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2004 Volume 21 Issue 10
2004, 21(10): 973-979
Abstract:
As important organic intermediates, terminal aryl acetylenes have been widely applied in the organic and polymer field. The effect of reactants(alkynylzinc reagents and aryl halides reagent), catalysts(palladium-catalyst and cocatalyst) and other reaction conditions on the synthesis of terminal aryl acetylene are reviewed. The reaction mechanisms of palladium catalyzed coupling elimination reaction are discussed, showing that palladium-catalyzed coupling-elimination reaction is an effective method in the synthesis of the terminal aryl acetylene.
As important organic intermediates, terminal aryl acetylenes have been widely applied in the organic and polymer field. The effect of reactants(alkynylzinc reagents and aryl halides reagent), catalysts(palladium-catalyst and cocatalyst) and other reaction conditions on the synthesis of terminal aryl acetylene are reviewed. The reaction mechanisms of palladium catalyzed coupling elimination reaction are discussed, showing that palladium-catalyzed coupling-elimination reaction is an effective method in the synthesis of the terminal aryl acetylene.
2004, 21(10): 980-984
Abstract:
TiO2-SnO2 nanoparticles were prepared by sol-gel method. XRD, IR and XPS were used to characterize the nanoparticles. The photocatalytic oxidation of heptane was used as model reaction to measure the photocatalytic activity of the TiO2-SnO2 nanoparticles. The particle size of TiO2-SnO2 increases from 10.0 nm to 34.2 nm as the calcination temperature increases and the structure changes from anatase to rutile at 500~600℃. At the same time, the photocatalytic activity in heptane degradation is decreased. The particles with n(Sn)/n(Ti)=0.06, afford the best photocatalytic activity.
TiO2-SnO2 nanoparticles were prepared by sol-gel method. XRD, IR and XPS were used to characterize the nanoparticles. The photocatalytic oxidation of heptane was used as model reaction to measure the photocatalytic activity of the TiO2-SnO2 nanoparticles. The particle size of TiO2-SnO2 increases from 10.0 nm to 34.2 nm as the calcination temperature increases and the structure changes from anatase to rutile at 500~600℃. At the same time, the photocatalytic activity in heptane degradation is decreased. The particles with n(Sn)/n(Ti)=0.06, afford the best photocatalytic activity.
2004, 21(10): 985-988
Abstract:
The phase relation of chloropoinnoite water pseudo binary system at 273 K to 453 K has been studied by phase equilibrium method. The results show that the phase transformation products of chloropinnoite in the water are clearly influenced by the temperature:from273 K to 314 K inderite 2MgO·3B2O3·15H2O, from 314 K to 360 K poinnoiteit MgO·B2O3·3H2O, and from 360 K to 453 K a new hydrated borate, α ascharite, 2MgO·B2O3·2H2O are formed respectively. The solubility of these magnesium borates has been determined at various temperatures, and a mechanism of dissolution and phase transformation is proposed.
The phase relation of chloropoinnoite water pseudo binary system at 273 K to 453 K has been studied by phase equilibrium method. The results show that the phase transformation products of chloropinnoite in the water are clearly influenced by the temperature:from273 K to 314 K inderite 2MgO·3B2O3·15H2O, from 314 K to 360 K poinnoiteit MgO·B2O3·3H2O, and from 360 K to 453 K a new hydrated borate, α ascharite, 2MgO·B2O3·2H2O are formed respectively. The solubility of these magnesium borates has been determined at various temperatures, and a mechanism of dissolution and phase transformation is proposed.
2004, 21(10): 989-992
Abstract:
Alkoxy group and fluorine atom were introduced onto the carbon chain of the substituent of the pyrimidine ring, and 12 novel sulfonylurea compounds with mono substituent in the pyrimidine ring were synthesized. The structures of all compounds were confirmed by 1H NMR and elemental analysis. Herbicidal activity tests including IC50 in rape root and pot experiments were carried out. The results show that the herbicidal activity decreases as the hydrogen atoms of the alkoxy group at 4-position of the pyrimidine ring are substituted by alkyl, alkoxy groups or fluorine atoms.
Alkoxy group and fluorine atom were introduced onto the carbon chain of the substituent of the pyrimidine ring, and 12 novel sulfonylurea compounds with mono substituent in the pyrimidine ring were synthesized. The structures of all compounds were confirmed by 1H NMR and elemental analysis. Herbicidal activity tests including IC50 in rape root and pot experiments were carried out. The results show that the herbicidal activity decreases as the hydrogen atoms of the alkoxy group at 4-position of the pyrimidine ring are substituted by alkyl, alkoxy groups or fluorine atoms.
