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1996 Volume 13 Issue 3
1996, 13(3): 1-6
Abstract:
The research,commercial and potential applications concerning the solvent extraction of metal ions with organophosphine compounds,Cyanex extractants commercialized by American Cyanamid Co.,in the past ten years were briefly reviewed.
The research,commercial and potential applications concerning the solvent extraction of metal ions with organophosphine compounds,Cyanex extractants commercialized by American Cyanamid Co.,in the past ten years were briefly reviewed.
1996, 13(3): 7-11
Abstract:
Polyaniline composite positive film was prepared by using chemically synthesized polyaniline powder and plasticized polymer solid state electrolyte PEO-LiClO4.Its morphology was investigated with SEM.The electrochemical performance of the film and solid state lithium battery have been studied.
Polyaniline composite positive film was prepared by using chemically synthesized polyaniline powder and plasticized polymer solid state electrolyte PEO-LiClO4.Its morphology was investigated with SEM.The electrochemical performance of the film and solid state lithium battery have been studied.
1996, 13(3): 12-15
Abstract:
The polypropylene glycol polyurethane modified by polyhexylene carbonate diol (HPPU)was synthesized from polyhexylene carbonate diol(PHCD),polypropylene glycol (PPG),4,4'-diphenylmethane diisocyanate(MDI)and 1,4-butylene diol(BDO)by one-step technique.Its IR speetra,mechanical properties,resistance to hydrolysis and rheological behavior were studied.The results show that both the tensile strength and tensile stress at 100% and 300% strain increase with increasing content of PHCD in soft segment.When PHCD content in soft segment is 51.29%,the tensile strength increases to 150% of that of the non-modified PU.After dipping in water at 40℃ for 42 days,the retention of tensile strength is no less than 84%.
The polypropylene glycol polyurethane modified by polyhexylene carbonate diol (HPPU)was synthesized from polyhexylene carbonate diol(PHCD),polypropylene glycol (PPG),4,4'-diphenylmethane diisocyanate(MDI)and 1,4-butylene diol(BDO)by one-step technique.Its IR speetra,mechanical properties,resistance to hydrolysis and rheological behavior were studied.The results show that both the tensile strength and tensile stress at 100% and 300% strain increase with increasing content of PHCD in soft segment.When PHCD content in soft segment is 51.29%,the tensile strength increases to 150% of that of the non-modified PU.After dipping in water at 40℃ for 42 days,the retention of tensile strength is no less than 84%.
1996, 13(3): 16-19
Abstract:
Strongly basic ion exchange resin-supported phenyl selenide was prepared by reducing phSeSeph with polymer-supported borohydride.Its reactions with halides and epoxides in different conditions were studied.
Strongly basic ion exchange resin-supported phenyl selenide was prepared by reducing phSeSeph with polymer-supported borohydride.Its reactions with halides and epoxides in different conditions were studied.
1996, 13(3): 20-24
Abstract:
The investigation of the electrooxidation processes of(OEP)Co(Ⅱ)was carried out utilizing cyclic voltammetry(CV),electrochemical CV titration and in-situ thin-layer UV-Visible spectroelectrochemistry in 1,2-dichloroethane solution.It was indicated that Br can coordinate axially with(OEP)Co(Ⅱ)and three one-electron oxidation steps lead(OEP) Co(Ⅱ)to the formation of five-or six-dentate coodination species.The formation constants of these species were estimated.The electrooxidation mechanism of(OEP)Co(Ⅱ)in the presence of Br- anions was given.
The investigation of the electrooxidation processes of(OEP)Co(Ⅱ)was carried out utilizing cyclic voltammetry(CV),electrochemical CV titration and in-situ thin-layer UV-Visible spectroelectrochemistry in 1,2-dichloroethane solution.It was indicated that Br can coordinate axially with(OEP)Co(Ⅱ)and three one-electron oxidation steps lead(OEP) Co(Ⅱ)to the formation of five-or six-dentate coodination species.The formation constants of these species were estimated.The electrooxidation mechanism of(OEP)Co(Ⅱ)in the presence of Br- anions was given.
1996, 13(3): 25-29
Abstract:
Nine title compounds were synthesized from α-ethoxycarbonylcyclododecanone by reduction and condensation with aldehydes or ketones.Their structure was confirmed by IR, MS,1 NMR and elemental analysis.Conformational analysis of possible stereoisomers was carried out and the result was supported by 1 NMR.The pesticidal activities were examined and some of them found to be effective in promoting the growth of plant.
