A novel purification process is involved to obtain the high purity[>99%(by mass)]dodecanedioic acid(DC_(12)).It involves a re-crystallization followed by molecular distillation from the crude product.The objective ...A novel purification process is involved to obtain the high purity[>99%(by mass)]dodecanedioic acid(DC_(12)).It involves a re-crystallization followed by molecular distillation from the crude product.The objective of this study is to investigate general conditions,feed rate,distilling temperature and vacuum,necessary for centrifugal distillation of DC_(12).Under the optimum conditions,distilling temperature 180℃,pressure 30 Pa and feed flow rate700 ml·h^(-1),the purity of DC_(12) in the residence reached 97.55%with a yield of 53.18%by the analysis of gas chromatography.Multiple-pass distillation made a considerable contribution by improving the purity to99.22%.Additionally,the effect of pretreatment(re-crystallization) on distillation process was revealed through a series of comparative experiments.展开更多
It is difficult to treat 2-amino-thiazoline-4-carboxylic acid (ATC) waste liquid effectively at present for its characteristics of high chemical oxygen demand (COD), high salinity and low biodegradability. In orde...It is difficult to treat 2-amino-thiazoline-4-carboxylic acid (ATC) waste liquid effectively at present for its characteristics of high chemical oxygen demand (COD), high salinity and low biodegradability. In order to solve this problem, this paper presents several kinds of physical-chemical treatment unit techniques, including acid separation, catalytic oxidation and coagulation. First of all, acid separation was adopted to precipitate relevant organics at isoelectric point. When the temperature and pH value of acid separation were controlled at about 5 ℃ and 2.2 respectively, the COD removal rate could reach 27.600. Secondly, oxidation was used to break chemical constitution of refractory organics. The optimal reaction parameters of catalytic oxidation should be 20 ℃, pH adjusted to 5.0 and [Fe2+] 300 mg/L. Then with 500 H2O2 added and after one-hour reaction, the COD removal rate could achieve about 5200. Finally, coagulation was adopted to remove a portion of refractory organics, and 1500 polymeric molysite flocculant was the best for the coagulation, and the COD removal rate could reach about 1500. Therefore, the proposed feasible process of physical-chemical pretreatment for ATC waste liquid could have about 7000 COD removed in total.展开更多
Silica gel thin-layer plates covered with L-arginine and copper acetate were used for the separation of amino acid enantiomers, The chromatographic selectivity and the effects of plate different preparation methods, s...Silica gel thin-layer plates covered with L-arginine and copper acetate were used for the separation of amino acid enantiomers, The chromatographic selectivity and the effects of plate different preparation methods, sample molecular structure and solvent compositions on resolution performance were also discussed.展开更多
The extraction and separation of heavy rare earths(REs) using newly synthesized a-aminophosphonic acid extractant 2-ethylhexyl-3-(2-ethylhexylamino)pentan-3-yl phosphonic acid(HEHAPP, HA) in nheptane were invest...The extraction and separation of heavy rare earths(REs) using newly synthesized a-aminophosphonic acid extractant 2-ethylhexyl-3-(2-ethylhexylamino)pentan-3-yl phosphonic acid(HEHAPP, HA) in nheptane were investigated from chloride medium. The extraction stoichiometries of lanthanum, gadolinium, yttrium and lutetium are determined to be REA3 by the slope analysis method. The favorable separation factors of adjacent heavy REs(Ⅲ),i.e. β(Y/Ho), β(Er/Y),β(Tm/Er),β(Yb/Tm) and β(Lu/Yb), are determined to be1.87,1.36, 3.21,3.22 and 1.93, respectively, when extracted from a binary system at proper condition. The loading capacities of HA for Ho, Er, Yb and Lu increase in the order Ho 〈 Er 〈 Yb 〈 Lu with the values being 0.201, 0.205, 0.216 and 0.229 mol/L, respectively. So HA would be a potential extractant for the separation of heavy REs(Ⅲ). Among inorganic acids such as H2 SO4, HNO3 and HCl, HCl is tested to be the most effective stripping agent.展开更多