2004, 21(10): 993-996
Abstract:
Four methyl-subsituted poly(aryl-ether-ketone)s were prepared by electrophilic polymerization of 4,4'-bis(o-methylphenoxy)diphenylketone(Me-DPO-BP) and 1,4-bis(4-(2-methylphenoxy)benzoyl) benzene (Me-DPOTPK), respectively with terephthaloyl(TPC) or isophthaloyl(IPC) in 1,2-dichloroethane and in the presence of DMF and AlCl3. The polymers were characterized by FT-IR, 1H NMR, 13C NMR, DSC, TGA and WAXD techniques. The results show that the Tg of the polymers are 156~170℃ and Tm 175~254℃. The four polymers exhibit high thermal stability, and their crystallinity is lower than that of polyaromatic ether ketone ketone(PEKK). The polymers have good chemical resistance.
Four methyl-subsituted poly(aryl-ether-ketone)s were prepared by electrophilic polymerization of 4,4'-bis(o-methylphenoxy)diphenylketone(Me-DPO-BP) and 1,4-bis(4-(2-methylphenoxy)benzoyl) benzene (Me-DPOTPK), respectively with terephthaloyl(TPC) or isophthaloyl(IPC) in 1,2-dichloroethane and in the presence of DMF and AlCl3. The polymers were characterized by FT-IR, 1H NMR, 13C NMR, DSC, TGA and WAXD techniques. The results show that the Tg of the polymers are 156~170℃ and Tm 175~254℃. The four polymers exhibit high thermal stability, and their crystallinity is lower than that of polyaromatic ether ketone ketone(PEKK). The polymers have good chemical resistance.
2004, 21(10): 997-1001
Abstract:
The adsorption behavior of 2-naphthalenesulfonic acid(2-NSA), p-tuluenesulfonic acid(p TSA), p-chlorobenesulfonic acid(p-CBSA), and 4,4'-dinitrostilibene 2,2'-disulfonic acid(DNS) onto a macroporous weakly basic anion-exchanger(D301) have been investigated. The results indicated that it is a favorable and spontaneous adsorption process, and the adsorption isotherm data can be satisfactorily fitted with the Redlich Peterson equation. The adsorption of strong aromatic sulfonic acids on D301 is due to electrostatic interaction, whereas the adsorption of weak aromatic sulfonic acids DNS on D301 is a result of Van der Waals forces. Positive △H and △S values show that the process of adsorption of 2-naphthalenesulfonic acid, p-tuluenesul fonic acid, p-chlorobenesulfonic acid on D301 is endothermic and entropy driven. The negative △H and △S values for DNS acid indicate that the adsorption is exothermic and enthalpy driven.
The adsorption behavior of 2-naphthalenesulfonic acid(2-NSA), p-tuluenesulfonic acid(p TSA), p-chlorobenesulfonic acid(p-CBSA), and 4,4'-dinitrostilibene 2,2'-disulfonic acid(DNS) onto a macroporous weakly basic anion-exchanger(D301) have been investigated. The results indicated that it is a favorable and spontaneous adsorption process, and the adsorption isotherm data can be satisfactorily fitted with the Redlich Peterson equation. The adsorption of strong aromatic sulfonic acids on D301 is due to electrostatic interaction, whereas the adsorption of weak aromatic sulfonic acids DNS on D301 is a result of Van der Waals forces. Positive △H and △S values show that the process of adsorption of 2-naphthalenesulfonic acid, p-tuluenesul fonic acid, p-chlorobenesulfonic acid on D301 is endothermic and entropy driven. The negative △H and △S values for DNS acid indicate that the adsorption is exothermic and enthalpy driven.
2004, 21(10): 1002-1005
Abstract:
TiO2/SiO2 aerogel was prepared by non supercritical drying process. The molar ratio of TiO2 to SiO2 was 1:3. After calcination at 500℃ the TiO2/SiO2 aerogel still had a high BET area(283.26 m2/g) and the pore diameter between 2~30 nm. The results of photocatalytic degradation of pyridine over the aerogel in weak acidic, neutral, and weak basic pyridine solution indicate that the aerogel is more active than TiO2 powder. At pH=9, the TiO2/SiO2 aerogel shows the highest photocatalytic activity, and the degradation ratio of pyridine increases up to 97% when the reaction time is 6.5 h, compared to only 70% for TiO2 powders.
TiO2/SiO2 aerogel was prepared by non supercritical drying process. The molar ratio of TiO2 to SiO2 was 1:3. After calcination at 500℃ the TiO2/SiO2 aerogel still had a high BET area(283.26 m2/g) and the pore diameter between 2~30 nm. The results of photocatalytic degradation of pyridine over the aerogel in weak acidic, neutral, and weak basic pyridine solution indicate that the aerogel is more active than TiO2 powder. At pH=9, the TiO2/SiO2 aerogel shows the highest photocatalytic activity, and the degradation ratio of pyridine increases up to 97% when the reaction time is 6.5 h, compared to only 70% for TiO2 powders.