Nine title compounds were synthesized from α-ethoxycarbonylcyclododecanone by reduction and condensation with aldehydes or ketones.Their structure was confirmed by IR, MS,1 NMR and elemental analysis.Conformational analysis of possible stereoisomers was carried out and the result was supported by 1 NMR.The pesticidal activities were examined and some of them found to be effective in promoting the growth of plant.
1996, 13(3): 30-33
Abstract:
Tungstogalliumate heteropoly compound containing Cu(Ⅱ)was synthesized and characterized.The results of ESR shows that Cu(Ⅱ)is in the distorted octahedral field. The coordination bond Cu-O is found to be partially covalent.The data of variable temperature susceptibility approach Curie-Weiss law,Xm=C/(T-θ).
Tungstogalliumate heteropoly compound containing Cu(Ⅱ)was synthesized and characterized.The results of ESR shows that Cu(Ⅱ)is in the distorted octahedral field. The coordination bond Cu-O is found to be partially covalent.The data of variable temperature susceptibility approach Curie-Weiss law,Xm=C/(T-θ).
1996, 13(3): 34-37
Abstract:
It was found in this paper that only when sufficient amount of promoter molecules are adsorbed on the electrode surface,can the promoter effectively accelerate the electrochemical reaction of cytochrome c.For a promoter such as 2,2'-bipyridine,whose molecules possess weak adsorption strength on the electrode surface,a prolonged adsorption time, such as 10 hours,is required to attain the adsorption equilibrium with sufficient amout of promoter molecules adsorbed on the electrode surface.Therefore,it is better to use a modified procedure with prolonged dipping time to minimize the differences in promoter effects brought about by variations in the adsorption strength of the promoter molecules.
It was found in this paper that only when sufficient amount of promoter molecules are adsorbed on the electrode surface,can the promoter effectively accelerate the electrochemical reaction of cytochrome c.For a promoter such as 2,2'-bipyridine,whose molecules possess weak adsorption strength on the electrode surface,a prolonged adsorption time, such as 10 hours,is required to attain the adsorption equilibrium with sufficient amout of promoter molecules adsorbed on the electrode surface.Therefore,it is better to use a modified procedure with prolonged dipping time to minimize the differences in promoter effects brought about by variations in the adsorption strength of the promoter molecules.
1996, 13(3): 38-40
Abstract:
In this paper water-in-oil microemulsion phase composition and properties of Triton X-100~n-hexanol/cyclohexane/water system were studied.It shows that when Triton X-100 and n-hexanol is in weight ratio of 3:2,this water-in-oil microemulsion system has extensive and stable microemulsion phase regions.This system is insensitive to pH value, and still has extensive and stable microemulsion phase regions at varying temperatures from 11℃~40℃.
In this paper water-in-oil microemulsion phase composition and properties of Triton X-100~n-hexanol/cyclohexane/water system were studied.It shows that when Triton X-100 and n-hexanol is in weight ratio of 3:2,this water-in-oil microemulsion system has extensive and stable microemulsion phase regions.This system is insensitive to pH value, and still has extensive and stable microemulsion phase regions at varying temperatures from 11℃~40℃.
1996, 13(3): 41-45
Abstract:
Phase behaviour and solubilization of cholesterol in liquid crystal phase of C12(EO)4-H2O system and C12(EO)4-lecithin-H2O system were investigated.The phase diagram of C12(EO)4-lecithin-water-cholesterol system was similar to lecithin-water-cholesterol system.In C12(EO)4-H2O ststem,where cholesterol was solubilized,the concentration range of C12(EO)4 in liquid crystal was broader than that without cholesterol.The results of X-ray diffraction showed that,when cholesterol was solubilized into C12(EO)4-H2O lamellar liquid crystal,the thickness of amphiphile bilayer d0 increased,the amphiphile molecular array was more compact and the penetration of water molecules decreased.
Phase behaviour and solubilization of cholesterol in liquid crystal phase of C12(EO)4-H2O system and C12(EO)4-lecithin-H2O system were investigated.The phase diagram of C12(EO)4-lecithin-water-cholesterol system was similar to lecithin-water-cholesterol system.In C12(EO)4-H2O ststem,where cholesterol was solubilized,the concentration range of C12(EO)4 in liquid crystal was broader than that without cholesterol.The results of X-ray diffraction showed that,when cholesterol was solubilized into C12(EO)4-H2O lamellar liquid crystal,the thickness of amphiphile bilayer d0 increased,the amphiphile molecular array was more compact and the penetration of water molecules decreased.
