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2000 Volume 17 Issue 5
2000, 17(5): 465-470
Abstract:
A series of strong solid-acid catalysts Zr(SO4)2 calcined at different temperatures and supported Zr(SO4)2/Al2O3(or SiO2) were prepared. The effects of supporter and calcination temperature on the crystal form, structure, specific surface, acid content and acid strength of the catalysts were investigated by XRD, IR, BET, specific surface, TG-DTA, NH3-TPD and the Hammett indicator measurements. The results showed that as a supporter Al2O3 could obviously retard the decomposition of Zr(SO4)2, crystal phase transform of ZrO2 and considerably increase the acid content and acid strength of the catalysts. In the alkylation of isobutane with butenes the Zr(SO4)2 catalyst samples calcined at 913 and 1023 K showed the best activity and for supported catalyst Zr(SO4)2/Al2O3 the best activity was achieved when m (Zr(SO4)2)/m(Al2O3)=0.5~1.0. All of the catalysts revealed good selectivity for C80.
A series of strong solid-acid catalysts Zr(SO4)2 calcined at different temperatures and supported Zr(SO4)2/Al2O3(or SiO2) were prepared. The effects of supporter and calcination temperature on the crystal form, structure, specific surface, acid content and acid strength of the catalysts were investigated by XRD, IR, BET, specific surface, TG-DTA, NH3-TPD and the Hammett indicator measurements. The results showed that as a supporter Al2O3 could obviously retard the decomposition of Zr(SO4)2, crystal phase transform of ZrO2 and considerably increase the acid content and acid strength of the catalysts. In the alkylation of isobutane with butenes the Zr(SO4)2 catalyst samples calcined at 913 and 1023 K showed the best activity and for supported catalyst Zr(SO4)2/Al2O3 the best activity was achieved when m (Zr(SO4)2)/m(Al2O3)=0.5~1.0. All of the catalysts revealed good selectivity for C80.
2000, 17(5): 471-474
Abstract:
The kinetics of mass transfer in extraction of zinc with raw Cyanex 302 on hollow fiber membrane assembly was studied. The effects of feed solution acidity, concentration of Cyanex 302 and metal ions, and flow rates of aqueous and organic phases on the mass transfer coefficients were discussed. The kinetic equation is derived as follows R=7.22×10-5Vc[HL]0.852cZn2+0.524cH+-0.264/S and the reaction rate constants were calculated.
The kinetics of mass transfer in extraction of zinc with raw Cyanex 302 on hollow fiber membrane assembly was studied. The effects of feed solution acidity, concentration of Cyanex 302 and metal ions, and flow rates of aqueous and organic phases on the mass transfer coefficients were discussed. The kinetic equation is derived as follows R=7.22×10-5Vc[HL]0.852cZn2+0.524cH+-0.264/S and the reaction rate constants were calculated.
2000, 17(5): 475-478
Abstract:
The amorphous Ni-Mo-Co alloy electrodes were prepared by electro-deposition. The properties of three electrodes different in molar ratio content of Ni2+, Co2+ and Mo6+ were compared at pH=9.5 and 40~50℃. Their morphology, element composition and crystal structure were evaluated by SEM, EDAX and XRD analyses. The electrodeposited alloys are amorpohous, silver bright and compact. The catalytic property of the alloy electrodes in hydrogen evolution reaction in 1 mol/L NaOH solution was studied by linear sweep voltammetry and ac impedence measurement. The electrodes have lower overpotential and better catalytic property than pure Ni electrode.
The amorphous Ni-Mo-Co alloy electrodes were prepared by electro-deposition. The properties of three electrodes different in molar ratio content of Ni2+, Co2+ and Mo6+ were compared at pH=9.5 and 40~50℃. Their morphology, element composition and crystal structure were evaluated by SEM, EDAX and XRD analyses. The electrodeposited alloys are amorpohous, silver bright and compact. The catalytic property of the alloy electrodes in hydrogen evolution reaction in 1 mol/L NaOH solution was studied by linear sweep voltammetry and ac impedence measurement. The electrodes have lower overpotential and better catalytic property than pure Ni electrode.
