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2002 Volume 19 Issue 6
2002, 19(6): 511-516
Abstract:
The recent active researches of the grafting of organic monolayers through Si-C bond on the H-terminated silicon surfaces are summarized, showing the potential applications in microelectronics, chemical/biochemical sensors, nanometer techniques and solar energy, etc.
The recent active researches of the grafting of organic monolayers through Si-C bond on the H-terminated silicon surfaces are summarized, showing the potential applications in microelectronics, chemical/biochemical sensors, nanometer techniques and solar energy, etc.
2002, 19(6): 517-520
Abstract:
The extraction equilibrium experiments for benzoic acid in dilute solution were carried out using tributyl phosphate(TBP) in kerosene, n-octanol, n-butanol, hexane, heptane, benzene and MIBK as extractants. The extraction equilibrium equations have been deducted and the apparent extraction equilibrium constants were obtained by the regression of the experimental data. The results showed that the distribution coefficient(D) of benzoic acid depended on the polarity of the solvent in the order of n-octanol > n-butanol > MIBK > benzene > hexane(heptane). The stronger the polarity, the larger the distribution coefficient. The extractability of n-octanol was equivalent to that of 30% TBP-kerosene, and n-octanol is a promising extractant for commercial use.
The extraction equilibrium experiments for benzoic acid in dilute solution were carried out using tributyl phosphate(TBP) in kerosene, n-octanol, n-butanol, hexane, heptane, benzene and MIBK as extractants. The extraction equilibrium equations have been deducted and the apparent extraction equilibrium constants were obtained by the regression of the experimental data. The results showed that the distribution coefficient(D) of benzoic acid depended on the polarity of the solvent in the order of n-octanol > n-butanol > MIBK > benzene > hexane(heptane). The stronger the polarity, the larger the distribution coefficient. The extractability of n-octanol was equivalent to that of 30% TBP-kerosene, and n-octanol is a promising extractant for commercial use.
2002, 19(6): 521-526
Abstract:
Ten 5-O-triphenylsilyl 4"-O-carbonyl Avermectin B1a were prepared by esterification reaction of 5-O-triphenylsilyl Avermectin B1a with corresponding carboxylic acids in the systems of 1,3-dicyclohexylcarbodiimide (DCC)/4-dimethylaminopyridine(DMAP) in good yield(55%~76%). Their chemical structures were confirmed by IR, 1H NMR, 13C NMR and MS. The preliminary bioa-ssay results showed that some of the title compounds have good insecticidal activities against Aphis gossypii Glover and Tetranychus truncatus Ehara.
Ten 5-O-triphenylsilyl 4"-O-carbonyl Avermectin B1a were prepared by esterification reaction of 5-O-triphenylsilyl Avermectin B1a with corresponding carboxylic acids in the systems of 1,3-dicyclohexylcarbodiimide (DCC)/4-dimethylaminopyridine(DMAP) in good yield(55%~76%). Their chemical structures were confirmed by IR, 1H NMR, 13C NMR and MS. The preliminary bioa-ssay results showed that some of the title compounds have good insecticidal activities against Aphis gossypii Glover and Tetranychus truncatus Ehara.
2002, 19(6): 527-530
Abstract:
A series of the title compounds 5 were synthesized by reduction of compound 4 by using NaBH4. The later were obtained by 1,4-nucleophilic addition of 1,3-diaryl-2-[(1H-1,2,4-triazol-1-yl)methyl]-2-propen-1-one 7 with substituted thiophenol. The structures of compounds 5 were characterized by elemental analysis, 1H NMR and IR spectral measurements. Most of compounds 5 were found to have weak fungicidal activities against Puccinia recondita for wheat.
A series of the title compounds 5 were synthesized by reduction of compound 4 by using NaBH4. The later were obtained by 1,4-nucleophilic addition of 1,3-diaryl-2-[(1H-1,2,4-triazol-1-yl)methyl]-2-propen-1-one 7 with substituted thiophenol. The structures of compounds 5 were characterized by elemental analysis, 1H NMR and IR spectral measurements. Most of compounds 5 were found to have weak fungicidal activities against Puccinia recondita for wheat.