1996, 13(3): 46-49
Abstract:
A one-pot selective synthesis of phenylglycine with high yield from benzaldehyde, chloroform,potassium hydroxide and ammonia in the presence of phase-transfer catalyst (PTC)and β-cyclodextrin(β-CD)binary catalyst system has been studied.Results obtained are far superior to that of other similar methods.The data show that PTC β-CD is a more efficient catalyst than either PTC or β-CD alone,and both cationic and nonionie PTC-β-CD can enhance the production of phenylglycine with good yields and selectivities.A preliminary mechanism is also discussed.
A one-pot selective synthesis of phenylglycine with high yield from benzaldehyde, chloroform,potassium hydroxide and ammonia in the presence of phase-transfer catalyst (PTC)and β-cyclodextrin(β-CD)binary catalyst system has been studied.Results obtained are far superior to that of other similar methods.The data show that PTC β-CD is a more efficient catalyst than either PTC or β-CD alone,and both cationic and nonionie PTC-β-CD can enhance the production of phenylglycine with good yields and selectivities.A preliminary mechanism is also discussed.
1996, 13(3): 50-54
Abstract:
The dissociation constants of N-salicylideneamino acids(Sal:A)and stability contants of binary complexes of Ni(Ⅰ)-salicylideneamino acid and Ni(Ⅱ)-α-amino acid and ternary mixed ligand complexes of Ni(Ⅱ)-N-salicylideneamino acid(ligand A)-α-amino acid (ligand B)at(25±0.1)℃ and in the presence of 0.1mol/dm3 KNO3 have been determined by pH method.The a-amino acids(Aa)used were glycine(Gly),L-serine(Ser),L-valine (Val),L-leucine(Leu),L-isoleucine(Iso)and L-proline(Pro).It was found that the linear free energy relationship(LFER)exists nicely between the following parameter pairs logβ120 and pK2A,logβ102 and pK2B,logβ111 andp pK2A,logβ111 and pK2B.The △logK was used to characterize the stability of ternary complexes related to the stability of parent binary complexes. The hydrophobic ligand-ligand interaction in the Ni(Sal:P)(P denotes phenylalanine)was studied.
The dissociation constants of N-salicylideneamino acids(Sal:A)and stability contants of binary complexes of Ni(Ⅰ)-salicylideneamino acid and Ni(Ⅱ)-α-amino acid and ternary mixed ligand complexes of Ni(Ⅱ)-N-salicylideneamino acid(ligand A)-α-amino acid (ligand B)at(25±0.1)℃ and in the presence of 0.1mol/dm3 KNO3 have been determined by pH method.The a-amino acids(Aa)used were glycine(Gly),L-serine(Ser),L-valine (Val),L-leucine(Leu),L-isoleucine(Iso)and L-proline(Pro).It was found that the linear free energy relationship(LFER)exists nicely between the following parameter pairs logβ120 and pK2A,logβ102 and pK2B,logβ111 andp pK2A,logβ111 and pK2B.The △logK was used to characterize the stability of ternary complexes related to the stability of parent binary complexes. The hydrophobic ligand-ligand interaction in the Ni(Sal:P)(P denotes phenylalanine)was studied.
1996, 13(3): 55-59
Abstract:
The effects of anions(SH- and SCN-)on inhibition and adsorption behaviors of butyltrimethylphosphonium bromide(BTMPB)for corrosion inhibition of aluminum have been studied by using the differential polarization resistance and impedance determination techniques in 1 mol/L Al(ClO4)3 solution at 25~45℃.The results showed that SH- or SCN- can increase prominently the inhibitive efficiency of BTMPB for corrosion inhibition of aluminum,and that the synergistic effect of corrosion inhibition appears between the anions and BTMPB.The adsorption of BTMPB follows Langmuir isotherm on the aluminum surface in 1 mol/L Al(ClO4)3 solution,and it belongs to the physical adsorption.When the anions are added to 1 mol/L Al(ClO4)3 solution containing BTMPB,the adsorption of BTMPB belongs to the chemical adsorption,and it follows the amended Bockris-Swinkels isotherm.
The effects of anions(SH- and SCN-)on inhibition and adsorption behaviors of butyltrimethylphosphonium bromide(BTMPB)for corrosion inhibition of aluminum have been studied by using the differential polarization resistance and impedance determination techniques in 1 mol/L Al(ClO4)3 solution at 25~45℃.The results showed that SH- or SCN- can increase prominently the inhibitive efficiency of BTMPB for corrosion inhibition of aluminum,and that the synergistic effect of corrosion inhibition appears between the anions and BTMPB.The adsorption of BTMPB follows Langmuir isotherm on the aluminum surface in 1 mol/L Al(ClO4)3 solution,and it belongs to the physical adsorption.When the anions are added to 1 mol/L Al(ClO4)3 solution containing BTMPB,the adsorption of BTMPB belongs to the chemical adsorption,and it follows the amended Bockris-Swinkels isotherm.
