Nervonic acid is the world’s first and only potent substance that can repair damaged nerve fibers and promote nerve cell regeneration with high nutritional value.The wide variety of fatty acids in plant oils and fats...Nervonic acid is the world’s first and only potent substance that can repair damaged nerve fibers and promote nerve cell regeneration with high nutritional value.The wide variety of fatty acids in plant oils and fats with similar structures makes the large-scale separation and purification of high-purity nervonic acid very difficult.A new combined process of molecular distillation,urea inclusion and solvent crystallization was established to prepare high-purity nervonic acid with the mixed fatty acids obtained after saponification and acidification of Acer truncatum Bunge oil as raw materials.First,according to the difference in the mean free path of fatty acids,molecular distillation was used to separate and remove C16 saturated fatty acid of palmitic acid and four C18-C20 fatty acids of stearic,oleic,linoleic,and linolenic acids.The content of C16-C20 fatty acids decreased from 72.92% to 19.22% after two-stage molecular distillation processes,in which the contents of saturated fatty acid of palmitic acid decreased to about 0.5%.Then,according to the difference in carbon chain length and saturation of fatty acid,the contents of C22-C24 saturated fatty acids of tetracosanoic and docosanoic acids decreased to 0.21% and 0.07% by urea inclusion with urea/free fatty acid preparation by saponification(SPOMFs)ratio as 0.6.In addition,all saturated fatty acids were basically separated.Finally,according to the difference in the solubility of fatty acids in solvents,the C18-C20 unsaturated fatty acids of oleic,linoleic,and linolenic acids and C22 unsaturated fatty acid of erucic acid were removed by solvent crystallization.The content of C18-C20 unsaturated fatty acids decreased to less than 5% with pentanol as the solvent after the first stage solvent crystallization.The content of erucic acid decreased to 3.47% with anhydrous ethanol as the solvent after the second to fifth stage solvent crystallization.The combined process of molecular distillation,urea inclusion and low temperature crystallization innovatively adopted an efficient,simple and easy-toindustrial solvent crystallization method to separate erucic and nervonic acids,obtaining nervonic acid with purity of 96.53% and final yield of 47.99%.展开更多
To identify the effect of solvents and anthracene on the purification of carbazole,the solvent crystallization of carbazole was investigated with xylene,chlorobenzene and tetrachloroethylene(TCE)as solvents under two ...To identify the effect of solvents and anthracene on the purification of carbazole,the solvent crystallization of carbazole was investigated with xylene,chlorobenzene and tetrachloroethylene(TCE)as solvents under two forced circulation cooling(FCC)modes.The co-crystalline experimental data were obtained from runs carried out at different anthracene levels between 1%(mass)and 10%(mass).The results showed that a uniform flake carbazole crystal obtained when using xylene and chlorobenzene under the FCC-1 mode with gradual cooling rate.Nevertheless,fine flake crystals grown under shock cooling of FCC-2 mode.It is beneficial to improving the purity of carbazole with chlorobenzene as solvent under cooling mode of FCC-1.Anthracene could promote the growth of carbazole in solution,and it has a significant influence on the purification of carbazole.展开更多
Palm fatty acid distillate （PFAD）, a by-product of deodorization in palm oil refining, contains about 0.7%-1% vitamin E. The advantage of PFAD over other vitamin E sources is higher amount of tocotrienols than that ...Palm fatty acid distillate （PFAD）, a by-product of deodorization in palm oil refining, contains about 0.7%-1% vitamin E. The advantage of PFAD over other vitamin E sources is higher amount of tocotrienols than that of tocopherols. Vitamin E purification of unsaponiable matter of PFAD was aimed to remove other impurities to obtain high vitamin E concentration, mainly tocotrienols. This research used low temperature solvent crystallization to purify vitamin E. To optimize response of vitamin concentration, a response surface method was applied with three factors, i.e., the ratio between solvent and unsaponifiable matter （A）, crystallization temperature （B）, and crystallization time （C）. The relation of three factors was quadratic with equation Y = -128.54361 ＋ 41.33904A - 0.87995B ＋ 1.58941C ＋ 0.00290AB - 0.044324AC ＋ 0.00120BC - 3.33113A2 - 0.039535B2 - 0.02710C2. The optimum crystallization condition was obtained at ratio of solventto unsaponifiable matter of 6.04：1, crystallization temperature of-10.54 ℃, and crystallization time of 24.16 hours. Vitamin E enriched fraction from optimum crystallization conditions contained vitamin E of 20.13% （w/w）.展开更多