2002, 19(6): 531-534
Abstract:
A sol-gel method was developed for the preparation of SrBi2Ta2O9(SBT) ferroelectric ceramic thin films using soluble inorganic salts Sr(NO3)2、Bi(NO3)3 and HTaF6 in the presence of citric acid, EDTA and ethylene glycol as organic coordina-tion agents. The results showed that the coordination agents in the precursor solution are an important factor affecting the stability of sol and formation of SBT phase. The solution coordinated with EDTA and glycol could form a stable and homogeneous sol and produce a single SBT phase thin films by spin coat approach on Al2O3 substrate. The effects of volatility of Bi2O3 at high temperature and the annealing temperatures of the films on the preparation were also discussed. A smooth, well crystallized, stoichiometric SrBi2Ta2O9 ferroelectric thin film with uniform crystallite size could be obtained on Al2O3 substrate at calcining temperature of 700℃ in an oxygen atmosphere from the Bi being feeded in excess of 40%.
A sol-gel method was developed for the preparation of SrBi2Ta2O9(SBT) ferroelectric ceramic thin films using soluble inorganic salts Sr(NO3)2、Bi(NO3)3 and HTaF6 in the presence of citric acid, EDTA and ethylene glycol as organic coordina-tion agents. The results showed that the coordination agents in the precursor solution are an important factor affecting the stability of sol and formation of SBT phase. The solution coordinated with EDTA and glycol could form a stable and homogeneous sol and produce a single SBT phase thin films by spin coat approach on Al2O3 substrate. The effects of volatility of Bi2O3 at high temperature and the annealing temperatures of the films on the preparation were also discussed. A smooth, well crystallized, stoichiometric SrBi2Ta2O9 ferroelectric thin film with uniform crystallite size could be obtained on Al2O3 substrate at calcining temperature of 700℃ in an oxygen atmosphere from the Bi being feeded in excess of 40%.
2002, 19(6): 535-538
Abstract:
The corrosion inhibition action of benzotriazole(BTA), 2-mercapto benzoxazole(MBO) and 2-mercapto benzimidazole(MBI) for copper in 0.5 mol/L HCl solution was investigated by potentiodynamic polarization and impedance spectroscopy. Coupon tests showed that the best inhibition efficiency was 91.6% by using MBI in concentration of ca. 10-3 mol/L. The molecular structure parameters of BTA, MBO and MBI were obtained via MM2 forcefield program and PPP-SCF quantum chemical calculation, which indicated that MBI has the higher HOMO and LUMO energy, as well as larger c electron density.
The corrosion inhibition action of benzotriazole(BTA), 2-mercapto benzoxazole(MBO) and 2-mercapto benzimidazole(MBI) for copper in 0.5 mol/L HCl solution was investigated by potentiodynamic polarization and impedance spectroscopy. Coupon tests showed that the best inhibition efficiency was 91.6% by using MBI in concentration of ca. 10-3 mol/L. The molecular structure parameters of BTA, MBO and MBI were obtained via MM2 forcefield program and PPP-SCF quantum chemical calculation, which indicated that MBI has the higher HOMO and LUMO energy, as well as larger c electron density.
2002, 19(6): 539-543
Abstract:
The factors influenting the formation of organic monolayers derived by alkenes on hydrogen-termined silicon(111) and the passivation of the monolayer covered surface toward oxidation have been investigated preliminarily by using interfacial differential capacity analysis. The results demonstrated that the both reaction conditions and reactivity of the grafting molecules could affect the quality of the monolayers. In the conditions selected where the volume fraction of the grafted molecules was about 90% on the surface modified by alkenes, only limited passivation of monolayers toward oxidation was observed. The parameters of capacity properties of the organic monolayers formed with a series of alkene molecules on silicon(111) surface were also meassured.