1996, 13(3): 60-64
Abstract:
Four new binuclear complexes,[Cu2(IPHTA)(phen)4](ClO4)2(1),[Cu2(IPHTA)(tmen)4](ClO4)2·H2O(2),[Co2(IPHTA)(phen)4](ClO4)2(3)and[Co2(IPHTA)(tmen)4](ClO4)2(4)(IPHTA,phen and tmen denote isophthalato dianion; 1,10-phenanthroline and N,N,N',N'-tetramethylethlenediamine respectively)were synthesized and characterized by elemental analysis,IR,electronic spectra,conductivity and variable temperature magnetic susceptibility measurements.Based on the Heisenberg model, the exchange integral,J,was found to be 2.30 cm-1for(1),3.82 cm-1for(2),8.09 cm-1 for(3)and 8.20 cm-1for(4),indicating that a weak ferromagnetic spin exchange interaction occurs between the two metal ions.The biological activities of the complexes were also tested.
Four new binuclear complexes,[Cu2(IPHTA)(phen)4](ClO4)2(1),[Cu2(IPHTA)(tmen)4](ClO4)2·H2O(2),[Co2(IPHTA)(phen)4](ClO4)2(3)and[Co2(IPHTA)(tmen)4](ClO4)2(4)(IPHTA,phen and tmen denote isophthalato dianion; 1,10-phenanthroline and N,N,N',N'-tetramethylethlenediamine respectively)were synthesized and characterized by elemental analysis,IR,electronic spectra,conductivity and variable temperature magnetic susceptibility measurements.Based on the Heisenberg model, the exchange integral,J,was found to be 2.30 cm-1for(1),3.82 cm-1for(2),8.09 cm-1 for(3)and 8.20 cm-1for(4),indicating that a weak ferromagnetic spin exchange interaction occurs between the two metal ions.The biological activities of the complexes were also tested.
1996, 13(3): 65-68
Abstract:
The stability constants of ternary complexes of Cd(ATP)(Aa)and of corresponding binary complexes have been determined by potentiometric pH titration in solution at 37℃ and at 0.10 mol/L ionic strength(ATP=adenosine triphosphate,Aa=alanine(ala),methionine(met),phenylalanine(phe)or tryptophan(trp)respectively).The relative stabilities of the ternary complexes in the amino acid ligand order are trp- >met- >phe- >ala-.The possible reasons have been discussed in terms of intramolecular ligand-ligand interactions specially the hydrophobic association including aromatic ring stacking.In order to characterize the intramolecular ligand-ligand interaction quantitatively,the equilibrium constants,K1,of transfer between opened species(in the absense of the ligand-ligand interaction)and closed species(with ligand-ligand interaction)have been calculated.The results show that the closed species of ternary complexes containing trp,met or phe as one of ligands are the major components in solution.
The stability constants of ternary complexes of Cd(ATP)(Aa)and of corresponding binary complexes have been determined by potentiometric pH titration in solution at 37℃ and at 0.10 mol/L ionic strength(ATP=adenosine triphosphate,Aa=alanine(ala),methionine(met),phenylalanine(phe)or tryptophan(trp)respectively).The relative stabilities of the ternary complexes in the amino acid ligand order are trp- >met- >phe- >ala-.The possible reasons have been discussed in terms of intramolecular ligand-ligand interactions specially the hydrophobic association including aromatic ring stacking.In order to characterize the intramolecular ligand-ligand interaction quantitatively,the equilibrium constants,K1,of transfer between opened species(in the absense of the ligand-ligand interaction)and closed species(with ligand-ligand interaction)have been calculated.The results show that the closed species of ternary complexes containing trp,met or phe as one of ligands are the major components in solution.
1996, 13(3): 69-71
Abstract:
The properties of thiourea dioxide(TD)in solution were studied by potentiometric method.By analyzing the potential-time curves of various TD solutions with different pH and temperature,it was found that the pH value and temperature deeply affect the structure, reducing power and stability of TD solutions.TD is very stable in neutral solutions at room temperature.With the increase of basicity and temperature,the concentration of the tautomer B and the reducing power of TD solutions were enhanced,while the stability of TD decreased.