2000, 17(5): 479-482
Abstract:
Two series of compounds:(1-oxa-2,6,7-trioxa-1-phosphobicyclo[2,2,2]octane-4-)methtyl-N-substituted carbamates and 1-(1-oxa-2,6,7-trioxa-1-phosphobicyclo[2,2,2]octane-4-)formyl-2-substituted benzoyl hydrazines were synthesized. The structures of all these compounds were confirmed by 1H NMR, IR and elemental analysis. Some of them were verified by MS. The biological activities of these two series of compounds were examined.
Two series of compounds:(1-oxa-2,6,7-trioxa-1-phosphobicyclo[2,2,2]octane-4-)methtyl-N-substituted carbamates and 1-(1-oxa-2,6,7-trioxa-1-phosphobicyclo[2,2,2]octane-4-)formyl-2-substituted benzoyl hydrazines were synthesized. The structures of all these compounds were confirmed by 1H NMR, IR and elemental analysis. Some of them were verified by MS. The biological activities of these two series of compounds were examined.
2000, 17(5): 483-486
Abstract:
Three methods of catalyst preparation:coprecipitation, impregnation and complex precipitation for methylformate(MF) synthesis directly from synthetic gas were compared. The kinds of precipitants, calcination temperature, feeding process of reactants on the catalyst activity and yield of methylformate have been investigated by XRD and BET surface area measurements. The results showed that the more the active phase of copper manganate and the greater the surface area of the catalyst, the more the active the catalyst prepared.
Three methods of catalyst preparation:coprecipitation, impregnation and complex precipitation for methylformate(MF) synthesis directly from synthetic gas were compared. The kinds of precipitants, calcination temperature, feeding process of reactants on the catalyst activity and yield of methylformate have been investigated by XRD and BET surface area measurements. The results showed that the more the active phase of copper manganate and the greater the surface area of the catalyst, the more the active the catalyst prepared.
2000, 17(5): 487-490
Abstract:
The title heteropoly tungstophosphates M4[PW11NbO2]·x H2O(M=Me4N+,Hep4N+,K+) and MnH4-nPW11(NbO2)O39]·x H2O(M=Me4N+,Et4N+,Bu4N+ and Hep4N+) were synthesized and characterized. The IR, UV spectrometry, polarography and chemical titration confirmed the existence of NbO2 groups in the complexes. All their 183W NMR spectra have six peaks, showing the Keggin structure of anions in the com-pounds. Experiments on oxidation of maleic acid into tartaric acid showed that the complexes containing peroxy ions exhibited higher catalytic activity than those without peroxy ions.
The title heteropoly tungstophosphates M4[PW11NbO2]·x H2O(M=Me4N+,Hep4N+,K+) and MnH4-nPW11(NbO2)O39]·x H2O(M=Me4N+,Et4N+,Bu4N+ and Hep4N+) were synthesized and characterized. The IR, UV spectrometry, polarography and chemical titration confirmed the existence of NbO2 groups in the complexes. All their 183W NMR spectra have six peaks, showing the Keggin structure of anions in the com-pounds. Experiments on oxidation of maleic acid into tartaric acid showed that the complexes containing peroxy ions exhibited higher catalytic activity than those without peroxy ions.
2000, 17(5): 491-494
Abstract:
The emulsion polymerization of aniline in a system consisted of non-polar or weakly polar solvent, functionized protonic acid and water was carried out using (NH4)2 S2O8 as oxidant. The effects of emulsion polymerization conditions:doping acid, oxidant, reaction time and temperature, water content on the solubility, conductivity and yield of polyaniline were studied. The polyaniline synthesized shows much higher solubility in organic solvents than those synthesized by chemical oxidation polymerization. The PAn-DBSA (dodecylbenzene sulfonic acid) obtained in yield of 80% with conductivity over 1 S/cm.
The emulsion polymerization of aniline in a system consisted of non-polar or weakly polar solvent, functionized protonic acid and water was carried out using (NH4)2 S2O8 as oxidant. The effects of emulsion polymerization conditions:doping acid, oxidant, reaction time and temperature, water content on the solubility, conductivity and yield of polyaniline were studied. The polyaniline synthesized shows much higher solubility in organic solvents than those synthesized by chemical oxidation polymerization. The PAn-DBSA (dodecylbenzene sulfonic acid) obtained in yield of 80% with conductivity over 1 S/cm.
