A novel series of poly(aryl ether sulfone ketone)s (PPESKs) containing phthalazinone and biphenyl moieties were prepared by two-step nucleophilic polycondensation reaction. The ^-Mw values of these copolymers were...A novel series of poly(aryl ether sulfone ketone)s (PPESKs) containing phthalazinone and biphenyl moieties were prepared by two-step nucleophilic polycondensation reaction. The ^-Mw values of these copolymers were between 38,330 and 67,900. The glass transition temperatures (Tg) and 5% decomposition temperatures were ranged in 253-269 ℃ and 488-500 ℃, respectively, The structures of these copolymers were confirmed by FT-IR and ^1H NMR. Moreover, all the resultant copolymers were amorphous determined by wide angle X-ray diffraction (WAXD).展开更多
A new monomer, 1,4-bis(4-fluorobenzoyl) naphthalene(compound 2) was synthesized via a two-step reaction. 1,4-Naphthalenedicarboxylic acid chloride(compound 1) was prepared by using the acyl chlorization reaction of 1,...A new monomer, 1,4-bis(4-fluorobenzoyl) naphthalene(compound 2) was synthesized via a two-step reaction. 1,4-Naphthalenedicarboxylic acid chloride(compound 1) was prepared by using the acyl chlorization reaction of 1,4-naphthalenedicarboxylic acid with thionyl chloride. The Friedel-Crafts acylation of compound 1 with fluorobenzene afforded compound 2 in a 80% yield. The polycondensation of compound 2 with various bisphenols in tetramethylene sulfone(TMS) in the presence of excess potassium carbonate as a condensation reagent was carried out at 210 ℃ to quantitatively afford the corresponding poly(aryl ether ketone)s(compounds 3_8) containing 1,4-naphthalene moieties. Thermal analyses showed that the polymers have T g values ranging from 496 to 500 K and are thermally stable in air with initial mass loss above 500 ℃. These novel polymers exhibited an excellent solubility in organic solvents including NMP, DMAc, and chloroform, etc. In addition, the glass transition temperatures of these polymers increased and the polymers became insoluble in chloroform after treated at 260 ℃, indicating the occurrence of a thermal crosslinking reaction.展开更多
In this paper,a series of optically active MeO-BIPHEP-type ligands,(S)-6,6′-dimethoxy-2,2’-bis(di-p-alkoxyphenylphosphine)- 1,1′-biphenyl were synthesized and used to prepare the ruthenium complex.The effects o...In this paper,a series of optically active MeO-BIPHEP-type ligands,(S)-6,6′-dimethoxy-2,2’-bis(di-p-alkoxyphenylphosphine)- 1,1′-biphenyl were synthesized and used to prepare the ruthenium complex.The effects of para-substituted were observed,the results showed that the ruthenium catalysts[diphosphine RuCl;diamine]containing both t-Bu and i-Pr substitutions have better activities and enantioselectivities than the non-substituted ruthenium catalysts in the asymmetric hydrogenation of acetophenone.展开更多
A new poly(aryl ether ketone) containing biphenylphthalazinone moiety was prepared by the reaction of 4-(4-hydroxybiphenyl) phthalazine-1-one with 4, 4'-difluorobenzophenone. The monomer and the polymer were chara...A new poly(aryl ether ketone) containing biphenylphthalazinone moiety was prepared by the reaction of 4-(4-hydroxybiphenyl) phthalazine-1-one with 4, 4'-difluorobenzophenone. The monomer and the polymer were characterized by FT-IR and H-1-NMR. Some properties of this polymer were described.展开更多
A novel heterocyclic poly (aryl ether ketone ketone) (PPEKK) containing cyclohexenering was prepared from 1-methyl-cyclohex-1-ene-4, 5 -diyl-bis(4-chlorophenyl methanone) and 4 (4-hydroxyphenyl)(2H) phthalazin-1-one. ...A novel heterocyclic poly (aryl ether ketone ketone) (PPEKK) containing cyclohexenering was prepared from 1-methyl-cyclohex-1-ene-4, 5 -diyl-bis(4-chlorophenyl methanone) and 4 (4-hydroxyphenyl)(2H) phthalazin-1-one. The polymer was characterized by FTIR, 1HNMR, DSC,TG and X-ray analysis.展开更多
A novel soluble poly(aryl ether ketone) was prepared by the reaction of 4-(3-phenyl-4-hydroxyphenyl)phthalazinone with 4,4'-difluorobenzophenone. The polymer was characterized by DSC, TGA and X-ray diffraction.