The properties of thiourea dioxide(TD)in solution were studied by potentiometric method.By analyzing the potential-time curves of various TD solutions with different pH and temperature,it was found that the pH value and temperature deeply affect the structure, reducing power and stability of TD solutions.TD is very stable in neutral solutions at room temperature.With the increase of basicity and temperature,the concentration of the tautomer B and the reducing power of TD solutions were enhanced,while the stability of TD decreased.
1996, 13(3): 72-74
Abstract:
The synthesis of(La,Ce,Tb)PO4 by means of microwave heating is reported. The analysis of X-ray powder diffraction data shows that the phosphor belongs to the monoclinic system with the structure of monazite.The phosphor has the maximum excitation peak at λex=273.5 nm and maximum emission peak at λem=543 nm,the latter being the characteristic emission of Tb3+ ion.The effects of different flux and(NH4)2HPO4 dosage on the luminescence intensity are examined and the chromatic coordinates and related chromatic temperature are measured.
The synthesis of(La,Ce,Tb)PO4 by means of microwave heating is reported. The analysis of X-ray powder diffraction data shows that the phosphor belongs to the monoclinic system with the structure of monazite.The phosphor has the maximum excitation peak at λex=273.5 nm and maximum emission peak at λem=543 nm,the latter being the characteristic emission of Tb3+ ion.The effects of different flux and(NH4)2HPO4 dosage on the luminescence intensity are examined and the chromatic coordinates and related chromatic temperature are measured.
1996, 13(3): 75-77
Abstract:
Poly(vinyl chloride)/poly(propylene carbonate)blends are prepared by methods of solution and melting,and are proved immiscible by DSC,but their immiscibility degrees are affected by molccular weight and blending ratio.PVC content in PPC-rich phase in solution blends is calculated according to glass transition temperature(Tg).As coupling agent, NBR-PPC elastomer has a great compatibility effect on PVC/PPC blends.The amount and molecular weight of PPC influence the mechanical properties of PVC/PPC blends.
Poly(vinyl chloride)/poly(propylene carbonate)blends are prepared by methods of solution and melting,and are proved immiscible by DSC,but their immiscibility degrees are affected by molccular weight and blending ratio.PVC content in PPC-rich phase in solution blends is calculated according to glass transition temperature(Tg).As coupling agent, NBR-PPC elastomer has a great compatibility effect on PVC/PPC blends.The amount and molecular weight of PPC influence the mechanical properties of PVC/PPC blends.
1996, 13(3): 78-80
Abstract:
Using the extraction system consisting of trioctylamine and 1-octanal,the complexing extraction of glycollic acid from dilute solution was studied,the effects of temperature and extractant concentration on the distribution coefficient were discussed,and the constitution of complex and thermal effect(-△H)of extraction were determined.In addition, that two bonding types took part in the process of Lewis acid-base complexing extraction were confirmed further through analyzing the infra-red spectrum of glycollic acid loaded organic phase.
Using the extraction system consisting of trioctylamine and 1-octanal,the complexing extraction of glycollic acid from dilute solution was studied,the effects of temperature and extractant concentration on the distribution coefficient were discussed,and the constitution of complex and thermal effect(-△H)of extraction were determined.In addition, that two bonding types took part in the process of Lewis acid-base complexing extraction were confirmed further through analyzing the infra-red spectrum of glycollic acid loaded organic phase.
1996, 13(3): 81-83
Abstract:
Microdomain morphology in styrene-butadiene-styrene triblock copolymer(SBS) and polystyrene(PS)blends was investigated as a function of PS concentration and molecular weight.The triblock copolymer containing 28% of PS resembles cylindrical morphology. Two PS with molecular weight of 500 and 12,000,respectively,were blended with the triblock copolymer up to a concentration of 25%.It was found that the microdomain morphology did not change with the addition of low molecular weight PS up to the concentration of 25%,while the cylinder-lamellar transition was observed for the blends containing the high molecular weight PS.The difference between the two systems is attributed to the addition of the homopolymer,which not only changes the volume fraction of one component,but also varies the values of)ON(where χ is the interaction parameter and N is the polymerization index of copolymer).Thus the microdomain morphology in blends of block copolymer and homopolymer is determined by the composition and the values of χN,and the latter determines whether the blend is in the strong segregation limit or the weak segregation limit.In the strong segregation limit,the microdomain morphology depends strongly on the composition; while in the weak segregation limit,it is weakly dependent on the composition.This is in good agreement with the predictions of mean-field theory.