The factors influenting the formation of organic monolayers derived by alkenes on hydrogen-termined silicon(111) and the passivation of the monolayer covered surface toward oxidation have been investigated preliminarily by using interfacial differential capacity analysis. The results demonstrated that the both reaction conditions and reactivity of the grafting molecules could affect the quality of the monolayers. In the conditions selected where the volume fraction of the grafted molecules was about 90% on the surface modified by alkenes, only limited passivation of monolayers toward oxidation was observed. The parameters of capacity properties of the organic monolayers formed with a series of alkene molecules on silicon(111) surface were also meassured.
2002, 19(6): 544-547
Abstract:
Tung oil prepolymer was prepared by mixing tung oil with anhydrous aluminum chloride at 230℃ for 1 h. Asphalt was modified by tung oil perpolymer through mixing at 240℃ until no 993 cm-1 band was observed. Intrinsic viscosity number [Z] measurement and TLC were used to monitor the prepolymerization reaction. The results showed that the prepolymer react mainly with the colloid and asphaltene compositions of asphalt. Part of the modified asphalt acts as an interfacial agent which is in favor of the compatibility of the mixture. The copolymer of asphaltene/tung oil prepolymer could not only reduce the asphaltene's rigidity and incompatibility, but also stabilize the colloid part of asphalt improving its penetration and low temperature ductility. A good result was obtained by adding 3%~6%(mass fraction) tung oil prepolymer into the asphalt.
Tung oil prepolymer was prepared by mixing tung oil with anhydrous aluminum chloride at 230℃ for 1 h. Asphalt was modified by tung oil perpolymer through mixing at 240℃ until no 993 cm-1 band was observed. Intrinsic viscosity number [Z] measurement and TLC were used to monitor the prepolymerization reaction. The results showed that the prepolymer react mainly with the colloid and asphaltene compositions of asphalt. Part of the modified asphalt acts as an interfacial agent which is in favor of the compatibility of the mixture. The copolymer of asphaltene/tung oil prepolymer could not only reduce the asphaltene's rigidity and incompatibility, but also stabilize the colloid part of asphalt improving its penetration and low temperature ductility. A good result was obtained by adding 3%~6%(mass fraction) tung oil prepolymer into the asphalt.
2002, 19(6): 548-551
Abstract:
Polymercaptoaniline electrode material was synthesized. Its physical and chemical properties were characterized and analyzed with granularity, specific area, UV, SEM and charge discharge test. The experiments show that when used as positive electrode in lithium battery, the polymer material has first discharge capacity of 155 mA·h/g; after activation its discharge capacity reaches about 180 mA·h/g.
Polymercaptoaniline electrode material was synthesized. Its physical and chemical properties were characterized and analyzed with granularity, specific area, UV, SEM and charge discharge test. The experiments show that when used as positive electrode in lithium battery, the polymer material has first discharge capacity of 155 mA·h/g; after activation its discharge capacity reaches about 180 mA·h/g.
2002, 19(6): 552-555
Abstract:
Antimony doped tin dioxide(ATO) nanoparticles prepared by heterogeneous precipitation have been investigated as funcion of grain size, cell volume and electrical property in relation to Sb doped level and calcination temperature. It is found that the crystal grows up in two steps. The activation energies of crystal growth were calculated to be 21.94 and 4.52 kJ/mol, respectively.
Antimony doped tin dioxide(ATO) nanoparticles prepared by heterogeneous precipitation have been investigated as funcion of grain size, cell volume and electrical property in relation to Sb doped level and calcination temperature. It is found that the crystal grows up in two steps. The activation energies of crystal growth were calculated to be 21.94 and 4.52 kJ/mol, respectively.
2002, 19(6): 556-559
Abstract:
A novel aromatic diamine 2-(4-aminophenyl)-4-(3-chloro 4 amimo phenoxybenzene)-2,3-phthalazinone-1(1) containing aza hetero-cycle was synthesized from 4-(3-chloro-4-hydroxyphenyl)-2,3-phthalazinone-1(OC-HPPZ) and used to prepare a new class of aromatic polyamides from various arylene dicarboxylic acids using Yamazaki method via direct polycondensation. The structure of diamine monomer and polymers was characterized by MS、FTIR and 1H NMR. The polyamides obtained had high molecular weight with the inherent viscosity of 0.60~0.76 dL/g, glass transition temperature of 298.6~320.3℃ and 10% mass loss over 447℃ under N2. The polymers were readily soluble in polar solvents such as NMP、DMF and m-cresol. Clear, tough films can be obtained from their DMAc solution by casting.