In this work,the stable layer structure of serpentine,which seriously restricts the extraction of magnesium,was broken down,and a nearly 94%leaching efficiency of Mg was obtained by adding 5%fluorite powder.Compared w...In this work,the stable layer structure of serpentine,which seriously restricts the extraction of magnesium,was broken down,and a nearly 94%leaching efficiency of Mg was obtained by adding 5%fluorite powder.Compared with the system without fluorite,the Mg leaching efficiency increased by 36.42%.This result was achieved because the complexation of fluorinion(F)with Si in serpentine promoted a distorted tetrahedral orientation,which led to a loose crystal structure of serpentine and contributed to exposing more Mg for a remarkable increase in Mg recovery.It is suggested that fluorite powder could replace expensive assisted reagents in the leaching process,which would markedly decreased the cost.Moreover,an energy-efficient‘‘solvent displacement crystallization”(SDC)method was employed to efficiently recover magnesium(99.04%)from pregnant solutions.At the same time,the reuse of fluorinecontaining solutions was explored.展开更多
The size and weight fraction of crystals of pure ice or dimethylsulfoxide (DMSO) in poly(vinyl alcohol) (PVA) gel prepared from a mixed solvent of DMSO/water were determined from melting peaks observed by differential...The size and weight fraction of crystals of pure ice or dimethylsulfoxide (DMSO) in poly(vinyl alcohol) (PVA) gel prepared from a mixed solvent of DMSO/water were determined from melting peaks observed by differential scanning calorimetry (DSC). The depression of the melting point with respect to the equilibrium melting point and the melting enthalpy gave the crystal size and weight fraction, respectively. The sizes were in the range of a few nm to tens of nm, depending on the composition ratio of the mixed solvent (DMSO/water) and the polymer concentration. Based on the weight fraction, the critical condition at which the whole solvent became non-freezable was estimated, and it was found to depend on both the PVA concentration and the DMSO/water ratio. When the solvent was pure water, the critical PVA concentration was as high as 86.4 wt%, while for pure DMSO solvent it was 50.1 wt%.展开更多
The metal-organic framework（MOF）{[Cu（L1）_（0.5）（CN）]·4H_2O·3DMSO}_n（1） was assembled by 1,4-bis（3？,5？-dicyano-2？,6？-di（pyrid-4-yl）-1？,4？-dihydropyridyl）benzene（L1） together with copper c...The metal-organic framework（MOF）{[Cu（L1）_（0.5）（CN）]·4H_2O·3DMSO}_n（1） was assembled by 1,4-bis（3？,5？-dicyano-2？,6？-di（pyrid-4-yl）-1？,4？-dihydropyridyl）benzene（L1） together with copper cyanide at room temperature. In 1,the Cu~＋ ions are linked by CN-anions into a 1D helical chain,which is further fused together by tetradentate L1 ligands to build an extended 3D porous framework with two different types of functionalized channels. 1 crystallizes in the monoclinic,space group P21/c with a = 17.8729（6）,b = 8.7298（3）,c = 22.7524（9） ？,β = 96.072（4）o,V = 3530.1（2） ？~3,μ = 0.845 mm-1,Dc = 1.352 Mg/m^3,Z = 4,Mr = 718.35,F（000） = 1500,S = 1.081,the final R = 0.0877 and wR = 0.2275 for 6975 observed reflections with I 〉 2σ（I）.展开更多
A novel and efficient methodology for obtaining highly active photocatalyst of bi phase TiO 2 with small particle size and high specific surface area was developed by solvent evaporation induced crystallization (SE...A novel and efficient methodology for obtaining highly active photocatalyst of bi phase TiO 2 with small particle size and high specific surface area was developed by solvent evaporation induced crystallization (SEIC) method at low temperature. The prepared TiO 2 powder was characterized with X ray diffraction (XRD), transmission electron microscopy (TEM) and BET surface areas. The photocatalytic activity was evaluated by the photocatalytic oxidation of acetone in air. The results showed that the photocatalytic activity of the TiO 2 powder prepared by this method approached that of Degussa P25. This may be attributed to the fact that the prepared TiO 2 powder had larger specific surface areas (265 m 2·g -1 ) and smaller crystallite size (about 5 nm), but relatively low crystallinity, as compared with Degussa P25.展开更多