Microdomain morphology in styrene-butadiene-styrene triblock copolymer(SBS) and polystyrene(PS)blends was investigated as a function of PS concentration and molecular weight.The triblock copolymer containing 28% of PS resembles cylindrical morphology. Two PS with molecular weight of 500 and 12,000,respectively,were blended with the triblock copolymer up to a concentration of 25%.It was found that the microdomain morphology did not change with the addition of low molecular weight PS up to the concentration of 25%,while the cylinder-lamellar transition was observed for the blends containing the high molecular weight PS.The difference between the two systems is attributed to the addition of the homopolymer,which not only changes the volume fraction of one component,but also varies the values of)ON(where χ is the interaction parameter and N is the polymerization index of copolymer).Thus the microdomain morphology in blends of block copolymer and homopolymer is determined by the composition and the values of χN,and the latter determines whether the blend is in the strong segregation limit or the weak segregation limit.In the strong segregation limit,the microdomain morphology depends strongly on the composition; while in the weak segregation limit,it is weakly dependent on the composition.This is in good agreement with the predictions of mean-field theory.
1996, 13(3): 84-86
Abstract:
A series of polyimides is prepared using 5-trifluoromethyl-1,3-phenylenediamine with dianhydrides of different structures.Polyamic acids prepared from this diamine are converted to imide films by thermal method.The polyimide films in most cases are ereasable and do not break on the fold line.Most polyimide films are in light color and soluble in m-cresol and DMAc.The polyimides have high glass transition temperature and thermostability.
A series of polyimides is prepared using 5-trifluoromethyl-1,3-phenylenediamine with dianhydrides of different structures.Polyamic acids prepared from this diamine are converted to imide films by thermal method.The polyimide films in most cases are ereasable and do not break on the fold line.Most polyimide films are in light color and soluble in m-cresol and DMAc.The polyimides have high glass transition temperature and thermostability.
1996, 13(3): 87-89
Abstract:
We have prepared covalently modified graphite electrodes(CelValM)that bind L-valine methyl ester to their surface via amide bonds,thereby providing a stable,chiral interfacial region for the reduction of acetophenone.The optical yield(o.y.)and chemical yield (c.y.)of S(-)-1-phenylethanol were measured as a function of CelValM cathode potential, current density,amount of electricity passed,substrate concentration,pH,and the number of repeated use of electrodes.The highest o.y.was 15.8%.The characteristics and kinetic parameters of electrode processes were determined by potentiodynamic method and rotating disk electrode.A possible mechanism of the asymmetric electroreduction of acetophenone was forwarded.
We have prepared covalently modified graphite electrodes(CelValM)that bind L-valine methyl ester to their surface via amide bonds,thereby providing a stable,chiral interfacial region for the reduction of acetophenone.The optical yield(o.y.)and chemical yield (c.y.)of S(-)-1-phenylethanol were measured as a function of CelValM cathode potential, current density,amount of electricity passed,substrate concentration,pH,and the number of repeated use of electrodes.The highest o.y.was 15.8%.The characteristics and kinetic parameters of electrode processes were determined by potentiodynamic method and rotating disk electrode.A possible mechanism of the asymmetric electroreduction of acetophenone was forwarded.
1996, 13(3): 90-92
Abstract:
The extraction of lanthanide ions(La3+,Pr3+,Nd3+,Gd3+)from nitric acid solution with mixtures of bis-(1'-phenyl-3'-methyl-5'-pyrazolone-4'-yl)ethanedione (H2BPMPED or H2A)and phenanthroline(phen)has been studied.The synergic extraction coefficent of neodymium is 3.56.The composition of extracted compound of neodymium is shown to be NdA·HA·phen.The pH values of half extraction of La3+,Pr3+,Nd3+,Gd3+ are 4.12,3.74,3.46,3.11 respectively.The extraction equilibrium constants enthalpy change and entropy change of the reaction have been calculated.
The extraction of lanthanide ions(La3+,Pr3+,Nd3+,Gd3+)from nitric acid solution with mixtures of bis-(1'-phenyl-3'-methyl-5'-pyrazolone-4'-yl)ethanedione (H2BPMPED or H2A)and phenanthroline(phen)has been studied.The synergic extraction coefficent of neodymium is 3.56.The composition of extracted compound of neodymium is shown to be NdA·HA·phen.The pH values of half extraction of La3+,Pr3+,Nd3+,Gd3+ are 4.12,3.74,3.46,3.11 respectively.The extraction equilibrium constants enthalpy change and entropy change of the reaction have been calculated.