A novel aromatic diamine 2-(4-aminophenyl)-4-(3-chloro 4 amimo phenoxybenzene)-2,3-phthalazinone-1(1) containing aza hetero-cycle was synthesized from 4-(3-chloro-4-hydroxyphenyl)-2,3-phthalazinone-1(OC-HPPZ) and used to prepare a new class of aromatic polyamides from various arylene dicarboxylic acids using Yamazaki method via direct polycondensation. The structure of diamine monomer and polymers was characterized by MS、FTIR and 1H NMR. The polyamides obtained had high molecular weight with the inherent viscosity of 0.60~0.76 dL/g, glass transition temperature of 298.6~320.3℃ and 10% mass loss over 447℃ under N2. The polymers were readily soluble in polar solvents such as NMP、DMF and m-cresol. Clear, tough films can be obtained from their DMAc solution by casting.
2002, 19(6): 560-563
Abstract:
The influences of plasticizers EC(ethylene carbonate), DME(dimethoxy ethane), DEC(diethyl-carbonate), EMC(methyl ethyl carbonate) and PC(propylene carbonate) in various combination on the conductivity and performance of gelled polymer electrolytes at different temperatures have been investigated as functions of charge-discharge properties of LiCoO2 and graphitized carbon fiber. The highest conductivity of gel polymer electrolyte was obtained with plasticizers EC-DME as 0.188 S/m at room temperature. The first discharge specific capacity of LiCoO2 with combination plasticizer was about 145 mA·h/g, and the effect of plasticizer is not obvious. The discharge specific capacity of graphitized carbon fiber in EC DEC EMC was 300 mA·h/g, with the initial coulomb efficiency being about 95%.
The influences of plasticizers EC(ethylene carbonate), DME(dimethoxy ethane), DEC(diethyl-carbonate), EMC(methyl ethyl carbonate) and PC(propylene carbonate) in various combination on the conductivity and performance of gelled polymer electrolytes at different temperatures have been investigated as functions of charge-discharge properties of LiCoO2 and graphitized carbon fiber. The highest conductivity of gel polymer electrolyte was obtained with plasticizers EC-DME as 0.188 S/m at room temperature. The first discharge specific capacity of LiCoO2 with combination plasticizer was about 145 mA·h/g, and the effect of plasticizer is not obvious. The discharge specific capacity of graphitized carbon fiber in EC DEC EMC was 300 mA·h/g, with the initial coulomb efficiency being about 95%.
2002, 19(6): 564-568
Abstract:
By electrolyzing iron net anode in 14 mol/L NaOH solution in a diaphragm electrolyzer with anodic chamber gap of 15 to 22 mm, Na2FeO4 in concentration of 0.23 to 0.32 mol/L could be obtained when the apparent anodic current density was of 160 to 280 A/m2 and the electrolysis time for 5~6 hours. Adding the Na2FeO4 and KOH solutions alternately to the reactor at 20℃ and the reaction time of 30 min, the solid K2FeO4 with purity over 95% could be obtained after precipitation, washing and drying. It is found that the dissolution of K2FeO4 in solutions of KOH, NaOH and in their mixture was affected by common ion effect as well as strong salting-out effect. The reduction rate of soild K2FeO4 by methanol was proportional to the content of water in methanol solution.
By electrolyzing iron net anode in 14 mol/L NaOH solution in a diaphragm electrolyzer with anodic chamber gap of 15 to 22 mm, Na2FeO4 in concentration of 0.23 to 0.32 mol/L could be obtained when the apparent anodic current density was of 160 to 280 A/m2 and the electrolysis time for 5~6 hours. Adding the Na2FeO4 and KOH solutions alternately to the reactor at 20℃ and the reaction time of 30 min, the solid K2FeO4 with purity over 95% could be obtained after precipitation, washing and drying. It is found that the dissolution of K2FeO4 in solutions of KOH, NaOH and in their mixture was affected by common ion effect as well as strong salting-out effect. The reduction rate of soild K2FeO4 by methanol was proportional to the content of water in methanol solution.