2000, 17(5): 495-498
Abstract:
Ten heteropoly compounds were synthesized. Their toxicity to the cells of dog kidney and activity for anti-fox encephalitis virus at nontoxic concentrations were tested by cell culture method. Some of the compounds had high anti-FEV activity at nontoxic concentration, among them HPC-9 had IC50 of 8 mg/L, TC50 of 530 mg/L and TI of 66. The antivirus mechanism of the compounds has been discussed briefly.
Ten heteropoly compounds were synthesized. Their toxicity to the cells of dog kidney and activity for anti-fox encephalitis virus at nontoxic concentrations were tested by cell culture method. Some of the compounds had high anti-FEV activity at nontoxic concentration, among them HPC-9 had IC50 of 8 mg/L, TC50 of 530 mg/L and TI of 66. The antivirus mechanism of the compounds has been discussed briefly.
2000, 17(5): 499-502
Abstract:
The preparation process of nanosize spinel type pigments via W/O microemulsion treatment was studied. The nanosize cobalt blue particles were confirmed by XRD and TEM. The UV spectra and coloring parameters of the pigments were determined. The formation mechanism and quantum size effect of the pigments were discussed.
The preparation process of nanosize spinel type pigments via W/O microemulsion treatment was studied. The nanosize cobalt blue particles were confirmed by XRD and TEM. The UV spectra and coloring parameters of the pigments were determined. The formation mechanism and quantum size effect of the pigments were discussed.
2000, 17(5): 503-506
Abstract:
The doped LiMxMn2O4(M=La,Nd,Y) was synthesized from gel precursor on heating in microwave oven. The precursor was obtained from Li2CO3 and Mn(NO3)2 in mixture of citric acid and ethandiol. XRD data indicated the higher phase purity of the sample as compared with that obtained in muffle heating. Charge and discharge experiments revealed that doped LiM0.006 Mn2O4 have better electrochemical behavior than those undoped ones and obtained from muffle heating. Doping of La, Nd and Y increased the specific discharge capacity and charge/discharge performance of the cells.
The doped LiMxMn2O4(M=La,Nd,Y) was synthesized from gel precursor on heating in microwave oven. The precursor was obtained from Li2CO3 and Mn(NO3)2 in mixture of citric acid and ethandiol. XRD data indicated the higher phase purity of the sample as compared with that obtained in muffle heating. Charge and discharge experiments revealed that doped LiM0.006 Mn2O4 have better electrochemical behavior than those undoped ones and obtained from muffle heating. Doping of La, Nd and Y increased the specific discharge capacity and charge/discharge performance of the cells.
2000, 17(5): 507-511
Abstract:
The 2nd-order polarizability values of two imidazole compounds:2-p-acetami-nophenyl-4,5-di-p-nitrophenylimidazole and 2-p-nitrophenyl-4,5-di-p-acetaminophenyl imidazole in different solvents were estimated by a solvatochromic method based on Bilot-Kawshi and Lippert equations. The Uvalues of two compounds are 24.47×10-30 esu and 16.80×10-30 esu, respectively, in good agreement with those by FF/PM3 quantum chemistry calculations. The results indicated that the main contributors for static U0 are not the λmax, but the transition oscillator strength f and dipole differentce Δ_.
The 2nd-order polarizability values of two imidazole compounds:2-p-acetami-nophenyl-4,5-di-p-nitrophenylimidazole and 2-p-nitrophenyl-4,5-di-p-acetaminophenyl imidazole in different solvents were estimated by a solvatochromic method based on Bilot-Kawshi and Lippert equations. The Uvalues of two compounds are 24.47×10-30 esu and 16.80×10-30 esu, respectively, in good agreement with those by FF/PM3 quantum chemistry calculations. The results indicated that the main contributors for static U0 are not the λmax, but the transition oscillator strength f and dipole differentce Δ_.