Poly( aryl ether ketone) copolymers containing 2,7-naphthylene and hydroquinone(HQ) moieties with various compositions were prepared by the reaction of 4,4'-difluorobenzophenone(DFB) 2,7-naphthylene and hydroqu...Poly( aryl ether ketone) copolymers containing 2,7-naphthylene and hydroquinone(HQ) moieties with various compositions were prepared by the reaction of 4,4'-difluorobenzophenone(DFB) 2,7-naphthylene and hydroquinone in the presence of sodium carbonate and potassium carbonate ( 19: 1, mass ratio) in diphenyl sulfone (DPS). The thermal analysis results of the copolymers show that the glass transition temperatures(Tgs) increase, while the melting temperatures(Tra) and tile 5.0% weight loss temperatures ( Td ) decrease with the increase of the 2,7-naphthalene moieties. For the copolymers synthesized at a molar fraction of 2,7-naphthalene in the difluoro monomers being over 0.30, no peaks corresponding to the cold crystallization temperature and the melting temperature could be detected, indicating that these copolymers are almost amorphous. The crystal structures of the copolymers with a molar fraction of 2,7-naphthalene being less than 0. 30 are rhombic.展开更多
A phosphrous-containing poly(aryl ether ketone) was synthesized derived from bisphenol-A and bis[4-(4- fluorobenzoyl)phenyl] phenyl phosphine oxide (FPPPO) by nucleophilic substitution reaction. The structure of...A phosphrous-containing poly(aryl ether ketone) was synthesized derived from bisphenol-A and bis[4-(4- fluorobenzoyl)phenyl] phenyl phosphine oxide (FPPPO) by nucleophilic substitution reaction. The structure of the polymer was characterized by FT-IR, ^1H-NMR and ^31p-NMR. The thermal property of the PAEK was measured by DSC and TGA. The glass transition temperature (Tg) of the polymer was 205℃, and the 5% weight loss temperature under nitrogen was 475℃. Good solubility of the polymer in organic solvents, such as N-methylpyrrolidone, dimethylformamide, dimethylacetamide, dimethylsulfoxide and chloroalkanes was observed, flexible film was obtained from the polymer's CH2Cl2 solution. The limiting oxygen index (LOI) of the PAEK was 40, which indicated that organic phosphorus moiety can offer good flame retardant property to the polymer.展开更多
A series of Poly(arly ether sulfone ether ketone)s containing pendant methyl groups were synthesized by the reaction of 4,4'-[sulfonylbis (1,4-phenylene)dioxy] dibenzoyl chloride (SODBC) with 4,4'- diphenoxy d...A series of Poly(arly ether sulfone ether ketone)s containing pendant methyl groups were synthesized by the reaction of 4,4'-[sulfonylbis (1,4-phenylene)dioxy] dibenzoyl chloride (SODBC) with 4,4'- diphenoxy diphenylsulfone (DPODPS), 4,4'- di(2-methylphenoxy) diphenylsulfone (o-Me-DPODPS), 4,4'- di(3-methylphenoxy) diphenylsulfone (m-Me-DPODPS), 4,4'- di (2,6-bimethylphenoxy) biphenylsulfone(o-Me2-DPODPS) respectively, in a mixture of 1,2-dichloroethane (DCE) and N-methylpyrrolidone (NMP). These reactions were catalyzed by anhydrous aluminum chloride (AlCl). The characteristic of copolymers were studied by means of advanced analytical techniques such as FT-IR,1H-NMR, DSC, TGA and WAXD. The results show glass transition temperature (Tg) in the range of 193-206℃, thermally stable in excess of 434℃ and excellent solubility in polar solvents. Methyl-substituted Poly(aryl ether sulfone ketone)s had higher glass transition temperatures, lower initial decomposition temperatures than the unsubstituted ones.展开更多
The rheometries ARES rheometer was applied to determining the rheological behavior of a thermotropic liquid crystalline poly (aryl ether ketone). The viscosity of the material decreases with increasing temperature. re...The rheometries ARES rheometer was applied to determining the rheological behavior of a thermotropic liquid crystalline poly (aryl ether ketone). The viscosity of the material decreases with increasing temperature. reaching a minimum in the nematic state, then slightly increases with further raising the temperature in the biphase.展开更多