2002, 19(6): 569-573
Abstract:
The acrylate copolymer latexes modified with organosilicone were prepared by seeding emulsion copolymerization in the presence of peroxide and complex redox initial system. When m(MMA):m(BA)=55:43, k(Si)=8%~16%,K(emulsifier)=4% and k(initiater)=0.5% an emulsion of good property for coatings could be obtained. The structures of copolymers characterized by FTIR and DSC showed that it is a copolymeration between organosilicone and acrylates, neither hydrolyzation nor condensation occurred in latexes.
The acrylate copolymer latexes modified with organosilicone were prepared by seeding emulsion copolymerization in the presence of peroxide and complex redox initial system. When m(MMA):m(BA)=55:43, k(Si)=8%~16%,K(emulsifier)=4% and k(initiater)=0.5% an emulsion of good property for coatings could be obtained. The structures of copolymers characterized by FTIR and DSC showed that it is a copolymeration between organosilicone and acrylates, neither hydrolyzation nor condensation occurred in latexes.
2002, 19(6): 574-577
Abstract:
The influence of Bi3+ ions in sulfuric acid electrolyte on the cathode behavior of lead-acid battery has been investigated by cyclic voltammetry(CV), cathodic polarization and electrochemical impedance spectroscopy(EIS). The results demonstrated that bismuth ion can be deposited on the cathode surface in the course of charging, resulting in the decrease of both cathode hydrogen overpotential and discharge capacity. The deposition of bismuth ions due to ion displacement may also lead to a quick formation of PbSO4 film on the electrode surface. The thickened PbSO4 film might retard the migration of H+ and HSO4- ions, decreasing the self-discharge of battery at open potential.
The influence of Bi3+ ions in sulfuric acid electrolyte on the cathode behavior of lead-acid battery has been investigated by cyclic voltammetry(CV), cathodic polarization and electrochemical impedance spectroscopy(EIS). The results demonstrated that bismuth ion can be deposited on the cathode surface in the course of charging, resulting in the decrease of both cathode hydrogen overpotential and discharge capacity. The deposition of bismuth ions due to ion displacement may also lead to a quick formation of PbSO4 film on the electrode surface. The thickened PbSO4 film might retard the migration of H+ and HSO4- ions, decreasing the self-discharge of battery at open potential.
2002, 19(6): 578-581
Abstract:
The distribution behavior of haloid complexes of gold(Ⅲ) in the polyethylene glycol ammonium sulphate aqueous biphasic system have been investigated as function of the concentration of acids and ammonium sulphate and the kind of salts. The distribution ratio order of the three haloid complexes was found to be: DAu(AuI4-) > DAu(AuBr4-) > DAu(AuCl4-). The extraction mechanism for gold(Ⅲ) was discussed based on the results of such as UV and IR spectra measurements.
The distribution behavior of haloid complexes of gold(Ⅲ) in the polyethylene glycol ammonium sulphate aqueous biphasic system have been investigated as function of the concentration of acids and ammonium sulphate and the kind of salts. The distribution ratio order of the three haloid complexes was found to be: DAu(AuI4-) > DAu(AuBr4-) > DAu(AuCl4-). The extraction mechanism for gold(Ⅲ) was discussed based on the results of such as UV and IR spectra measurements.
2002, 19(6): 582-584
Abstract:
5-Bromo-6-methoxy-2-propionylnaphthalene(1) was hydrodebrominate by bubbling of H2 in solution of i-PrOH and 20% KOH(aq) at 60℃, using 10% Pd/C as catalyst in the presence of cation surfactant CTAB to give 6-methoxy-2-propionylnaphthalene(2).