1996, 13(3): 93-95
Abstract:
Tb(Ⅲ)/Ca(Ⅱ)-L-glutamic acid-L-threonine systems were studied at 37℃ and in solution with an ionic strength of 0.15 mol/L(NaCl)by potentiometric titration.The stability constants of Tb(Ⅲ),Ca(Ⅱ)complexes with L-glutamic acid and L-threonine were obtained.Results show that Tb(Ⅲ),Ca(Ⅱ)ternary complexes are the main species among all species in ternary systems and that Tb(Ⅲ)complexes are more stable than Ca(Ⅱ)complexes.
Tb(Ⅲ)/Ca(Ⅱ)-L-glutamic acid-L-threonine systems were studied at 37℃ and in solution with an ionic strength of 0.15 mol/L(NaCl)by potentiometric titration.The stability constants of Tb(Ⅲ),Ca(Ⅱ)complexes with L-glutamic acid and L-threonine were obtained.Results show that Tb(Ⅲ),Ca(Ⅱ)ternary complexes are the main species among all species in ternary systems and that Tb(Ⅲ)complexes are more stable than Ca(Ⅱ)complexes.
1996, 13(3): 96-98
Abstract:
The effect of pre-eatalyst homogeneous reaction on the selective oxidation of propane over Bi-V-Mo-O catalyst in a glass reactor has been investigated.It was found that a majority of propane molecules is activated in the homogeneous reaction stage through radical Chain mechanism and the homogeneous reaction may influence the final product distribution.The catalytic reaction would not take place unless there is a homogeneous reaction which aims at activating propane.The results show that it is the propene,the reactive intermediate of homogeneous reaction,that will be further oxidized to produce acrolein in the presence of catalyst.The catalytic reaction of propane is a combination of homogeneous and heterogeneous reactions.
The effect of pre-eatalyst homogeneous reaction on the selective oxidation of propane over Bi-V-Mo-O catalyst in a glass reactor has been investigated.It was found that a majority of propane molecules is activated in the homogeneous reaction stage through radical Chain mechanism and the homogeneous reaction may influence the final product distribution.The catalytic reaction would not take place unless there is a homogeneous reaction which aims at activating propane.The results show that it is the propene,the reactive intermediate of homogeneous reaction,that will be further oxidized to produce acrolein in the presence of catalyst.The catalytic reaction of propane is a combination of homogeneous and heterogeneous reactions.
1996, 13(3): 99-101
Abstract:
The reaction of E(EDTB)Cu](CH3COO)2 with H3PMo12O40 in absolute ethanol produces[(EDTB)Cu](HPMo12O40)(C2H5OH)6,in which EDTB is N,N,N',N'-tetrakis[(2-benzimidazolyl)methyl]-1,2-ethanediamine.A comparative study of IR spectra、UV-Vis spectra,1 NMR and elemental analysis for the product and reference molecule[(EDTB) Cu](NO3)2 confirms the structure of the title compound.
The reaction of E(EDTB)Cu](CH3COO)2 with H3PMo12O40 in absolute ethanol produces[(EDTB)Cu](HPMo12O40)(C2H5OH)6,in which EDTB is N,N,N',N'-tetrakis[(2-benzimidazolyl)methyl]-1,2-ethanediamine.A comparative study of IR spectra、UV-Vis spectra,1 NMR and elemental analysis for the product and reference molecule[(EDTB) Cu](NO3)2 confirms the structure of the title compound.
1996, 13(3): 102-104
Abstract:
The solubilities and refractive indices of the saturated solutions of C6H12O6C2H5OH-H2O ternary system have been determined.The solubility curve and refractive index curve of the system at 35℃ consist of 3 branches,corresponding to C6H12O6·10H2O, C6H12O6·H2O,and C6H12O6 respectively.The composition of eutectic solutions at two nonvariant points is(C6H12O6:7.07%,C2H5OH:17.07%) and (C6H12O6:0.05%,C2H5OH:91.21%).
The solubilities and refractive indices of the saturated solutions of C6H12O6C2H5OH-H2O ternary system have been determined.The solubility curve and refractive index curve of the system at 35℃ consist of 3 branches,corresponding to C6H12O6·10H2O, C6H12O6·H2O,and C6H12O6 respectively.The composition of eutectic solutions at two nonvariant points is(C6H12O6:7.07%,C2H5OH:17.07%) and (C6H12O6:0.05%,C2H5OH:91.21%).