2000, 17(5): 512-515
Abstract:
A blue electroluminescent polymer dioctyloxyl substituted polyparaphenylene(DOO-PPP) was synthesized in nitrobenzene via a chemical oxidative route using FeCl3 as catalyst. The effects of FeCl3 amount, temperature, reaction time and monomer concentration on the yield and moleclar weight of DOO-PPP were investigated. The polymer exhibited analogical thermogravimetric behavior both in air and N2, the peak wavelength of its photoluminescence spectrum in CHCl3 was at 426 nm.
A blue electroluminescent polymer dioctyloxyl substituted polyparaphenylene(DOO-PPP) was synthesized in nitrobenzene via a chemical oxidative route using FeCl3 as catalyst. The effects of FeCl3 amount, temperature, reaction time and monomer concentration on the yield and moleclar weight of DOO-PPP were investigated. The polymer exhibited analogical thermogravimetric behavior both in air and N2, the peak wavelength of its photoluminescence spectrum in CHCl3 was at 426 nm.
2000, 17(5): 516-519
Abstract:
Poly(styrene-butadiene-styrene)(SBS) were modified by reacting with (RfCO2)2 in CH2Cl2 at room temperature to give Rf-SBS polymers. All the fluoroalkylated products were characterized by IR and 19F NMR spectra. It is shown that Rf and RfCO2 groups were only added onto the double bonds of SBS polymer chain via single electron transfer(SET) mechanism. The Rf-SBS polymers showed good water- and oil-repellency and low refractive indices.
Poly(styrene-butadiene-styrene)(SBS) were modified by reacting with (RfCO2)2 in CH2Cl2 at room temperature to give Rf-SBS polymers. All the fluoroalkylated products were characterized by IR and 19F NMR spectra. It is shown that Rf and RfCO2 groups were only added onto the double bonds of SBS polymer chain via single electron transfer(SET) mechanism. The Rf-SBS polymers showed good water- and oil-repellency and low refractive indices.
2000, 17(5): 520-523
Abstract:
A new type of butylacrylate-rosins-sucrose ester polyurethane was synthesized and a IPN material was prepared by blending it with polyacrylate(PA). The structure and property of the product were examined by FTIR, TGA and DSC. The effects of TDI-TMP and PA on the product were investigated.
A new type of butylacrylate-rosins-sucrose ester polyurethane was synthesized and a IPN material was prepared by blending it with polyacrylate(PA). The structure and property of the product were examined by FTIR, TGA and DSC. The effects of TDI-TMP and PA on the product were investigated.
2000, 17(5): 524-526
Abstract:
The polymerization of acrylonitrile was first studied using (C9H7)2Y(_-Et)2 AlEt2 as a single-component catalyst. The catalytic activity could be greatly increased when PhONa was added to the catalyst in amount of n(PhONa)/n(Cat)=3. A mechanism related to the polymerization initiation of AN is proposed.
The polymerization of acrylonitrile was first studied using (C9H7)2Y(_-Et)2 AlEt2 as a single-component catalyst. The catalytic activity could be greatly increased when PhONa was added to the catalyst in amount of n(PhONa)/n(Cat)=3. A mechanism related to the polymerization initiation of AN is proposed.
2000, 17(5): 527-529
Abstract:
Ten thiazoline compounds were synthesized starting from tetrahydrothiazoles. Their fungicidal activities against Phoma asparagi, Gibberella zeae, Cercospora beticola and Alteraria solani were examined. Some of them gave considerable good results.
Ten thiazoline compounds were synthesized starting from tetrahydrothiazoles. Their fungicidal activities against Phoma asparagi, Gibberella zeae, Cercospora beticola and Alteraria solani were examined. Some of them gave considerable good results.
2000, 17(5): 530-532
Abstract:
The Ni/Al2O3 catalysts were prepared by two impregnation methods:common and promoted with support salt, for CH4/CO2 reforming and studied by using TPR, TPD, TPMC(Temperature programmed methane decomposition carbon deposition) and activity test techniques. The results showed that the coke formation of the catalysts promoted with support salt(aluminium nitrate) was reduced to one sixth and the dispersion increased by 72.7% in comparison with catalyst prepared by common impregnation method. The interactions between Ni and Al with O on the surface of the support salt promoted catalyst appeared stronger.