In order to study the aqueous stability of rare earth and thorium elements and the reaction mechanism of hydrochloric acid leaching of roasted bastnaesite,Eh-pH diagrams for La-,Nd-,Ce-,Th-(Cl)-(F)-H2 O systems at...In order to study the aqueous stability of rare earth and thorium elements and the reaction mechanism of hydrochloric acid leaching of roasted bastnaesite,Eh-pH diagrams for La-,Nd-,Ce-,Th-(Cl)-(F)-H2 O systems at 20 ℃ were depicted using HSC Chemistry 6.0 software. Eh-pH diagrams of La-, Ce-,Nd-and Th-Cl-H2 O systems show that trivalent rare earth would be leached into solution by adjusting the acidity of the leaching solution, while tetravalent cerium and thorium would be remained in the leaching residue. And in the case that the pH value of the leaching solution is lower than 2, tetravalent cerium would be partially reduced by chlorine ions(Cl^-), which is well agreed with the industrial production. It can be inferred from Eh-pH diagrams for the systems La-, Nd-,Ce-, Th-F-H2 O that the leached trivalent rare earth ions(RE^(3+)) and tetravalent thorium ions(Th^(4+)) are preferentially combined with fluorine ions(F) to form sediment during non-reductive acid leaching of roasted bastnaesite. However,when controlling the pH value of the leaching solution below 0, fluorine and tetravalent cerium in the roasted bastnaesite would be leached out in the form of soluble [CeF3]~+ complex. That means the precipitation of REF3 and ThF4·2.5 H2 O can be avoided in the leaching step. According to Eh-pH diagrams for the system Ce-F-Cl-H2 O, [CeF3]~+ in the leaching solution would be reduced to CeF3 precipitate in the presence of Cl^-, that is to say, tetravalent cerium and fluorine would be firstly leached out to form[CeF3]~+,which would then be reduced to CeF3 precipitate by Cl^-in the hydrochloric acid leaching process of roasted bastnaesite.展开更多
Solvothermal reaction of 3-aminoisonicotinic acid(Haina) and Cu(NO_3)_2·2.5H_2O gave a novel twodimensional(2D) microporous metal–organic framework, [Cu(aina)_2(DMF)]·DMF(1, DMF = N,N-dimethylfor...Solvothermal reaction of 3-aminoisonicotinic acid(Haina) and Cu(NO_3)_2·2.5H_2O gave a novel twodimensional(2D) microporous metal–organic framework, [Cu(aina)_2(DMF)]·DMF(1, DMF = N,N-dimethylformamide). Single-crystal X-ray crystallographic study of compound 1 revealed that Cu(II)ions are linked by ainaàligands forming square grid-like layers, which stack together via multiple hydrogen bonding interactions. The solvent-free framework of 1a displayed considerable porosity(void = 46.5%) with one-dimensional(1D) open channels(4.7 ? ? 4.8 ?) functionalized by amino groups.Gas sorption measurements of 1 revealed selective carbon dioxide(CO_2) and acetylene(C_2H_2) adsorption over methane(CH_4) and nitrogen(N_2) at ambient temperature.展开更多
Ionic liquids(ILs) immobilized on silica as novel high performance liquid chromatography(HPLC)stationary phases have attracted considerable attention. However, it has not been applied to protein separation. In thi...Ionic liquids(ILs) immobilized on silica as novel high performance liquid chromatography(HPLC)stationary phases have attracted considerable attention. However, it has not been applied to protein separation. In this paper, N-methylimidazolium IL-modified silica-based stationary phase(Silpr Mim)was prepared and investigated as a novel multi-interaction stationary phase charged positively for protein separation. The results indicate that all of the basic proteins tested cannot be absorbed on this novel stationary phase, whereas all of the acidic proteins tested can be retained, and the baseline separation of eight kinds of acidic protein standards can be achieved when performed in reversed phase/ion-exchange chromatography(RPLC/IEC) mode. Compared with commonly used commercial octadecylated silica(ODS) column, the novel stationary phase can show selectivity and good resolution to acidic proteins, which has a promising application in the separation and analyses of acidic proteins from the complex samples in proteomics. In addition, the chromatographic behavior of proteins, the effect of the ligand structure and the retention mechanism on this stationary phase were also investigated.展开更多
The strategy of expert system for high performance liquid chromatography was discussed, the attentions are mainly placed on the knowledge base for selection of column system, separation modes and detection modes in th...The strategy of expert system for high performance liquid chromatography was discussed, the attentions are mainly placed on the knowledge base for selection of column system, separation modes and detection modes in the analysis of amino acids, peptides and proteins.展开更多
文摘A novel purification process is involved to obtain the high purity[>99%(by mass)]dodecanedioic acid(DC_(12)).It involves a re-crystallization followed by molecular distillation from the crude product.The objective of this study is to investigate general conditions,feed rate,distilling temperature and vacuum,necessary for centrifugal distillation of DC_(12).Under the optimum conditions,distilling temperature 180℃,pressure 30 Pa and feed flow rate700 ml·h^(-1),the purity of DC_(12) in the residence reached 97.55%with a yield of 53.18%by the analysis of gas chromatography.Multiple-pass distillation made a considerable contribution by improving the purity to99.22%.Additionally,the effect of pretreatment(re-crystallization) on distillation process was revealed through a series of comparative experiments.