Soluble reacitve copoly (aryl ether ketone ketone) was synthesized from the condensation of 2.2 ' .3.3 ' .6.6 ' -hexaphenyl-4.4 ' -diphenol. 2.2-p-hydroxyphenl 1-tso-propane. and 1-methyl-cyclohex-1-en...Soluble reacitve copoly (aryl ether ketone ketone) was synthesized from the condensation of 2.2 ' .3.3 ' .6.6 ' -hexaphenyl-4.4 ' -diphenol. 2.2-p-hydroxyphenl 1-tso-propane. and 1-methyl-cyclohex-1-ene-4.5-diyl-bis) (4-fluorophenyl methanone). FT-IR. DSC and TGA were used to characterize the novel polymer.展开更多
High performance polymers have received considerable attention over the past decade owing to their increased demands as replacements for metals or ceramics in automotive, aerospace, and microelectronic industries. Pol...High performance polymers have received considerable attention over the past decade owing to their increased demands as replacements for metals or ceramics in automotive, aerospace, and microelectronic industries. Poly(aryl ether ketone)s(PAEKs) are a class of important high-performance aromatic polymers with excellent mechanical properties, good solvent resistance, size-accuracy, electrical characteristics, and superior thermal stability. However,展开更多
A novel poly (aryl ether ketone) (PPEK) containing phthalazinone and naphthalene moieties was prepared by the nucleophilic displacement reaction of 4-(4-hydroxyphenyl) (2H) phthalazin-1-one with 1-chloro-4-(4-chlorobe...A novel poly (aryl ether ketone) (PPEK) containing phthalazinone and naphthalene moieties was prepared by the nucleophilic displacement reaction of 4-(4-hydroxyphenyl) (2H) phthalazin-1-one with 1-chloro-4-(4-chlorobenzoyl) naphthalene. The polymer was characterized by FTIR, H-1-NMR, DSC, TGA and WAXD.展开更多
A kind of novel heat-resistant, high performance engineering thermoplastic phthalazinone poly(aryl ether sulfone ketone) (PPESK) containing a carboxyl group in its side chain was prepared by the nucleophilic displacem...A kind of novel heat-resistant, high performance engineering thermoplastic phthalazinone poly(aryl ether sulfone ketone) (PPESK) containing a carboxyl group in its side chain was prepared by the nucleophilic displacement reaction of 4-(4-hydroxylphenyl)- 1 (2H)-phthalazinone with di(4-chlorophenyl) sulfone, 4,4'-difluoro-benzophenone and phenolphthalin in sulfolane in the presence of K2CO3 to produce high molecular weight polymers which can be dissolved in some polar solvents such as chloroform and nitrobenzene at room temperature and can be easily cast into flexible, yellowish and transparent films. PPESK is an amorphous polymer having a decomposition temperature above 400degreesC, which indicates that it has high thermal stability. At the same time, the thermal properties of PPESKs with dicyandiamide (DICY) as curing agent indicated that the heat-resistance properties of the PPESKs are improved after curing. The apparent activation energy (A-E) of the cross-linking reaction and the reaction order (n) of PPESK/DICY were found to be 52.2 kJ/mol and ca. 1.0, respectively. Therefore, the cross-linking reaction is approximately a first order reaction.展开更多
A new monomer of 4, 4-biphenyl-bis[4-phthalazin-1(2H)-one] was synthesized from biphenyl and phthalic anhydride, and a novel copoly(aryl ether ketone) (PPEK) was synthesized from 2, 2-bis(4-hydroxyphenyl)-propane (BPA...A new monomer of 4, 4-biphenyl-bis[4-phthalazin-1(2H)-one] was synthesized from biphenyl and phthalic anhydride, and a novel copoly(aryl ether ketone) (PPEK) was synthesized from 2, 2-bis(4-hydroxyphenyl)-propane (BPA), 4, 4'-biphenyl-bis-[4-phthalazin-1(2H)-one], 4, 4- difluorodiphenylketone (DFK). The monomer and copolymer were characterized by FT-IR and 1H-NMR. DSC and TGA were used to the novel polymer.展开更多
In a facile procedure, 2-(1, 3-dithian-2-ylidene)-l-aryl ketones 1 vere reduced with magnesium in methanol to give α-aryl-β -(1, 3-dithane) alcohols 2 in good to high yields.