The Ni/Al2O3 catalysts were prepared by two impregnation methods:common and promoted with support salt, for CH4/CO2 reforming and studied by using TPR, TPD, TPMC(Temperature programmed methane decomposition carbon deposition) and activity test techniques. The results showed that the coke formation of the catalysts promoted with support salt(aluminium nitrate) was reduced to one sixth and the dispersion increased by 72.7% in comparison with catalyst prepared by common impregnation method. The interactions between Ni and Al with O on the surface of the support salt promoted catalyst appeared stronger.
2000, 17(5): 533-535
Abstract:
rac-Tetra(m-nitrobenzene)porphyrin, H2TNO2PP, synthesized from o-nitro-benzaldehyde and pyrrole was reduced to H2TamPP, from which tetra(o-phenylacetyl benzene) porphyrin and especially its T,T,T,T-isomer were obtained. The T,T,T,T-isomer was used as hapten to immunize BALB/C mice. The latter gave antibody value of 320 as determined by ELISA method, indicating that the artificial hapten could induce the production of antibody without use of carrier.
rac-Tetra(m-nitrobenzene)porphyrin, H2TNO2PP, synthesized from o-nitro-benzaldehyde and pyrrole was reduced to H2TamPP, from which tetra(o-phenylacetyl benzene) porphyrin and especially its T,T,T,T-isomer were obtained. The T,T,T,T-isomer was used as hapten to immunize BALB/C mice. The latter gave antibody value of 320 as determined by ELISA method, indicating that the artificial hapten could induce the production of antibody without use of carrier.
2000, 17(5): 536-538
Abstract:
The title compound, a fine artificial sweetener of high sweetness and low caloricity, has been synthesized using Upinene from turpentine oil as raw material by 4-step reactions:epoxidation, isomerization, oxidation and oximation. The product was obtained with 99% purity in total yield of 22.5%.
The title compound, a fine artificial sweetener of high sweetness and low caloricity, has been synthesized using Upinene from turpentine oil as raw material by 4-step reactions:epoxidation, isomerization, oxidation and oximation. The product was obtained with 99% purity in total yield of 22.5%.
2000, 17(5): 539-541
Abstract:
Three series of poly(aryl ether ketone)s(PAEKs) were synthesized from varied ratio of 1-chloro-4-(4-chlorobenzoyl)naphthalene and 4,4'-difluorobenzophenone with three different bisphenols respectively. The polymers have been studied by IR、DSC, mechanical property and solubility measurements. The results showed that the Tg of the polymers increased with the increase of 1,4-naphthylene and the tensile strength got a maximum at a certain naphthylene content. The PAEKs were soluble plastics with excellent heat resistance and good tensile strength.
Three series of poly(aryl ether ketone)s(PAEKs) were synthesized from varied ratio of 1-chloro-4-(4-chlorobenzoyl)naphthalene and 4,4'-difluorobenzophenone with three different bisphenols respectively. The polymers have been studied by IR、DSC, mechanical property and solubility measurements. The results showed that the Tg of the polymers increased with the increase of 1,4-naphthylene and the tensile strength got a maximum at a certain naphthylene content. The PAEKs were soluble plastics with excellent heat resistance and good tensile strength.
2000, 17(5): 542-544
Abstract:
The stainless steel matrix was dipped in a solution containing palladium and silver ions to prepare palladium-silver membrane by electroless plating. The effects of solution composition and pH value on film compositions and morphology were studied. The SEM photos showed the uniform and compact structure of the membrane. XRD results revealed the isolated state of metals in membrane. Heat treatment first under vacuum below 300℃ and then under Ar atmosphere at about 800℃ tends to formation of alloy metals, reducing the innerstress among films and increasing the cohesive force between films and matrix.
The stainless steel matrix was dipped in a solution containing palladium and silver ions to prepare palladium-silver membrane by electroless plating. The effects of solution composition and pH value on film compositions and morphology were studied. The SEM photos showed the uniform and compact structure of the membrane. XRD results revealed the isolated state of metals in membrane. Heat treatment first under vacuum below 300℃ and then under Ar atmosphere at about 800℃ tends to formation of alloy metals, reducing the innerstress among films and increasing the cohesive force between films and matrix.