文摘It is difficult to treat 2-amino-thiazoline-4-carboxylic acid (ATC) waste liquid effectively at present for its characteristics of high chemical oxygen demand (COD), high salinity and low biodegradability. In order to solve this problem, this paper presents several kinds of physical-chemical treatment unit techniques, including acid separation, catalytic oxidation and coagulation. First of all, acid separation was adopted to precipitate relevant organics at isoelectric point. When the temperature and pH value of acid separation were controlled at about 5 ℃ and 2.2 respectively, the COD removal rate could reach 27.600. Secondly, oxidation was used to break chemical constitution of refractory organics. The optimal reaction parameters of catalytic oxidation should be 20 ℃, pH adjusted to 5.0 and [Fe2+] 300 mg/L. Then with 500 H2O2 added and after one-hour reaction, the COD removal rate could achieve about 5200. Finally, coagulation was adopted to remove a portion of refractory organics, and 1500 polymeric molysite flocculant was the best for the coagulation, and the COD removal rate could reach about 1500. Therefore, the proposed feasible process of physical-chemical pretreatment for ATC waste liquid could have about 7000 COD removed in total.
文摘Silica gel thin-layer plates covered with L-arginine and copper acetate were used for the separation of amino acid enantiomers, The chromatographic selectivity and the effects of plate different preparation methods, sample molecular structure and solvent compositions on resolution performance were also discussed.
基金Project supported by National Basic Research Program of China(973 program,2012CBA01206)the National Natural Science Foundation of China(21521092,51222404)the Strategic Priority Research Program of CAS(XDA02030100)
文摘The extraction and separation of heavy rare earths(REs) using newly synthesized a-aminophosphonic acid extractant 2-ethylhexyl-3-(2-ethylhexylamino)pentan-3-yl phosphonic acid(HEHAPP, HA) in nheptane were investigated from chloride medium. The extraction stoichiometries of lanthanum, gadolinium, yttrium and lutetium are determined to be REA3 by the slope analysis method. The favorable separation factors of adjacent heavy REs(Ⅲ),i.e. β(Y/Ho), β(Er/Y),β(Tm/Er),β(Yb/Tm) and β(Lu/Yb), are determined to be1.87,1.36, 3.21,3.22 and 1.93, respectively, when extracted from a binary system at proper condition. The loading capacities of HA for Ho, Er, Yb and Lu increase in the order Ho 〈 Er 〈 Yb 〈 Lu with the values being 0.201, 0.205, 0.216 and 0.229 mol/L, respectively. So HA would be a potential extractant for the separation of heavy REs(Ⅲ). Among inorganic acids such as H2 SO4, HNO3 and HCl, HCl is tested to be the most effective stripping agent.