2004, 21(10): 1006-1010
Abstract:
The precursor Ti(OEt)4 prepared by anodic dissolution of metallic titanium in absolute ethanol was directly hydrolyzed by a sol-gel process to give nano-TiO2 film on a titanium electrode(Ti/nano-TiO2). Redox behavior and electrocatalytic activity of the Ti/nano-TiO2 electrode was investigated by cyclic voltammetry, potential step chronoampermetry, and bulk electrolysis. The results indicated that there were two pairs of well defined redox peaks for Ti/nano-TiO2 film electrode in the 1 mol/L H2SO4 in correspondence with TiO2/Ti2O3 and TiO2/Ti(OH)3 reversible electrode processes with E1/2r being -0.56 V and -0.96 V(vs.SCE), respectively, at 0.1 V/s. Ti/nano-TiO2 electrode showed a high heterogeneous electrocatalytic activitiy in acidic medium in reduction of o-nitrophenol. The indirect electroreduction of o-nitrophenol to o-aminophenol by TiⅣ/TiⅢ redox pair on nano TiO2 film surface is believed to follow chemical catalysis mechanism(EC'). In preparative electrolysis at 50℃ on Ti/nano-TiO2 electrode the current efficiency for o-aminophenol was over 90%.
The precursor Ti(OEt)4 prepared by anodic dissolution of metallic titanium in absolute ethanol was directly hydrolyzed by a sol-gel process to give nano-TiO2 film on a titanium electrode(Ti/nano-TiO2). Redox behavior and electrocatalytic activity of the Ti/nano-TiO2 electrode was investigated by cyclic voltammetry, potential step chronoampermetry, and bulk electrolysis. The results indicated that there were two pairs of well defined redox peaks for Ti/nano-TiO2 film electrode in the 1 mol/L H2SO4 in correspondence with TiO2/Ti2O3 and TiO2/Ti(OH)3 reversible electrode processes with E1/2r being -0.56 V and -0.96 V(vs.SCE), respectively, at 0.1 V/s. Ti/nano-TiO2 electrode showed a high heterogeneous electrocatalytic activitiy in acidic medium in reduction of o-nitrophenol. The indirect electroreduction of o-nitrophenol to o-aminophenol by TiⅣ/TiⅢ redox pair on nano TiO2 film surface is believed to follow chemical catalysis mechanism(EC'). In preparative electrolysis at 50℃ on Ti/nano-TiO2 electrode the current efficiency for o-aminophenol was over 90%.
2004, 21(10): 1011-1015
Abstract:
The interaction of water soluble p-(N,N'-dimethylaminomethyl)calix\arene(CX8) with calf thymus DNA has been studied by UV-vis spectroscopy and fluorescence spectrophotometry using methylene blue(MB) as a probe. The effect of solution pH, ionic strength, common organic solvents and surfactants on the UV adsorption and fluorescence intensity were investigated. The results show that there is a strong electrostatic interaction between DNA and CX8. Scatchard curves indicated that the electrostatic interaction occurs between DNA and CX8, i.e. CX8 can compete for the electrostatic bonding sites of MB on DNA.
The interaction of water soluble p-(N,N'-dimethylaminomethyl)calix\arene(CX8) with calf thymus DNA has been studied by UV-vis spectroscopy and fluorescence spectrophotometry using methylene blue(MB) as a probe. The effect of solution pH, ionic strength, common organic solvents and surfactants on the UV adsorption and fluorescence intensity were investigated. The results show that there is a strong electrostatic interaction between DNA and CX8. Scatchard curves indicated that the electrostatic interaction occurs between DNA and CX8, i.e. CX8 can compete for the electrostatic bonding sites of MB on DNA.
2004, 21(10): 1016-1019
Abstract:
The carboxylated MWNT was dispersed in acetone and a drop of the suspension on GCE was dried to yield a multi-wall carbon nanotube modified glassy carbon electrode(MWNT/GCME). Vitamin B6 could be directly determined using the MWNT/GCME as working electorde by cyclic voltammetry in a buffer solution of NH4Cl-NH3·H2O(pH=8.0). The results showed that the peak current was proportional to the concentration of VB6 over the concentration range of 1.0×10-6 to 1.0×10-3 mol/L at the scan rate of 100 mV/s, and the detection limit was 1.0×10-6 mol/L with a correlation coeffecient of 0.998. Using this modified electrode, the VB6 content in a VB6 tablet was determined satisfactorily.
