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
A fluorine containing monomer was synthesized and its polymer was prepared by aromatic nucleophilic substitution polycondensation of the monomer and 4,4′ difluorobenzophenone using potassium carbonate as the catalyst...A fluorine containing monomer was synthesized and its polymer was prepared by aromatic nucleophilic substitution polycondensation of the monomer and 4,4′ difluorobenzophenone using potassium carbonate as the catalyst and tetramethylene sulfone as solvent. The polymer properties were characterized by FTIR, NMR, DSC and the results showed that the T g of the polymer is 141 ℃ and the solubility of the polymer was obviously improved due to the introduction of (3 trifluoromethyl)phenyl group.展开更多
A kind of highly fluorinated bisphenol monomer was synthesized. It was characterized by FTIR, 1H NMR and MS. 6F PEEK and 6F PEEKK were prepared via aromatic nucleophilic substitution, based on [3,5 di(trifluoromethyl)...A kind of highly fluorinated bisphenol monomer was synthesized. It was characterized by FTIR, 1H NMR and MS. 6F PEEK and 6F PEEKK were prepared via aromatic nucleophilic substitution, based on [3,5 di(trifluoromethyl)] phenylhydroquinone and difluoro monomers. The T gs of 6F PEEK and 6F PEEKK are 423 and 436 K, respectively. The 6F polymers exhibit a high thermal stability and good solubility. The flexible, creasable and transparent thin films were easily obtained by compression moulding and solution casting.展开更多
Two novel poly(aryl ether ketone)s based on (3 methyl)phenylhydroquinone were synthesized via aromatic nucleophilic substitution reaction. The high molecular polymers were easily obtained because of the high reaction ...Two novel poly(aryl ether ketone)s based on (3 methyl)phenylhydroquinone were synthesized via aromatic nucleophilic substitution reaction. The high molecular polymers were easily obtained because of the high reaction activity of bisphenol monomer. The traces of DSC showed that the T gs of m TPEEK and m TPEEKK were 421 and 432 K, respectively. The two polymers exhibit a high thermal stability and good solubility. The transparent and flexible films were readily prepared with chloroform solution. The film of m TPEEK had a low dielectric constant( ε =2 7).展开更多
Novel thermotropic liquid crystalline poly(aryl ether ketone) was synthesized via the random copolycondensation of 4,4′ difluorobenzophenone, 4,4′ biphenol and tert butylhydroquinone. The results of differential sca...Novel thermotropic liquid crystalline poly(aryl ether ketone) was synthesized via the random copolycondensation of 4,4′ difluorobenzophenone, 4,4′ biphenol and tert butylhydroquinone. The results of differential scanning calorimetry, polarizing light microscope and X ray diffraction confirmed the liquid crystalline property of the polymer. The polymer may be of great use in blending with normal poly(aryl ether ketone)s.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A fluorine containing monomer was synthesized and its polymer was prepared by aromatic nucleophilic substitution polycondensation of the monomer and 4,4′ difluorobenzophenone using potassium carbonate as the catalyst and tetramethylene sulfone as solvent. The polymer properties were characterized by FTIR, NMR, DSC and the results showed that the T g of the polymer is 141 ℃ and the solubility of the polymer was obviously improved due to the introduction of (3 trifluoromethyl)phenyl group.
文摘A kind of highly fluorinated bisphenol monomer was synthesized. It was characterized by FTIR, 1H NMR and MS. 6F PEEK and 6F PEEKK were prepared via aromatic nucleophilic substitution, based on [3,5 di(trifluoromethyl)] phenylhydroquinone and difluoro monomers. The T gs of 6F PEEK and 6F PEEKK are 423 and 436 K, respectively. The 6F polymers exhibit a high thermal stability and good solubility. The flexible, creasable and transparent thin films were easily obtained by compression moulding and solution casting.
文摘Two novel poly(aryl ether ketone)s based on (3 methyl)phenylhydroquinone were synthesized via aromatic nucleophilic substitution reaction. The high molecular polymers were easily obtained because of the high reaction activity of bisphenol monomer. The traces of DSC showed that the T gs of m TPEEK and m TPEEKK were 421 and 432 K, respectively. The two polymers exhibit a high thermal stability and good solubility. The transparent and flexible films were readily prepared with chloroform solution. The film of m TPEEK had a low dielectric constant( ε =2 7).
文摘Novel thermotropic liquid crystalline poly(aryl ether ketone) was synthesized via the random copolycondensation of 4,4′ difluorobenzophenone, 4,4′ biphenol and tert butylhydroquinone. The results of differential scanning calorimetry, polarizing light microscope and X ray diffraction confirmed the liquid crystalline property of the polymer. The polymer may be of great use in blending with normal poly(aryl ether ketone)s.