5-Bromo-6-methoxy-2-propionylnaphthalene(1) was hydrodebrominate by bubbling of H2 in solution of i-PrOH and 20% KOH(aq) at 60℃, using 10% Pd/C as catalyst in the presence of cation surfactant CTAB to give 6-methoxy-2-propionylnaphthalene(2).
2002, 19(6): 585-587
Abstract:
Capillary zone electrophoresis(CZE) has been performed for determination of resveratrol in Rhizoma Polygoni Cuspidati in a non aqueous solution of tris(hydroxymethyl) aminomethane(THAM) and boric acid with methanol as solvent. The effects of solvent, electrolyte, pH, concentration, running time and voltage were examined. The total separation and determination could be completed within 11 min. Under the optimum conditions, the linear range of trans-resveratrol was 27~540 mg/L. The RSD(n=6) of peak area for resveratrol was 2.46% and the recovery was 103.4%.
Capillary zone electrophoresis(CZE) has been performed for determination of resveratrol in Rhizoma Polygoni Cuspidati in a non aqueous solution of tris(hydroxymethyl) aminomethane(THAM) and boric acid with methanol as solvent. The effects of solvent, electrolyte, pH, concentration, running time and voltage were examined. The total separation and determination could be completed within 11 min. Under the optimum conditions, the linear range of trans-resveratrol was 27~540 mg/L. The RSD(n=6) of peak area for resveratrol was 2.46% and the recovery was 103.4%.
2002, 19(6): 588-590
Abstract:
Co-U zeolites have been synthesized by hydrothermal method. The influence of synthesis conditions on the crystallization of Co-U zeolites has been investigated. The Si/Co ratios and structure of the products have been characterized by means of chemical analysis, XRD, IR, DTA, TEM, ICP and UV-vis diffuse reflectance spectra. The results show that the particles of Co-U zeolites are well distributed. The unit cell parameters of the resulting Co-U zealites are changed as compared with Al-U zeolite due to the presence of Co in the framework of zeolite.
Co-U zeolites have been synthesized by hydrothermal method. The influence of synthesis conditions on the crystallization of Co-U zeolites has been investigated. The Si/Co ratios and structure of the products have been characterized by means of chemical analysis, XRD, IR, DTA, TEM, ICP and UV-vis diffuse reflectance spectra. The results show that the particles of Co-U zeolites are well distributed. The unit cell parameters of the resulting Co-U zealites are changed as compared with Al-U zeolite due to the presence of Co in the framework of zeolite.
2002, 19(6): 591-593
Abstract:
Polyether ketone ether ketone ketones containing naphthalene ring were synthesized by low temperature solution polycondensation of 4,4'-bis(T-naphthoxy)benzophenone(DNBP), terephthaloyl chloride(TPC) and isophthaloyl chloride(IPC) in 1,2-dichloroethane and in the presence of AlCl3 and NMP. The polymers obtained were characterized by IR, DSC, TG, and WAXD methods. The results show that the polymers are non crystalline, soluble in NMP, DMF, and 1,2-dichloroethane(DCE), and have high glass transition temperature and good heat resistance.
Polyether ketone ether ketone ketones containing naphthalene ring were synthesized by low temperature solution polycondensation of 4,4'-bis(T-naphthoxy)benzophenone(DNBP), terephthaloyl chloride(TPC) and isophthaloyl chloride(IPC) in 1,2-dichloroethane and in the presence of AlCl3 and NMP. The polymers obtained were characterized by IR, DSC, TG, and WAXD methods. The results show that the polymers are non crystalline, soluble in NMP, DMF, and 1,2-dichloroethane(DCE), and have high glass transition temperature and good heat resistance.
2002, 19(6): 594-596
Abstract:
The halogen substituted anthranilic acid(1) was condensed with acetic anhydride to give halogen substituted-3-methyl-1H-2,4-benoxazin-1-one(2), which was further condensed with hydrazide (3) to give twelve novel halogen substituted-2-(3-methyl-5-substitued-4H-1,2,4-triazol-4-yl) benzoic acid. All compounds synthesized were identified by 1H NMR and elemental analyses.