The carboxylated MWNT was dispersed in acetone and a drop of the suspension on GCE was dried to yield a multi-wall carbon nanotube modified glassy carbon electrode(MWNT/GCME). Vitamin B6 could be directly determined using the MWNT/GCME as working electorde by cyclic voltammetry in a buffer solution of NH4Cl-NH3·H2O(pH=8.0). The results showed that the peak current was proportional to the concentration of VB6 over the concentration range of 1.0×10-6 to 1.0×10-3 mol/L at the scan rate of 100 mV/s, and the detection limit was 1.0×10-6 mol/L with a correlation coeffecient of 0.998. Using this modified electrode, the VB6 content in a VB6 tablet was determined satisfactorily.
2004, 21(10): 1020-1023
Abstract:
A Cu(Ⅱ) mononuclear complex CuHL of asymmetrical double Schiff base(Where H3L is N-3-carboxylsalicylidene-N'-salicylaldehyde diaminoethane) and a Cu(Ⅱ)-Zn(Ⅱ)-Cu(Ⅱ) trinuclear complex have been synthesized and characterized by elemental analysis, IR and UV-vis. The crystal and molecular structure of the trinuclear complex was determined by X-ray diffractometry. The work confirms that the trinuclear complex belongs to triclinic system and P1 space group. The cell parameters are a=1.186 2(2) nm, b=1.544 0(3) nm, c=1.948 8(4) nm; α=90.04(3)°, β=97.86(3)°, γ=90.12(3)°; V=3.535 6(12) nm3, Z=1; R1=0.061 4, wR2=0.131 9。
A Cu(Ⅱ) mononuclear complex CuHL of asymmetrical double Schiff base(Where H3L is N-3-carboxylsalicylidene-N'-salicylaldehyde diaminoethane) and a Cu(Ⅱ)-Zn(Ⅱ)-Cu(Ⅱ) trinuclear complex have been synthesized and characterized by elemental analysis, IR and UV-vis. The crystal and molecular structure of the trinuclear complex was determined by X-ray diffractometry. The work confirms that the trinuclear complex belongs to triclinic system and P1 space group. The cell parameters are a=1.186 2(2) nm, b=1.544 0(3) nm, c=1.948 8(4) nm; α=90.04(3)°, β=97.86(3)°, γ=90.12(3)°; V=3.535 6(12) nm3, Z=1; R1=0.061 4, wR2=0.131 9。
2004, 21(10): 1024-1028
Abstract:
Five dendritic composite silica carriers were prepared and tested in immobilization of porcine pancreas lipase(PPL). The experimental results showed that the content of amino groups on the carrier surface, the chain length and the properties of organic groups have important influence on immobilization efficiency of PPL and the relative activity of immobilized lipase. Among all the carriers, 0.5G' composite carrier showed the best efficiency in immobilizing PPL mainly due to its highest content(1.646 mmol/g) of amino group on the surface. The activity of immobilized lipase is obviously raised with the increase of the organic chain length and the content of amino group (1.5G >0.5G;2.0G >1.0G). The activity of immobilized lipase improved by 35.4% and 13.1%, respectively, when the carriers 0.5G and 1.5G were modified by hydrolysis, indicating that the carboxyl groups on the surface of the carrier favor the immobilization of lipase to the ester groups. The lipase immobilized on 0.5G' composite carrier showed the best activity at 40℃ and in the buffer of pH 7.5. The immobilization conditions were optimized, and the best stirring time was 30 min, and the optimal mass ratio of carrier to lipase about 1 000:75.
Five dendritic composite silica carriers were prepared and tested in immobilization of porcine pancreas lipase(PPL). The experimental results showed that the content of amino groups on the carrier surface, the chain length and the properties of organic groups have important influence on immobilization efficiency of PPL and the relative activity of immobilized lipase. Among all the carriers, 0.5G' composite carrier showed the best efficiency in immobilizing PPL mainly due to its highest content(1.646 mmol/g) of amino group on the surface. The activity of immobilized lipase is obviously raised with the increase of the organic chain length and the content of amino group (1.5G >0.5G;2.0G >1.0G). The activity of immobilized lipase improved by 35.4% and 13.1%, respectively, when the carriers 0.5G and 1.5G were modified by hydrolysis, indicating that the carboxyl groups on the surface of the carrier favor the immobilization of lipase to the ester groups. The lipase immobilized on 0.5G' composite carrier showed the best activity at 40℃ and in the buffer of pH 7.5. The immobilization conditions were optimized, and the best stirring time was 30 min, and the optimal mass ratio of carrier to lipase about 1 000:75.