Measuring the Hamiltonian of dipolar coupled spin systems is usually a difficult task due to the high complexity of their spectra. Currently, molecules with unknown geometrical structure and low symmetry are extremely...Measuring the Hamiltonian of dipolar coupled spin systems is usually a difficult task due to the high complexity of their spectra. Currently, molecules with unknown geometrical structure and low symmetry are extremely tedious or impossible to analyze by sheer spectral fitting. We present a novel method that addresses the problem of spectral analysis and report experimental results of extracting, by spectral fitting, the parameters of an oriented 6-spin system with very low symmetry in structure, without using apriori knowledge or assumptions on the molecular geometry or order parameters. The advantages of our method are achieved with the use of a new spectral analysis algorithm non-assigned frequency optimization of NMR spectra （NAFONS） and by the use of simplified spectra obtained by transition selective pulses. This new method goes beyond the limit of spectral analysis for dipolar coupled spin systems and is helpful for related fields, such as quantum computation and molecular structure analysis.展开更多
ZSM-22 （TON） zeolite crystal morphology was successfully controlled using a microwave-assisted solvothermal fabrication method. Different co-solvents, including ethanol, 2-propanol, glycerol, and ethylene glycol, we...ZSM-22 （TON） zeolite crystal morphology was successfully controlled using a microwave-assisted solvothermal fabrication method. Different co-solvents, including ethanol, 2-propanol, glycerol, and ethylene glycol, were also applied in the synthesis mixture. The effects of various parameters such as the aging time, the type and amount of co-solvent on the ZSM-22 crystal aspect ratio were investigated. When employing this microwave irradiation synthesis, a long aging time was crucial to obtain smaller and more uniform crystal sizes. The addition of co-solvent resulted in elongated ZSM-22 crystals, regard- less of the actual co-solvent used, although ZSM-22 zeolite crystallinity was sensitive to the co-solvent type. In general, the use of a co-solvent stimulated the appearance of ZSM-5 zeolite as an impurity and the amount of this impurity was proportional to the concentration of co-solvent in the synthesis mixture.展开更多
基金supported by the National Natural Science Foundation of China(22125802 and 22078010)Beijing Natural Science Foundation(2222017)Big Science Project from BUCT(XK180301).
文摘Nervonic acid is the world’s first and only potent substance that can repair damaged nerve fibers and promote nerve cell regeneration with high nutritional value.The wide variety of fatty acids in plant oils and fats with similar structures makes the large-scale separation and purification of high-purity nervonic acid very difficult.A new combined process of molecular distillation,urea inclusion and solvent crystallization was established to prepare high-purity nervonic acid with the mixed fatty acids obtained after saponification and acidification of Acer truncatum Bunge oil as raw materials.First,according to the difference in the mean free path of fatty acids,molecular distillation was used to separate and remove C16 saturated fatty acid of palmitic acid and four C18-C20 fatty acids of stearic,oleic,linoleic,and linolenic acids.The content of C16-C20 fatty acids decreased from 72.92% to 19.22% after two-stage molecular distillation processes,in which the contents of saturated fatty acid of palmitic acid decreased to about 0.5%.Then,according to the difference in carbon chain length and saturation of fatty acid,the contents of C22-C24 saturated fatty acids of tetracosanoic and docosanoic acids decreased to 0.21% and 0.07% by urea inclusion with urea/free fatty acid preparation by saponification(SPOMFs)ratio as 0.6.In addition,all saturated fatty acids were basically separated.Finally,according to the difference in the solubility of fatty acids in solvents,the C18-C20 unsaturated fatty acids of oleic,linoleic,and linolenic acids and C22 unsaturated fatty acid of erucic acid were removed by solvent crystallization.The content of C18-C20 unsaturated fatty acids decreased to less than 5% with pentanol as the solvent after the first stage solvent crystallization.The content of erucic acid decreased to 3.47% with anhydrous ethanol as the solvent after the second to fifth stage solvent crystallization.The combined process of molecular distillation,urea inclusion and low temperature crystallization innovatively adopted an efficient,simple and easy-toindustrial solvent crystallization method to separate erucic and nervonic acids,obtaining nervonic acid with purity of 96.53% and final yield of 47.99%.