The halogen substituted anthranilic acid(1) was condensed with acetic anhydride to give halogen substituted-3-methyl-1H-2,4-benoxazin-1-one(2), which was further condensed with hydrazide (3) to give twelve novel halogen substituted-2-(3-methyl-5-substitued-4H-1,2,4-triazol-4-yl) benzoic acid. All compounds synthesized were identified by 1H NMR and elemental analyses.
2002, 19(6): 597-599
Abstract:
The medical grade poly(vinylmethyl siloxane)(PVMS) and silica filled PVMS were crosslinked with benzoyl peroxide(BPO). The glass transition of the crosslinked silicone rubber was evaluated by measurment of thermally stimulated current(TSC). The releasing rate of 1-norgestrel(LNG) through the membrane of the vulcanized silicone rubber in saturated physiological salt solution and that from the intrauterine device(IUD) were determined. The results showed that the drug deli very behavour was influenced by the structure of PVMS molecules which were controlled by the content of BPO and silica used in vulcanization of PVMS. The burst effect at first stage of drug delivery was observed probably due to the interaction between LNG and macromolecules. The releasing curve of LNG from IUD could be kept constant for period of half a year.
The medical grade poly(vinylmethyl siloxane)(PVMS) and silica filled PVMS were crosslinked with benzoyl peroxide(BPO). The glass transition of the crosslinked silicone rubber was evaluated by measurment of thermally stimulated current(TSC). The releasing rate of 1-norgestrel(LNG) through the membrane of the vulcanized silicone rubber in saturated physiological salt solution and that from the intrauterine device(IUD) were determined. The results showed that the drug deli very behavour was influenced by the structure of PVMS molecules which were controlled by the content of BPO and silica used in vulcanization of PVMS. The burst effect at first stage of drug delivery was observed probably due to the interaction between LNG and macromolecules. The releasing curve of LNG from IUD could be kept constant for period of half a year.
2002, 19(6): 600-602
Abstract:
Solanesyl bromide(Ⅱ) was reacted with diethanolamine to give solanesyl diethanolamine(Ⅲ) which was acylated with 3,4,5-trimethoxybenzoyl chloride, acetic anhydride, benzoyl chloride and cinnamyl chloride to give i>N,N-di[(3,4,5 trimethoxybenzoyloxy)ethyl]solanesylamine(Ⅳ), N,N-di[(acetyloxy)ethyl] solanesylamine(Ⅴ), i>N,N-di[(benzoyloxy)ethyl]solanesylamine(Ⅵ), i>N,N-di[(cinnyloxy)ethyl]solanesylamine(Ⅶ) respectively. The structures of compounds Ⅲ~Ⅶ were confirmed by IR, 1H NMR, MS and elemental analysis.
Solanesyl bromide(Ⅱ) was reacted with diethanolamine to give solanesyl diethanolamine(Ⅲ) which was acylated with 3,4,5-trimethoxybenzoyl chloride, acetic anhydride, benzoyl chloride and cinnamyl chloride to give i>N,N-di[(3,4,5 trimethoxybenzoyloxy)ethyl]solanesylamine(Ⅳ), N,N-di[(acetyloxy)ethyl] solanesylamine(Ⅴ), i>N,N-di[(benzoyloxy)ethyl]solanesylamine(Ⅵ), i>N,N-di[(cinnyloxy)ethyl]solanesylamine(Ⅶ) respectively. The structures of compounds Ⅲ~Ⅶ were confirmed by IR, 1H NMR, MS and elemental analysis.
2002, 19(6): 603-605
Abstract:
Three tetraacetyl glucosyl esters of the ferrocenyl benzoic acids(compounds Ⅱ o,Ⅱ m,Ⅱ p) have been synthesized using a phase transfer catalyst(CTAB) in dichloroethane/water at 50℃. Their structures have been confirmed by elemental analysis, IR, 1H NMR and MS. The compounds were found to have antianemic activity. The RBC and HB values of the tested anemic rats were increased by 72 0% and 126 4%, respectively after abdomen injection.