2004, 21(10): 1029-1033
Abstract:
The viscosity behavior of poly(dimethyldiallylammonium chloride)(PDMDAAC) in polyferric sulfate solutions(PFS) have been investigated as a function of interactions between PDMDAAC and PFS by FT-IR, SEM and X-ray diffractometry. The results show that the PDMDAAC chains adopt stretching conformation in PFS solution because of their special pyrrole ring structure and become larger in size due to stronger electrostatic repulsion of the polyferric cations. The viscosity behavior of PDMDAAC in PFS solution is less affected by the total iron concentration and basicity of the PFS solution, but affected by the concentration of PDMDAAC in PFS. The PDMDAAC chains present physical entanglement when the concentration of PDMDAAC is above 2.0 g/L, stretch in the concentration range of 0.8~2.0 g/L, and behave as a polyelectrolyte at below 0.8 g/L. The FT-IR, SEM and XRD results indicate that PDMDAAC interacted with the main phase Fe4.67(SO4)6(OH)2·20H2O of PFS.
The viscosity behavior of poly(dimethyldiallylammonium chloride)(PDMDAAC) in polyferric sulfate solutions(PFS) have been investigated as a function of interactions between PDMDAAC and PFS by FT-IR, SEM and X-ray diffractometry. The results show that the PDMDAAC chains adopt stretching conformation in PFS solution because of their special pyrrole ring structure and become larger in size due to stronger electrostatic repulsion of the polyferric cations. The viscosity behavior of PDMDAAC in PFS solution is less affected by the total iron concentration and basicity of the PFS solution, but affected by the concentration of PDMDAAC in PFS. The PDMDAAC chains present physical entanglement when the concentration of PDMDAAC is above 2.0 g/L, stretch in the concentration range of 0.8~2.0 g/L, and behave as a polyelectrolyte at below 0.8 g/L. The FT-IR, SEM and XRD results indicate that PDMDAAC interacted with the main phase Fe4.67(SO4)6(OH)2·20H2O of PFS.
2004, 21(10): 1034-1037
Abstract:
Starch nanoparticles have been prepared from epichlorohydrin cross-linked starch in W/O microemulsion of n-hexane, surfactant(Span-60) and aqueous starch. The morphology and size distribution of sphe-rical nanoparticles, investigated by TEM and dynamic light scattering(DLS), have been correlated with starch concentration. The results show that the starch nanoparticles were spherical and their radius increased and distribution became broader with the increase of starch concentration. The diameter of the nanoparticles ranged from 15.6 to 226 nm with an average of 92.2 nm. The diameter of 69% of the particles was less than 100 nm.
Starch nanoparticles have been prepared from epichlorohydrin cross-linked starch in W/O microemulsion of n-hexane, surfactant(Span-60) and aqueous starch. The morphology and size distribution of sphe-rical nanoparticles, investigated by TEM and dynamic light scattering(DLS), have been correlated with starch concentration. The results show that the starch nanoparticles were spherical and their radius increased and distribution became broader with the increase of starch concentration. The diameter of the nanoparticles ranged from 15.6 to 226 nm with an average of 92.2 nm. The diameter of 69% of the particles was less than 100 nm.
2004, 21(10): 1038-1041
Abstract:
An alkali-soluble terpolymer P(MMA/EA/MAA) was synthesized. The effect of terpolymer concentration, amount of MAA and dodecylmercaptan (DDM) and pH on the surface activity of the terpolymer solution were investigated. The results showed that the surface tension of the polymer solution decreased with increase in terpolymer concentration and the amount of DDM. The polymer solution showed a minimum surface tension value when the mass fraction of MAA was 25% or the pH of the solution was 7.5.
An alkali-soluble terpolymer P(MMA/EA/MAA) was synthesized. The effect of terpolymer concentration, amount of MAA and dodecylmercaptan (DDM) and pH on the surface activity of the terpolymer solution were investigated. The results showed that the surface tension of the polymer solution decreased with increase in terpolymer concentration and the amount of DDM. The polymer solution showed a minimum surface tension value when the mass fraction of MAA was 25% or the pH of the solution was 7.5.
2004, 21(10): 1042-1045
Abstract:
EVA/OMMT nanocomposites have been prepared by melt-blending. The intercalated structures of EVA/OMMT nanocomposites were characterized by XRD. The effect of the content of organic montmorillonite(OMMT) on the dynamic mechanical behavior of EVA/OMMT nanocomposites was studied by DMA, and the results showed that the storage modulus of EVA/OMMT nanocomposites increased with the content of OMMT. The thermal stability of the EVA in the nanocomposites was studied by TGA.