基金supported by the National Natural Science Foundation of China(21776192,22038008)。
文摘To identify the effect of solvents and anthracene on the purification of carbazole,the solvent crystallization of carbazole was investigated with xylene,chlorobenzene and tetrachloroethylene(TCE)as solvents under two forced circulation cooling(FCC)modes.The co-crystalline experimental data were obtained from runs carried out at different anthracene levels between 1%(mass)and 10%(mass).The results showed that a uniform flake carbazole crystal obtained when using xylene and chlorobenzene under the FCC-1 mode with gradual cooling rate.Nevertheless,fine flake crystals grown under shock cooling of FCC-2 mode.It is beneficial to improving the purity of carbazole with chlorobenzene as solvent under cooling mode of FCC-1.Anthracene could promote the growth of carbazole in solution,and it has a significant influence on the purification of carbazole.
文摘Palm fatty acid distillate （PFAD）, a by-product of deodorization in palm oil refining, contains about 0.7%-1% vitamin E. The advantage of PFAD over other vitamin E sources is higher amount of tocotrienols than that of tocopherols. Vitamin E purification of unsaponiable matter of PFAD was aimed to remove other impurities to obtain high vitamin E concentration, mainly tocotrienols. This research used low temperature solvent crystallization to purify vitamin E. To optimize response of vitamin concentration, a response surface method was applied with three factors, i.e., the ratio between solvent and unsaponifiable matter （A）, crystallization temperature （B）, and crystallization time （C）. The relation of three factors was quadratic with equation Y = -128.54361 ＋ 41.33904A - 0.87995B ＋ 1.58941C ＋ 0.00290AB - 0.044324AC ＋ 0.00120BC - 3.33113A2 - 0.039535B2 - 0.02710C2. The optimum crystallization condition was obtained at ratio of solventto unsaponifiable matter of 6.04：1, crystallization temperature of-10.54 ℃, and crystallization time of 24.16 hours. Vitamin E enriched fraction from optimum crystallization conditions contained vitamin E of 20.13% （w/w）.
基金The authors gratefully thank the Fundamental Research Funds for the Central Universities(N2001018)Liaoning Revitaliza-tion Talents Program(XLYC1807089)for financial support。
文摘In this work,the stable layer structure of serpentine,which seriously restricts the extraction of magnesium,was broken down,and a nearly 94%leaching efficiency of Mg was obtained by adding 5%fluorite powder.Compared with the system without fluorite,the Mg leaching efficiency increased by 36.42%.This result was achieved because the complexation of fluorinion(F)with Si in serpentine promoted a distorted tetrahedral orientation,which led to a loose crystal structure of serpentine and contributed to exposing more Mg for a remarkable increase in Mg recovery.It is suggested that fluorite powder could replace expensive assisted reagents in the leaching process,which would markedly decreased the cost.Moreover,an energy-efficient‘‘solvent displacement crystallization”(SDC)method was employed to efficiently recover magnesium(99.04%)from pregnant solutions.At the same time,the reuse of fluorinecontaining solutions was explored.