1996, 13(3): 105-106
Abstract:
The ZSM-5 and Y zeolites were pulverized by air stream to form fine particles. The particle size distribution,surface area,IR and TPD spectra were determined for both of the raw and fine particles.The catalytic activity of fine particle in cumene cracking was compared with the raw on pulse microreactor connected on line with a chromatograph.After ZSM-5 and Y zeolites being pulverized,their B and L acid amount increased and catalytic activity improved apparently.
The ZSM-5 and Y zeolites were pulverized by air stream to form fine particles. The particle size distribution,surface area,IR and TPD spectra were determined for both of the raw and fine particles.The catalytic activity of fine particle in cumene cracking was compared with the raw on pulse microreactor connected on line with a chromatograph.After ZSM-5 and Y zeolites being pulverized,their B and L acid amount increased and catalytic activity improved apparently.
1996, 13(3): 107-108
Abstract:
A fullerene azobenzene derivative was synthesized by the reaction of C60 with fast black K salt.The product was isolated by means of silica gel chromatography and identified by field desorption mass spectrometry and 13C NMR spectroscopy,UV spectrometry and IR spectroscopy.Some of theoretical analyses were given.
A fullerene azobenzene derivative was synthesized by the reaction of C60 with fast black K salt.The product was isolated by means of silica gel chromatography and identified by field desorption mass spectrometry and 13C NMR spectroscopy,UV spectrometry and IR spectroscopy.Some of theoretical analyses were given.
1996, 13(3): 109-110
Abstract:
W-type zeolite WQD-1 is successfully synthesized with industrial sodium silicate, aluminium sulfate and potassium hydroxide.The equilibrium exchange quantity of zeolite WQD-1 in sea water and brine are 55 mg/g and 75 mg/g respectively.
W-type zeolite WQD-1 is successfully synthesized with industrial sodium silicate, aluminium sulfate and potassium hydroxide.The equilibrium exchange quantity of zeolite WQD-1 in sea water and brine are 55 mg/g and 75 mg/g respectively.
1996, 13(3): 111-112
Abstract:
The pyrolysis of polyborazinylamine precursors leading to boron nitride(BN)ceramics has been studied by means of DTA-TG-GC,FTIR and XRD.The results show that the pyrolysis starts at 180℃ and the loss of 60% weight mainly occurs under 600℃.N2, NH3 and HCl are given off during pyrolysis and h-BN ceramics are obtained at 1600℃.
The pyrolysis of polyborazinylamine precursors leading to boron nitride(BN)ceramics has been studied by means of DTA-TG-GC,FTIR and XRD.The results show that the pyrolysis starts at 180℃ and the loss of 60% weight mainly occurs under 600℃.N2, NH3 and HCl are given off during pyrolysis and h-BN ceramics are obtained at 1600℃.
1996, 13(3): 113-114
Abstract:
The preconcentration of residual quintozene in vegetable with a solid phase extraction column of Florisil and gas chromatographic determination was reported in this paper. This method is fast and efficient for residual quintozene analysis in vegetable.A 10% mixture of acetone-hexane was used as eluent that gave the best recoveries(92.0%~97.6%). The relative standard deviation is between 2.64%~6.07%.
The preconcentration of residual quintozene in vegetable with a solid phase extraction column of Florisil and gas chromatographic determination was reported in this paper. This method is fast and efficient for residual quintozene analysis in vegetable.A 10% mixture of acetone-hexane was used as eluent that gave the best recoveries(92.0%~97.6%). The relative standard deviation is between 2.64%~6.07%.
1996, 13(3): 115-116
Abstract:
A new synthetic method of 10-vinylphenothiazine with C2H2 under ordinary pressure was reported.A mixture of phenothiazine and KOH in DMSO was treated with C2H2 at 170℃ for 10 h to give 97% of yield.The reaction mechanism was explored preliminarily.
A new synthetic method of 10-vinylphenothiazine with C2H2 under ordinary pressure was reported.A mixture of phenothiazine and KOH in DMSO was treated with C2H2 at 170℃ for 10 h to give 97% of yield.The reaction mechanism was explored preliminarily.
1996, 13(3): 117-118
Abstract:
The thermograms of hydrolytic polymerization of Fe(Ⅲ)have been obtained using a thermal activity monitor.The heat of reaction(△rHmφ),the hydrolysis equilibrium constants(Kφ)and thermodynamic functions(△rGmφ,△rSmφ)at different temperatures have been calculated.
The thermograms of hydrolytic polymerization of Fe(Ⅲ)have been obtained using a thermal activity monitor.The heat of reaction(△rHmφ),the hydrolysis equilibrium constants(Kφ)and thermodynamic functions(△rGmφ,△rSmφ)at different temperatures have been calculated.