EVA/OMMT nanocomposites have been prepared by melt-blending. The intercalated structures of EVA/OMMT nanocomposites were characterized by XRD. The effect of the content of organic montmorillonite(OMMT) on the dynamic mechanical behavior of EVA/OMMT nanocomposites was studied by DMA, and the results showed that the storage modulus of EVA/OMMT nanocomposites increased with the content of OMMT. The thermal stability of the EVA in the nanocomposites was studied by TGA.
2004, 21(10): 1046-1050
Abstract:
Reaction of 5-chloro-2-hydroxybenzophenone(HCBP) with one amino group of 1,2-diaminobenzene gave a tridentate Schiff base ligand(HCBP PHEN). The free amino group in HCBP PHEN was then reacted with a series of α,ω-bis(3'-hydroxy 4'-formylphenyloxy)alkanes to yield the di-schiff base compounds(Bn). The compounds were characterized by elemental analysis, FT-IR, 1H NMR and UV-vis spectrophotometry. The spectral properties of the Bn have been discussed as a function of alkyl chain length, in comparison with that of the di-schiff base monomer(DT).
Reaction of 5-chloro-2-hydroxybenzophenone(HCBP) with one amino group of 1,2-diaminobenzene gave a tridentate Schiff base ligand(HCBP PHEN). The free amino group in HCBP PHEN was then reacted with a series of α,ω-bis(3'-hydroxy 4'-formylphenyloxy)alkanes to yield the di-schiff base compounds(Bn). The compounds were characterized by elemental analysis, FT-IR, 1H NMR and UV-vis spectrophotometry. The spectral properties of the Bn have been discussed as a function of alkyl chain length, in comparison with that of the di-schiff base monomer(DT).
2004, 21(10): 1051-1053
Abstract:
A novel poly(ether ether ketone) derived from 2-(6-oxide-6H-dibenz〈1,2>oxa phospho rin-6-yl)-1,4-dihydroxyphenylene, 4,4'-diflourodiphenylketone and bisphenol-A was synthesized by solution polycondensation. The influences of reaction time, and concentration of reactants on the polymerization were investigated. A copolymer with inherent viscosity of 1.44 was obtained. As characterized by FT-IR, 1H NMR and 31P NMR the product was a terpolymer, consisted of bisphenol A and difluorodiphenylketone. The DSC analysis show its Tg was 171℃. The copolymer was soluble in many polar solvents.
A novel poly(ether ether ketone) derived from 2-(6-oxide-6H-dibenz
2004, 21(10): 1054-1056
Abstract:
The nanoparticles of oxotitanium phthalocyanine(TiOPc) synthesized from titanium tetra-n-butoxide and 1,3-diiminoisoindole were prepared by liquid phase method using surfactant polyethylene glycol as a coating agent. The effects of surfactant type, content, preparation temperature and drying method were examined. When the mass ratio of polyethylene glycol to original TiOPc was 1:10, at ice bath temperature and by vacuum freeze drying method, TiOPc particles of 60 nm size were obtained. The product appeared to be an excellent photosensitive material with saturation potential of 540 V, residue potential of 20 V, half life of 0.2 s, and half discharge energy of 0.6l x·s.
The nanoparticles of oxotitanium phthalocyanine(TiOPc) synthesized from titanium tetra-n-butoxide and 1,3-diiminoisoindole were prepared by liquid phase method using surfactant polyethylene glycol as a coating agent. The effects of surfactant type, content, preparation temperature and drying method were examined. When the mass ratio of polyethylene glycol to original TiOPc was 1:10, at ice bath temperature and by vacuum freeze drying method, TiOPc particles of 60 nm size were obtained. The product appeared to be an excellent photosensitive material with saturation potential of 540 V, residue potential of 20 V, half life of 0.2 s, and half discharge energy of 0.6l x·s.
2004, 21(10): 1057-1059
Abstract:
Coupling water soluble and biodegradable poly(N-(2-hydroxyethyl)-L-glutamine)(PHEG) synthesized from poly((γ-benzyl)-L-glutamine) and 2-aminoethanol with 5-fluorouracil-1-acetic acid(FUA) as a simulated drug affords a polymer prodrug poly(N-(2-hydroxyethyl)-L-glutamine)-5-fluorouracil-1 acetic acid(PHEG-FUA). The conjugation between the polymer and the drug compound has been confirmed by IR, UV, 1H NMR and DSC. The content of 5 fluorouracil was determined to be about 26%(UV method). The in vitro test results show that the accumulated drug release amounts of PHEG FUA was 47.63% in phosphorus salt buffer solution (pH=7.2) during 120 h, indicating the conjugated compound has an obvious sustained release effect.