文摘The size and weight fraction of crystals of pure ice or dimethylsulfoxide (DMSO) in poly(vinyl alcohol) (PVA) gel prepared from a mixed solvent of DMSO/water were determined from melting peaks observed by differential scanning calorimetry (DSC). The depression of the melting point with respect to the equilibrium melting point and the melting enthalpy gave the crystal size and weight fraction, respectively. The sizes were in the range of a few nm to tens of nm, depending on the composition ratio of the mixed solvent (DMSO/water) and the polymer concentration. Based on the weight fraction, the critical condition at which the whole solvent became non-freezable was estimated, and it was found to depend on both the PVA concentration and the DMSO/water ratio. When the solvent was pure water, the critical PVA concentration was as high as 86.4 wt%, while for pure DMSO solvent it was 50.1 wt%.
基金supported by the Natural Science Foundation of Fujian Province(2012J06006,2014J05026,2006L2005)
文摘The metal-organic framework（MOF）{[Cu（L1）_（0.5）（CN）]·4H_2O·3DMSO}_n（1） was assembled by 1,4-bis（3？,5？-dicyano-2？,6？-di（pyrid-4-yl）-1？,4？-dihydropyridyl）benzene（L1） together with copper cyanide at room temperature. In 1,the Cu~＋ ions are linked by CN-anions into a 1D helical chain,which is further fused together by tetradentate L1 ligands to build an extended 3D porous framework with two different types of functionalized channels. 1 crystallizes in the monoclinic,space group P21/c with a = 17.8729（6）,b = 8.7298（3）,c = 22.7524（9） ？,β = 96.072（4）o,V = 3530.1（2） ？~3,μ = 0.845 mm-1,Dc = 1.352 Mg/m^3,Z = 4,Mr = 718.35,F（000） = 1500,S = 1.081,the final R = 0.0877 and wR = 0.2275 for 6975 observed reflections with I 〉 2σ（I）.
基金theNationalNaturalScienceFoundationofChina (No .5 0 2 72 0 49)
文摘A novel and efficient methodology for obtaining highly active photocatalyst of bi phase TiO 2 with small particle size and high specific surface area was developed by solvent evaporation induced crystallization (SEIC) method at low temperature. The prepared TiO 2 powder was characterized with X ray diffraction (XRD), transmission electron microscopy (TEM) and BET surface areas. The photocatalytic activity was evaluated by the photocatalytic oxidation of acetone in air. The results showed that the photocatalytic activity of the TiO 2 powder prepared by this method approached that of Degussa P25. This may be attributed to the fact that the prepared TiO 2 powder had larger specific surface areas (265 m 2·g -1 ) and smaller crystallite size (about 5 nm), but relatively low crystallinity, as compared with Degussa P25.
文摘Measuring the Hamiltonian of dipolar coupled spin systems is usually a difficult task due to the high complexity of their spectra. Currently, molecules with unknown geometrical structure and low symmetry are extremely tedious or impossible to analyze by sheer spectral fitting. We present a novel method that addresses the problem of spectral analysis and report experimental results of extracting, by spectral fitting, the parameters of an oriented 6-spin system with very low symmetry in structure, without using apriori knowledge or assumptions on the molecular geometry or order parameters. The advantages of our method are achieved with the use of a new spectral analysis algorithm non-assigned frequency optimization of NMR spectra （NAFONS） and by the use of simplified spectra obtained by transition selective pulses. This new method goes beyond the limit of spectral analysis for dipolar coupled spin systems and is helpful for related fields, such as quantum computation and molecular structure analysis.
文摘ZSM-22 （TON） zeolite crystal morphology was successfully controlled using a microwave-assisted solvothermal fabrication method. Different co-solvents, including ethanol, 2-propanol, glycerol, and ethylene glycol, were also applied in the synthesis mixture. The effects of various parameters such as the aging time, the type and amount of co-solvent on the ZSM-22 crystal aspect ratio were investigated. When employing this microwave irradiation synthesis, a long aging time was crucial to obtain smaller and more uniform crystal sizes. The addition of co-solvent resulted in elongated ZSM-22 crystals, regard- less of the actual co-solvent used, although ZSM-22 zeolite crystallinity was sensitive to the co-solvent type. In general, the use of a co-solvent stimulated the appearance of ZSM-5 zeolite as an impurity and the amount of this impurity was proportional to the concentration of co-solvent in the synthesis mixture.