基金Project supported by the National Natural Science Foundation of China(51404035)Beijing Nova program(Z161100004916108)
文摘In order to study the aqueous stability of rare earth and thorium elements and the reaction mechanism of hydrochloric acid leaching of roasted bastnaesite,Eh-pH diagrams for La-,Nd-,Ce-,Th-(Cl)-(F)-H2 O systems at 20 ℃ were depicted using HSC Chemistry 6.0 software. Eh-pH diagrams of La-, Ce-,Nd-and Th-Cl-H2 O systems show that trivalent rare earth would be leached into solution by adjusting the acidity of the leaching solution, while tetravalent cerium and thorium would be remained in the leaching residue. And in the case that the pH value of the leaching solution is lower than 2, tetravalent cerium would be partially reduced by chlorine ions(Cl^-), which is well agreed with the industrial production. It can be inferred from Eh-pH diagrams for the systems La-, Nd-,Ce-, Th-F-H2 O that the leached trivalent rare earth ions(RE^(3+)) and tetravalent thorium ions(Th^(4+)) are preferentially combined with fluorine ions(F) to form sediment during non-reductive acid leaching of roasted bastnaesite. However,when controlling the pH value of the leaching solution below 0, fluorine and tetravalent cerium in the roasted bastnaesite would be leached out in the form of soluble [CeF3]~+ complex. That means the precipitation of REF3 and ThF4·2.5 H2 O can be avoided in the leaching step. According to Eh-pH diagrams for the system Ce-F-Cl-H2 O, [CeF3]~+ in the leaching solution would be reduced to CeF3 precipitate in the presence of Cl^-, that is to say, tetravalent cerium and fluorine would be firstly leached out to form[CeF3]~+,which would then be reduced to CeF3 precipitate by Cl^-in the hydrochloric acid leaching process of roasted bastnaesite.
基金supported by the grant AX-1593(JCGZ)and AX1730(BC)from the Welch Foundation
文摘Solvothermal reaction of 3-aminoisonicotinic acid(Haina) and Cu(NO_3)_2·2.5H_2O gave a novel twodimensional(2D) microporous metal–organic framework, [Cu(aina)_2(DMF)]·DMF(1, DMF = N,N-dimethylformamide). Single-crystal X-ray crystallographic study of compound 1 revealed that Cu(II)ions are linked by ainaàligands forming square grid-like layers, which stack together via multiple hydrogen bonding interactions. The solvent-free framework of 1a displayed considerable porosity(void = 46.5%) with one-dimensional(1D) open channels(4.7 ? ? 4.8 ?) functionalized by amino groups.Gas sorption measurements of 1 revealed selective carbon dioxide(CO_2) and acetylene(C_2H_2) adsorption over methane(CH_4) and nitrogen(N_2) at ambient temperature.
基金supported by the National 863 Program(No.2006AA02Z227)Natural Science Foundation of Shaanxi Province(No.2011JZ002)+1 种基金the Foundation of Key Laboratory in Shaanxi Province(Nos.2010JS103,11JS097,14JS098)Shaanxi Provincial Science and Technology Co-ordinating innovation projects(No.2013SZS18-K01)
文摘Ionic liquids(ILs) immobilized on silica as novel high performance liquid chromatography(HPLC)stationary phases have attracted considerable attention. However, it has not been applied to protein separation. In this paper, N-methylimidazolium IL-modified silica-based stationary phase(Silpr Mim)was prepared and investigated as a novel multi-interaction stationary phase charged positively for protein separation. The results indicate that all of the basic proteins tested cannot be absorbed on this novel stationary phase, whereas all of the acidic proteins tested can be retained, and the baseline separation of eight kinds of acidic protein standards can be achieved when performed in reversed phase/ion-exchange chromatography(RPLC/IEC) mode. Compared with commonly used commercial octadecylated silica(ODS) column, the novel stationary phase can show selectivity and good resolution to acidic proteins, which has a promising application in the separation and analyses of acidic proteins from the complex samples in proteomics. In addition, the chromatographic behavior of proteins, the effect of the ligand structure and the retention mechanism on this stationary phase were also investigated.
基金Project supported by the National Natural Science Foundation of China.
文摘The strategy of expert system for high performance liquid chromatography was discussed, the attentions are mainly placed on the knowledge base for selection of column system, separation modes and detection modes in the analysis of amino acids, peptides and proteins.