Coupling water soluble and biodegradable poly(N-(2-hydroxyethyl)-L-glutamine)(PHEG) synthesized from poly((γ-benzyl)-L-glutamine) and 2-aminoethanol with 5-fluorouracil-1-acetic acid(FUA) as a simulated drug affords a polymer prodrug poly(N-(2-hydroxyethyl)-L-glutamine)-5-fluorouracil-1 acetic acid(PHEG-FUA). The conjugation between the polymer and the drug compound has been confirmed by IR, UV, 1H NMR and DSC. The content of 5 fluorouracil was determined to be about 26%(UV method). The in vitro test results show that the accumulated drug release amounts of PHEG FUA was 47.63% in phosphorus salt buffer solution (pH=7.2) during 120 h, indicating the conjugated compound has an obvious sustained release effect.
2004, 21(10): 1060-1062
Abstract:
The complex[Nd(C4H3OCOO)2·NO3·C10H8N2]2 was synthesized from Nd(NO3)3·nH2O, 2-furancarboxylic acid(C4H3OCOOH), and 2,2'-bipyridine(C10H8N2]2). The unit cell is triclinic and of Pī symmetry. Unit cell parameters are:P1, a=0.992 18(17) nm, b=1.023 05(17) nm, c=1.114 4(3) nm, α=86.778(8)°, β=76.153(5)°, γ=70.363(14)°, M=584.58, V=1.037 3(4) nm3, Z=1, Dcalc=1.877 Mg/m3, T=293(2) K. The final R=0.061 8, wR=0.164 4. Each Nd3+ ion is coordinated by five O atoms of four furancarboxylate groups, two O atoms of nitrate and two N atoms of 2,2'-bipyridine molecule, with a coordination number of 9. The four carboxylate groups coordinate in two modes:bridging and bridging chelating. The two Nd3+ ions in the dimer are held together by four carboxylate groups of furancarboxylic acid.
The complex[Nd(C4H3OCOO)2·NO3·C10H8N2]2 was synthesized from Nd(NO3)3·nH2O, 2-furancarboxylic acid(C4H3OCOOH), and 2,2'-bipyridine(C10H8N2]2). The unit cell is triclinic and of Pī symmetry. Unit cell parameters are:P1, a=0.992 18(17) nm, b=1.023 05(17) nm, c=1.114 4(3) nm, α=86.778(8)°, β=76.153(5)°, γ=70.363(14)°, M=584.58, V=1.037 3(4) nm3, Z=1, Dcalc=1.877 Mg/m3, T=293(2) K. The final R=0.061 8, wR=0.164 4. Each Nd3+ ion is coordinated by five O atoms of four furancarboxylate groups, two O atoms of nitrate and two N atoms of 2,2'-bipyridine molecule, with a coordination number of 9. The four carboxylate groups coordinate in two modes:bridging and bridging chelating. The two Nd3+ ions in the dimer are held together by four carboxylate groups of furancarboxylic acid.
2004, 21(10): 1063-1065
Abstract:
Ozonization processes of 15-tetracosenoic acid methyl ester(TAE) and 9-octadecenoic acid methyl ester(OAE) obtained from Malania Oleifera Chum oil have been monitored by combined gas chromato graphy-mass spectrometry(GC-MS) or gas chromatography(GC). The effect of reaction temperature and solvent(heptane, toluene, n-butyl acetate, ethanol, and heptane-ethanol) on the ozonization selectivity of TAE and OAE were investigated. The results show that TAE has good selectivity in heptane because of its small dielectric constant. The kTAE/kOAE of the ozonization reaction decreased with the increase of ethanol in heptane-ethanol, whereas the ozonization selectivities of TAE and OAE reduced with the increase of the reaction temperature.
Ozonization processes of 15-tetracosenoic acid methyl ester(TAE) and 9-octadecenoic acid methyl ester(OAE) obtained from Malania Oleifera Chum oil have been monitored by combined gas chromato graphy-mass spectrometry(GC-MS) or gas chromatography(GC). The effect of reaction temperature and solvent(heptane, toluene, n-butyl acetate, ethanol, and heptane-ethanol) on the ozonization selectivity of TAE and OAE were investigated. The results show that TAE has good selectivity in heptane because of its small dielectric constant. The kTAE/kOAE of the ozonization reaction decreased with the increase of ethanol in heptane-ethanol, whereas the ozonization selectivities of TAE and OAE reduced with the increase of the reaction temperature.
2004, 21(10): 1066-1068
Abstract:
A series of calix[6]-1,4-crown-based polymers with stable conformations were synthesized by reacting calix[6]-1,4-crown tetraester with poly(ethyleneimine), and their adsorption capabilities were studied. Their structures and shapes were characterized by elemental analyses, IR and SEM techniques. Their adsorption selectivities were found to be higher than that of calix[6] arene polymer without stable conformation. All of them showed good selective adsorption capability towards Cu2+ among the tested cations. The adsorption capacity of compound 2a towards Cu2+ at concentration of 0.2 mmol/L were 64.5×10-5 mol/mg.