2000, 17(5): 545-546
Abstract:
Title compound has been prepared at room temperature from N-phenylsu-lfonylprolylchloride with n(KCN)/n(CuCN)=1:1 as catalyst and identified by elemental analysis, IR and MS spectra. The influence of the catalyst constitution on the product distribution has been discussed briefly.
Title compound has been prepared at room temperature from N-phenylsu-lfonylprolylchloride with n(KCN)/n(CuCN)=1:1 as catalyst and identified by elemental analysis, IR and MS spectra. The influence of the catalyst constitution on the product distribution has been discussed briefly.
2000, 17(5): 547-549
Abstract:
The waste apple pomace was treated by cellulase to produce glucose. The results show that the optimum operating conditions are:at 50℃, pH=5, keep the concentration of cellulase to 20 μg/g medium, react time to 12 h and do not treat the apple pomace with alkali. In the range of the reacting time we adopted, the influence of the cellulose concentration can be ignored. The producing technique of the citric acid and the determine method of the citric acid also been studied by experiments.
The waste apple pomace was treated by cellulase to produce glucose. The results show that the optimum operating conditions are:at 50℃, pH=5, keep the concentration of cellulase to 20 μg/g medium, react time to 12 h and do not treat the apple pomace with alkali. In the range of the reacting time we adopted, the influence of the cellulose concentration can be ignored. The producing technique of the citric acid and the determine method of the citric acid also been studied by experiments.
2000, 17(5): 550-552
Abstract:
Five new 6-O-prolinated monoacetylbritannilactones have been synthesized from N-acetylprolyl chlorides with 4-N,N-dimethylaminopyridine as catalyst and characterized by elemental analysis, IR,1H NMR,1H-1H COSY and MS. The compound 3b displayed a good biological activity for human HL-60 cell in vitro(ED50=4.6 mg/L).
Five new 6-O-prolinated monoacetylbritannilactones have been synthesized from N-acetylprolyl chlorides with 4-N,N-dimethylaminopyridine as catalyst and characterized by elemental analysis, IR,1H NMR,1H-1H COSY and MS. The compound 3b displayed a good biological activity for human HL-60 cell in vitro(ED50=4.6 mg/L).
2000, 17(5): 553-554
Abstract:
Hydroxyethyl starch with molecular weight of 2.7×105~3.2×105 and substitution value of 0.47~0.54 was prepared. The product showed good thickening property and was stable at -15℃ for 48 hours.
Hydroxyethyl starch with molecular weight of 2.7×105~3.2×105 and substitution value of 0.47~0.54 was prepared. The product showed good thickening property and was stable at -15℃ for 48 hours.
2000, 17(5): 555-557
Abstract:
The Ti-supported lead dioxide electrode(Ti/PdO2) consisted of a Sb2O3/SnO2 semiconductive interlayer and electrodeposited PbO2 films was prepared. The optimum ratio of Sb2O3 to SnO2 was 15%~25%. Addition of NaF(0.40 g/L) in electroplating solution could decrease the rate of PbO2 deposition, which resulted in the formation of small crystal particles and compact PbO2 films. XRD study showed the U-form crystal of electrode. The electrode was tested in synthesis of 4-picoline acid by electro-oxidation of 4-picoline, showing good electroconductivity and stable life.
The Ti-supported lead dioxide electrode(Ti/PdO2) consisted of a Sb2O3/SnO2 semiconductive interlayer and electrodeposited PbO2 films was prepared. The optimum ratio of Sb2O3 to SnO2 was 15%~25%. Addition of NaF(0.40 g/L) in electroplating solution could decrease the rate of PbO2 deposition, which resulted in the formation of small crystal particles and compact PbO2 films. XRD study showed the U-form crystal of electrode. The electrode was tested in synthesis of 4-picoline acid by electro-oxidation of 4-picoline, showing good electroconductivity and stable life.
