A new biphenol-like monomer,4,4′-methylenebis[4-(1,4-phenylene)-phthalazin-1(2H)-one] was synthesized from phthalic anhydride and diphenylmethane in two steps.In the first step,Friedel-Crafts reaction was carried out...A new biphenol-like monomer,4,4′-methylenebis[4-(1,4-phenylene)-phthalazin-1(2H)-one] was synthesized from phthalic anhydride and diphenylmethane in two steps.In the first step,Friedel-Crafts reaction was carried out in 1,2-dichloroethane between diphenylmethane and phthalic anhydride.The obtained product was used in the second step with hydrazine monohydrate added into its solution,followed by recrystallization in acetic acid.The melting point showed by differential scanning calorimetry of the bis(phthalazinone) monomer was 338.1℃.The overall yield of the biphenol-like monomer was 60%.A new polyphthalazinone was prepared from 4,4′-difluorodiphenylketone(DFK) and 4,4′-methylenebis[4-(1,4-phenylene)-phthalazin-1(2H)-one] by solution polycondensation in N-methyl-2-pyrrolidone(NMP) with anhydrous K 2CO 3 as a catalyst.High molecular weight polymer was formed in 8 h at 190℃.The polymer was refined by precipitation from its 15% NMP solution with methanol as the precipitating agent.The powder of the polymer was dried in a vacuum oven under 120℃ for 48*!h and then under 200℃ for 4*!h.The intrinsic viscosity of the polymer was 0.58*!dL/g in NMP at 25℃.The polymer showed high glass transition temperature (T g) at 258℃ by DSC.The decomposition temperature for 5% weight loss (T d5) in nitrogen measured by thermogravimetric analysis occurred at 431℃.The solubility of the polymer was investigated at room temperature.The polymer was soluble in NMP,m-cresol and partially soluble in chloroform,and insoluble in N,N-dimethylacetamide (DMAc) and dimethyl sulfoxide (DMSO).The methylene group and bis-(phthalazinone) structure in the backbone of the polymer contribute much to the good solubility,and the rigid structure of bis(phthalazinone) retains its good thermal properties.展开更多
The ultrafiltration membrane was prepared from an aromatic polyamide containing 1,2-dihydro-4-phenyl(2H)phthalazinone moiety it is soluble in DMAc, DMF, NMP, DMSO and m-cresol. The effects of solvents, polymer concent...The ultrafiltration membrane was prepared from an aromatic polyamide containing 1,2-dihydro-4-phenyl(2H)phthalazinone moiety it is soluble in DMAc, DMF, NMP, DMSO and m-cresol. The effects of solvents, polymer concentration, additive, and temperature of gel bath on the membrane performance were studied. While DMAc was used as solvent and ethylene glycol methylether or diethyl ether was used as additive, the rejection against PEG12000 was up to 100% under 0 1 MPa.展开更多
A series of aromatic copolyamides were prepared from（1,2-dihydro-2-（4-aminophenyl）-4-[4-（4-）（aminophenoxyl）phenyl）]phthalazin-1-one（DHPZ-DA）,p-phenylenediamine（PPD）,1,4-bis（4-aminophenoxy） benzene（BAPOB...A series of aromatic copolyamides were prepared from（1,2-dihydro-2-（4-aminophenyl）-4-[4-（4-）（aminophenoxyl）phenyl）]phthalazin-1-one（DHPZ-DA）,p-phenylenediamine（PPD）,1,4-bis（4-aminophenoxy） benzene（BAPOB） and terephthaloyl dichloride by low temperature solution polycondensation.The polymers had relatively high inherent viscosities ranging from 1.74 dL/g to 4.31 dL/g.The polymers exhibit improved solubility in polar aprotic solvents with or without the addition of LiCl because of the introduction of twisted non-coplanar phthalazinone moieties and flexible ether linkages.The polymers had high thermal stability.Their glass transition temperature（Tg） values were in the range of 291～351℃,and the 5% and 10% weight loss temperatures in nitrogen were in the range of 486～504℃ and 509～528℃,respectively.WAXD measurements indicated that these copolyamides were amorphous.Most of the polymers exhibited lyotropic liquid crystalline characteristics in conc.H2SO4,NMP/（10 g/L LiCl） and DMAc/（10 g/L LiCl） solutions.The polyamides with excellent properties made it possible for the different processing and applications such as dry-wet spinning of fibers or the preparation of films,membranes and coatings.展开更多