A series of calix[6]-1,4-crown-based polymers with stable conformations were synthesized by reacting calix[6]-1,4-crown tetraester with poly(ethyleneimine), and their adsorption capabilities were studied. Their structures and shapes were characterized by elemental analyses, IR and SEM techniques. Their adsorption selectivities were found to be higher than that of calix[6] arene polymer without stable conformation. All of them showed good selective adsorption capability towards Cu2+ among the tested cations. The adsorption capacity of compound 2a towards Cu2+ at concentration of 0.2 mmol/L were 64.5×10-5 mol/mg.
2004, 21(10): 1069-1071
Abstract:
5-Arylidene thiazolineone derivatives are synthesized by solid state condensation of aromatic aldehydes with 2,4-thiazolidinedione or N-phenylrhodanine in the presence of NaAc at 120~140℃ for 10 min with yields of 55%~81.2%. The effect of reaction conditions are discussed. This is a simple, time-saving and enviro nmental friendly method for the preparation of 5-arylidene thiazolineone derivatives.
5-Arylidene thiazolineone derivatives are synthesized by solid state condensation of aromatic aldehydes with 2,4-thiazolidinedione or N-phenylrhodanine in the presence of NaAc at 120~140℃ for 10 min with yields of 55%~81.2%. The effect of reaction conditions are discussed. This is a simple, time-saving and enviro nmental friendly method for the preparation of 5-arylidene thiazolineone derivatives.
2004, 21(10): 1072-1074
Abstract:
The used perfluorosulfonic acid ion-exchange membrane was treated to recycle the perfluorosulfonic acid resin. The perfluorosulfonic acid resin/silica composite catalysts were prepared by a sol-gel method and characterized by FTIR, TG, BETmeasurements. The composite catalysts obtained were used in esterification of HAc and butyl alcohol. The results showed that at n(HAc):n(butyl alcohol)=1.3:1.0, 3 g catalyst, 110℃ and 2 h, butyl acetate could be obtained in yield of 92.4%.
The used perfluorosulfonic acid ion-exchange membrane was treated to recycle the perfluorosulfonic acid resin. The perfluorosulfonic acid resin/silica composite catalysts were prepared by a sol-gel method and characterized by FTIR, TG, BETmeasurements. The composite catalysts obtained were used in esterification of HAc and butyl alcohol. The results showed that at n(HAc):n(butyl alcohol)=1.3:1.0, 3 g catalyst, 110℃ and 2 h, butyl acetate could be obtained in yield of 92.4%.
2004, 21(10): 1075-1077
Abstract:
2,6-Dihydroxy toluene was synthesized from resorcinol in 4 steps:alkylation, methylacylation, Huang Ming-Long reaction and dealkylation. In first two steps ethylene dichloride was used as the solvent. This made the two reactions easy and the yields high, and also decreased the amount of DMF used in second step. The third step was a modified Huang Ming-Long reaction carried out at more mild condition. The total yield of the title compound was 62%.
2,6-Dihydroxy toluene was synthesized from resorcinol in 4 steps:alkylation, methylacylation, Huang Ming-Long reaction and dealkylation. In first two steps ethylene dichloride was used as the solvent. This made the two reactions easy and the yields high, and also decreased the amount of DMF used in second step. The third step was a modified Huang Ming-Long reaction carried out at more mild condition. The total yield of the title compound was 62%.
2004, 21(10): 1078-1080
Abstract:
Polymerization of tetrahydrofuran(THF) initiated by phosphotungstic acid was carried out in the presence of epichlorohydrin(ECH). The effect of ECH content, reaction time, and water content on the polymerization have been studied. The result shows that water was the main factor influencing the yield and relative molecular weight of the polymer. Another factor was the reaction time. The ECH content mainly affects the rate of the reaction. The light irradiation mainly affects the color of the polymer. Polytetrfuran with relative molecular weight of 2 000 was obtained in yield of 73.6% at reaction condition of 0℃, 4 h, n(H2O):n(PWA)=16.2:1.
Polymerization of tetrahydrofuran(THF) initiated by phosphotungstic acid was carried out in the presence of epichlorohydrin(ECH). The effect of ECH content, reaction time, and water content on the polymerization have been studied. The result shows that water was the main factor influencing the yield and relative molecular weight of the polymer. Another factor was the reaction time. The ECH content mainly affects the rate of the reaction. The light irradiation mainly affects the color of the polymer. Polytetrfuran with relative molecular weight of 2 000 was obtained in yield of 73.6% at reaction condition of 0℃, 4 h, n(H2O):n(PWA)=16.2:1.