2000, 17(5): 558-560
Abstract:
Four pyrimidine derivatives and six corresponding complexes with Cu(Ⅱ) and Zn(Ⅱ) were synthesized and characterized by elemental analysis, thermoanalysis, IR, UV spectra and molar conductivity measurements. Preliminary biological tests showed that complexes 1(CuL2Cl2(R=CH3)) and 5(ZnL2Cl2(R=n-C3H7)) exhibited a certain weeding activity against wheat and barnyard grass.
Four pyrimidine derivatives and six corresponding complexes with Cu(Ⅱ) and Zn(Ⅱ) were synthesized and characterized by elemental analysis, thermoanalysis, IR, UV spectra and molar conductivity measurements. Preliminary biological tests showed that complexes 1(CuL2Cl2(R=CH3)) and 5(ZnL2Cl2(R=n-C3H7)) exhibited a certain weeding activity against wheat and barnyard grass.
2000, 17(5): 561-562
Abstract:
Title compound was synthesized in five steps, starting from carbazole, and identified by IR,1H NMR and elemental analysis. It is a yellowisk needle crystal, mp 152~153℃, yield >4%.
Title compound was synthesized in five steps, starting from carbazole, and identified by IR,1H NMR and elemental analysis. It is a yellowisk needle crystal, mp 152~153℃, yield >4%.
2000, 17(5): 563-565
Abstract:
1,3-Benzodioxole was monochloromethylated directly by aqueous formaldehyde and hydrogen chloride gas in CCl4 in the presence of quaternary ammonium salts:C16H33-(CH3)3 NX(X=Br,Cl), C12H25(CH3)3 NCl,C12H25(CH3)2(C6H5CH2)NCl and (C4H9)4 NBr. With hexadecyltrimethylammonium bromide at temperature 60~65℃ and for 15 hours of reaction, 1,3-benzodioxole was converted to piperonyl chloride with conversion more than 98% and selectivity up to 97%. The method has advantages of high selectivity, high conversion, negligible by-products and easy workup of the main product.
1,3-Benzodioxole was monochloromethylated directly by aqueous formaldehyde and hydrogen chloride gas in CCl4 in the presence of quaternary ammonium salts:C16H33-(CH3)3 NX(X=Br,Cl), C12H25(CH3)3 NCl,C12H25(CH3)2(C6H5CH2)NCl and (C4H9)4 NBr. With hexadecyltrimethylammonium bromide at temperature 60~65℃ and for 15 hours of reaction, 1,3-benzodioxole was converted to piperonyl chloride with conversion more than 98% and selectivity up to 97%. The method has advantages of high selectivity, high conversion, negligible by-products and easy workup of the main product.
2000, 17(5): 566-568
Abstract:
The chloromethylated crosslinked polystyrene with chlorine content of 3.9, 3.7 and 2.7 mmol/g were prepared by chloromethylating crosslinked polystyrene with crosslinkage of 2%, 4% and 5% respectively. The insoluble quaternary ammonium bactericides with quaternary ammonium content of 2.6, 2.5 and 2.2 mmol/g quaterisated resin were prepared by treating the chloromethylated polystyrene with dimethyldodecyl ammonium. It is found that the more crosslinkages in chloromethylated polystyrene, the smaller the pore volume, the less the chlorine content, then the less the ammonium amount in resin and the less antibactericidal activity of the polymer bactericides.
The chloromethylated crosslinked polystyrene with chlorine content of 3.9, 3.7 and 2.7 mmol/g were prepared by chloromethylating crosslinked polystyrene with crosslinkage of 2%, 4% and 5% respectively. The insoluble quaternary ammonium bactericides with quaternary ammonium content of 2.6, 2.5 and 2.2 mmol/g quaterisated resin were prepared by treating the chloromethylated polystyrene with dimethyldodecyl ammonium. It is found that the more crosslinkages in chloromethylated polystyrene, the smaller the pore volume, the less the chlorine content, then the less the ammonium amount in resin and the less antibactericidal activity of the polymer bactericides.