文摘A new biphenol-like monomer,4,4′-methylenebis[4-(1,4-phenylene)-phthalazin-1(2H)-one] was synthesized from phthalic anhydride and diphenylmethane in two steps.In the first step,Friedel-Crafts reaction was carried out in 1,2-dichloroethane between diphenylmethane and phthalic anhydride.The obtained product was used in the second step with hydrazine monohydrate added into its solution,followed by recrystallization in acetic acid.The melting point showed by differential scanning calorimetry of the bis(phthalazinone) monomer was 338.1℃.The overall yield of the biphenol-like monomer was 60%.A new polyphthalazinone was prepared from 4,4′-difluorodiphenylketone(DFK) and 4,4′-methylenebis[4-(1,4-phenylene)-phthalazin-1(2H)-one] by solution polycondensation in N-methyl-2-pyrrolidone(NMP) with anhydrous K 2CO 3 as a catalyst.High molecular weight polymer was formed in 8 h at 190℃.The polymer was refined by precipitation from its 15% NMP solution with methanol as the precipitating agent.The powder of the polymer was dried in a vacuum oven under 120℃ for 48*!h and then under 200℃ for 4*!h.The intrinsic viscosity of the polymer was 0.58*!dL/g in NMP at 25℃.The polymer showed high glass transition temperature (T g) at 258℃ by DSC.The decomposition temperature for 5% weight loss (T d5) in nitrogen measured by thermogravimetric analysis occurred at 431℃.The solubility of the polymer was investigated at room temperature.The polymer was soluble in NMP,m-cresol and partially soluble in chloroform,and insoluble in N,N-dimethylacetamide (DMAc) and dimethyl sulfoxide (DMSO).The methylene group and bis-(phthalazinone) structure in the backbone of the polymer contribute much to the good solubility,and the rigid structure of bis(phthalazinone) retains its good thermal properties.
文摘The ultrafiltration membrane was prepared from an aromatic polyamide containing 1,2-dihydro-4-phenyl(2H)phthalazinone moiety it is soluble in DMAc, DMF, NMP, DMSO and m-cresol. The effects of solvents, polymer concentration, additive, and temperature of gel bath on the membrane performance were studied. While DMAc was used as solvent and ethylene glycol methylether or diethyl ether was used as additive, the rejection against PEG12000 was up to 100% under 0 1 MPa.
文摘A series of aromatic copolyamides were prepared from（1,2-dihydro-2-（4-aminophenyl）-4-[4-（4-）（aminophenoxyl）phenyl）]phthalazin-1-one（DHPZ-DA）,p-phenylenediamine（PPD）,1,4-bis（4-aminophenoxy） benzene（BAPOB） and terephthaloyl dichloride by low temperature solution polycondensation.The polymers had relatively high inherent viscosities ranging from 1.74 dL/g to 4.31 dL/g.The polymers exhibit improved solubility in polar aprotic solvents with or without the addition of LiCl because of the introduction of twisted non-coplanar phthalazinone moieties and flexible ether linkages.The polymers had high thermal stability.Their glass transition temperature（Tg） values were in the range of 291～351℃,and the 5% and 10% weight loss temperatures in nitrogen were in the range of 486～504℃ and 509～528℃,respectively.WAXD measurements indicated that these copolyamides were amorphous.Most of the polymers exhibited lyotropic liquid crystalline characteristics in conc.H2SO4,NMP/（10 g/L LiCl） and DMAc/（10 g/L LiCl） solutions.The polyamides with excellent properties made it possible for the different processing and applications such as dry-wet spinning of fibers or the preparation of films,membranes and coatings.
