their structures. The consequent decrease of the rate constant for different amines in any given solvent was found to be: primary > secondary > tertiary. This order results from steric effects of amines.展开更多
文摘The unsaturated quaternary ammonium salt diethyldiallylammonium chloride(DEDAAC) was synthesized in a two-step synthetic method. The influences of the adding method of raw materials and temperature on the yields of diethylallylamine (DEAA), and drying and temperature on the synthesis of DEDAAC were investigated. The content of in-process product DEAA was determined by non-aqueous titration. The structure of product DEDAAC was identified with IR, 1 H NMR and elemental analysis. The results show that adding allyl chloride and sodium hydroxide alternately can increase the yield of DEAA and decrease by-products. In further synthesizing of DEDAAC from DEAA, the step of drying DEAA is very necessary. When DEAA is dried by solid sodium hydroxide, good columnar crystals with a high purity(mp 199.5-201.0 ℃) are obtained; when DEAA is undried or the content of water in DEAA is above 20%, only platelets with bad quality are obtained even without crystals. The suitable synthesis conditions for DEAA and DEDAAC are 35 ℃, 6 h and 40 ℃, 36 h, respectively, and their yields are 69.7% and 67.3%, respectively.
基金Supported by Fujian Young and Middle-aged Teachers’Educational Research Project(No.JT180842)。
文摘The hydrogen-bonded organic framework(PFC-32),constructed by tetrahydroxyquinone(THQN)and diethylamine(DEA),was readily prepared via hydrothermal synthesis in DEF(N,N-diethylformamide).PFC-32 was characterized by PXRD,IR,UV-Vis,TGA and photoluminescence(PL).Single crystal analysis reveals that PFC-32 shows a three-dimensional(3 D)framework,where the THQN anions are coplanar and separated by DEA cations.PFC-32 displays intrinsic photoluminescence property owing to the alleviation of the aggregation-caused quenching(ACQ)effect caused byπ-πstacking.
基金ProjectsupportedbytheNationalNaturalScienceFoundationofChina (No .2 0 0 73 0 10 )
文摘The phase of AlPO-21 was hydrothermally synthesized in the reactant system of diethylamine-RB-Al_2O_3-P_2O_5-H_2O-C_2H_5OH. The crystals of AlPO-21 growing in this system crystallizes in monoclinic system,space group P2_1/n with a=0.8542(4) nm,b=1.7635(8) nm,c=0.9082(4) nm,β=108.234(5)°,V=1.2993(10) nm 3,Z=4,and the formula is [C_4H_ 10 NH_2] +~[Al_3P_3O_ 12 (OH)] -. The structure is resolved by the direct method and refined to R_1=0.0767 and wR_2=0.1627 based on 1719 observed reflections with I>2.0σ(I). An asymmetric unit consists of three PO_4 tetrahedra,one AlO_4 tetrahedron and two AlO_5 trigonal bipyramids. The framework is composed of 3-D uniform channels along [100],[001] and [101] with eight-membered oxygen ring windows. The powder sample of the MS was investigated with powder XRD,TG/DTG/DTA and the adsorption of water,methanol,n-hexane,ethylene,and ethane. The specific property for sieving molecules was observed on the adsorption isotherms,and proves the result of the single crystal structural analysis.
文摘The kinetics of SN2 reaction between phenacyl bromide and various amines in 12 different solvents were studied. Solvent effects on the rate of this reaction and free energy of activation, ΔG#, were interpreted by applying the Abraham-Kamlet-Taft (AKT) equation. The solvent polarity (π1*), solvent hydrogen-bond basicity (β1) and Hildebrand cohesive density energy (δ2H) are those parameters which increase the rate constant and decrease ΔG#, while solvent hydrogen-bond acidity (α1) will have the compensatory effect. A comparison among obtained values of second rate constants, k2 for different amines in a given solvent indicates that the amine reactivities are highly dependent on their structures. The consequent decrease of the rate constant for different amines in any given solvent was found to be: primary > secondary > tertiary. This order results from steric effects of amines.