2000, 17(5): 569-571
Abstract:
Tetrabromo-2,3-naphthophthalocyanine zinc(Ⅱ)(ZnNcBr4) was synthesized by refluxing 6-bromo-2,3-dicyanonaphthlene with anhydrous zinc chloride in n-amyl alcohol in the presence of 1,8-diazabicyclo[5,4,0]-undec-7-ene. The product was characterized by elemental analysis and IR. The absorption spectra in non-aqueous solvents and the thermal stability of the compound were studied. Its nonlinear optical limiting was explored by a double frequency Nd:YAG pulse laser system with wavelenth of 532 nm and pulse width of 8 ns and 23 ps.
Tetrabromo-2,3-naphthophthalocyanine zinc(Ⅱ)(ZnNcBr4) was synthesized by refluxing 6-bromo-2,3-dicyanonaphthlene with anhydrous zinc chloride in n-amyl alcohol in the presence of 1,8-diazabicyclo[5,4,0]-undec-7-ene. The product was characterized by elemental analysis and IR. The absorption spectra in non-aqueous solvents and the thermal stability of the compound were studied. Its nonlinear optical limiting was explored by a double frequency Nd:YAG pulse laser system with wavelenth of 532 nm and pulse width of 8 ns and 23 ps.
2000, 17(5): 572-574
Abstract:
A pair of reversible waves at 0.335 V(vs.SCE) in cyclic voltammograms caused by reaction of dopamine with aniline on a platinum electrode were observed in 1.0 mol/L HCl containing aniline. The linear ranges were 1.0×10-6~1.1×10-5 mol/L and 1.4×10-5~1.7×10-4 mol/L with detection limit of 5.0×10-7 mol/L. The oxidative peak of ascorbic acid was found at ca. 0.640 V. 100 times of ascorbic acid showed no interference to the determination of dopamine.
A pair of reversible waves at 0.335 V(vs.SCE) in cyclic voltammograms caused by reaction of dopamine with aniline on a platinum electrode were observed in 1.0 mol/L HCl containing aniline. The linear ranges were 1.0×10-6~1.1×10-5 mol/L and 1.4×10-5~1.7×10-4 mol/L with detection limit of 5.0×10-7 mol/L. The oxidative peak of ascorbic acid was found at ca. 0.640 V. 100 times of ascorbic acid showed no interference to the determination of dopamine.
2000, 17(5): 575-577
Abstract:
Polycarbonate was aminated by treating with tetraethylenepentamine in dichloromethane to give aminated PC(a-PC). The glass transition behavior and mechanical properties of epoxy resin toughened by a-PC were investigated. The system had a single glass transition temperature. Optimum mechanical properties were obtained when the mass fraction of a-PC was about 10%.
Polycarbonate was aminated by treating with tetraethylenepentamine in dichloromethane to give aminated PC(a-PC). The glass transition behavior and mechanical properties of epoxy resin toughened by a-PC were investigated. The system had a single glass transition temperature. Optimum mechanical properties were obtained when the mass fraction of a-PC was about 10%.
2000, 17(5): 578-580
Abstract:
The electroless Ni-Cu-P coatings with different Cu content have been deposited from alkaline bath. The surface morphology, microstructure and crystallization behaviour of the electroless Ni-Cu-P alloys have been studied by SEM, XRD and DSC. The results show that the concentration of CuSO4·5H2O in the bath has a great effect on the composition of the deposits and the deposition rate. The codeposition of a small amount of Cu makes the crystal grains of the deposits become smaller, but with the Cu content increasing, the deposits exhibit a larger grain size and a more coarse surface morphology. The thermal stability of Ni-Cu-P deposit increases with the Cu content increasing in the deposits.
The electroless Ni-Cu-P coatings with different Cu content have been deposited from alkaline bath. The surface morphology, microstructure and crystallization behaviour of the electroless Ni-Cu-P alloys have been studied by SEM, XRD and DSC. The results show that the concentration of CuSO4·5H2O in the bath has a great effect on the composition of the deposits and the deposition rate. The codeposition of a small amount of Cu makes the crystal grains of the deposits become smaller, but with the Cu content increasing, the deposits exhibit a larger grain size and a more coarse surface morphology. The thermal stability of Ni-Cu-P deposit increases with the Cu content increasing in the deposits.