Three tetraacetyl glucosyl esters of the ferrocenyl benzoic acids(compounds Ⅱ o,Ⅱ m,Ⅱ p) have been synthesized using a phase transfer catalyst(CTAB) in dichloroethane/water at 50℃. Their structures have been confirmed by elemental analysis, IR, 1H NMR and MS. The compounds were found to have antianemic activity. The RBC and HB values of the tested anemic rats were increased by 72 0% and 126 4%, respectively after abdomen injection.
2002, 19(6): 606-608
Abstract:
The monodispersed copolymer microspheres were prepared by soap-free emulsion copolymerization from methyl methacrylate(MMA), butyl acrylate(BA) and acrylic acid(AA). The microspheres have an average diameter dp=1.10 μm and monodispersity Cv=2.02%. The monodispersed core-shell copolymer microspheres having average diameter dp1.14 μm and Cv 1.18% were then prepared by seeding polymerization. It is confirmed from the number of seed microspheres and core-shell microspheres that the polymerization of shell monomers was carried out only on the seed microspheres.
The monodispersed copolymer microspheres were prepared by soap-free emulsion copolymerization from methyl methacrylate(MMA), butyl acrylate(BA) and acrylic acid(AA). The microspheres have an average diameter dp=1.10 μm and monodispersity Cv=2.02%. The monodispersed core-shell copolymer microspheres having average diameter dp1.14 μm and Cv 1.18% were then prepared by seeding polymerization. It is confirmed from the number of seed microspheres and core-shell microspheres that the polymerization of shell monomers was carried out only on the seed microspheres.
2002, 19(6): 609-610
Abstract:
Using triethylamine as a catalyst, two polyacrylates containing both acid anhydride and hydroxylic groups were prepared and could be cured with each other under ambient condition to give a coating with good performances. The crosslinking degree of the cured coating amounts to 77% at the catalyst mass fraction higher than 3.6%. With increasing the catalyst mass fraction from 3.6% to 5.4%, the hardness, flexibility and adhesion of the coating were all improved accordingly.
Using triethylamine as a catalyst, two polyacrylates containing both acid anhydride and hydroxylic groups were prepared and could be cured with each other under ambient condition to give a coating with good performances. The crosslinking degree of the cured coating amounts to 77% at the catalyst mass fraction higher than 3.6%. With increasing the catalyst mass fraction from 3.6% to 5.4%, the hardness, flexibility and adhesion of the coating were all improved accordingly.
2002, 19(6): 611-612
Abstract:
[Ga3(PO4)4]-(H3NCH2CH2)2NH2(abbr. to GaP-1) has been synthesized by a hydrothermal method. X ray crystal structure analysis indicates GaP-1 crystallizes in monoclinic, with space group C2/c, a=2.079 3(5) nm, b=1.194 2(2) nm, c=1.648 0(4) nm, U=117.064(14)°, V=3.644 2(13) nm3, Z=6, Dc=1.901 g/cm3, I≥2e(I)=2 274, R=0.055 6, Rw=0.134 8. GaP-1 is characteristic of the intercalation of disordered fully protonated diethylenetriamine among two dimensional inorganic framework built up from PO4, GaO5 and GaO6 primary structure units. The framework features 3-, 4-, 5-and 8-ring topological connectivity.
[Ga3(PO4)4]-(H3NCH2CH2)2NH2(abbr. to GaP-1) has been synthesized by a hydrothermal method. X ray crystal structure analysis indicates GaP-1 crystallizes in monoclinic, with space group C2/c, a=2.079 3(5) nm, b=1.194 2(2) nm, c=1.648 0(4) nm, U=117.064(14)°, V=3.644 2(13) nm3, Z=6, Dc=1.901 g/cm3, I≥2e(I)=2 274, R=0.055 6, Rw=0.134 8. GaP-1 is characteristic of the intercalation of disordered fully protonated diethylenetriamine among two dimensional inorganic framework built up from PO4, GaO5 and GaO6 primary structure units. The framework features 3-, 4-, 5-and 8-ring topological connectivity.