A new poly (aryl ether ketone) was successfully synthesized by nucleophilic substitution of bis-1,4-(4-chlorobenzoyl) benzene (BCBB) by 1,2-dihydro-4-(4-hydroxy phenyl) (2H)phthatazin-1-one (DHPZ) in appropriate condi...A new poly (aryl ether ketone) was successfully synthesized by nucleophilic substitution of bis-1,4-(4-chlorobenzoyl) benzene (BCBB) by 1,2-dihydro-4-(4-hydroxy phenyl) (2H)phthatazin-1-one (DHPZ) in appropriate condition. The polymer was characterized by FT-IR, H-1-NMR, DSC and TGA etc.展开更多
Two kinds of macrocyclic oligomers containing aromatic sulfide linkages have been synthesized by the solution polycondensation in high yield. The cyclic compounds were characterized by H-1 and C-13 NMR, by and MALDI -...Two kinds of macrocyclic oligomers containing aromatic sulfide linkages have been synthesized by the solution polycondensation in high yield. The cyclic compounds were characterized by H-1 and C-13 NMR, by and MALDI - TOF MS.展开更多
文摘A novel series of poly(aryl ether sulfone ketone)s (PPESKs) containing phthalazinone and biphenyl moieties were prepared by two-step nucleophilic polycondensation reaction. The ^-Mw values of these copolymers were between 38,330 and 67,900. The glass transition temperatures (Tg) and 5% decomposition temperatures were ranged in 253-269 ℃ and 488-500 ℃, respectively, The structures of these copolymers were confirmed by FT-IR and ^1H NMR. Moreover, all the resultant copolymers were amorphous determined by wide angle X-ray diffraction (WAXD).
基金Supported by the National Natural Science Foundation of China(No.5 0 2 0 30 0 4 )
文摘A new monomer, 1,4-bis(4-fluorobenzoyl) naphthalene(compound 2) was synthesized via a two-step reaction. 1,4-Naphthalenedicarboxylic acid chloride(compound 1) was prepared by using the acyl chlorization reaction of 1,4-naphthalenedicarboxylic acid with thionyl chloride. The Friedel-Crafts acylation of compound 1 with fluorobenzene afforded compound 2 in a 80% yield. The polycondensation of compound 2 with various bisphenols in tetramethylene sulfone(TMS) in the presence of excess potassium carbonate as a condensation reagent was carried out at 210 ℃ to quantitatively afford the corresponding poly(aryl ether ketone)s(compounds 3_8) containing 1,4-naphthalene moieties. Thermal analyses showed that the polymers have T g values ranging from 496 to 500 K and are thermally stable in air with initial mass loss above 500 ℃. These novel polymers exhibited an excellent solubility in organic solvents including NMP, DMAc, and chloroform, etc. In addition, the glass transition temperatures of these polymers increased and the polymers became insoluble in chloroform after treated at 260 ℃, indicating the occurrence of a thermal crosslinking reaction.
基金the NSFC(No.20272037),the Doctor's Foundation of Education Ministry of China(No.20030610022)Foundation of Xihua University(No.R0723315) and(No.07ZA109) for the financial support of this work.
文摘In this paper,a series of optically active MeO-BIPHEP-type ligands,(S)-6,6′-dimethoxy-2,2’-bis(di-p-alkoxyphenylphosphine)- 1,1′-biphenyl were synthesized and used to prepare the ruthenium complex.The effects of para-substituted were observed,the results showed that the ruthenium catalysts[diphosphine RuCl;diamine]containing both t-Bu and i-Pr substitutions have better activities and enantioselectivities than the non-substituted ruthenium catalysts in the asymmetric hydrogenation of acetophenone.
基金This work was supported by the National Natural Science Foundation of China.
文摘A new poly(aryl ether ketone) containing biphenylphthalazinone moiety was prepared by the reaction of 4-(4-hydroxybiphenyl) phthalazine-1-one with 4, 4'-difluorobenzophenone. The monomer and the polymer were characterized by FT-IR and H-1-NMR. Some properties of this polymer were described.
文摘A novel heterocyclic poly (aryl ether ketone ketone) (PPEKK) containing cyclohexenering was prepared from 1-methyl-cyclohex-1-ene-4, 5 -diyl-bis(4-chlorophenyl methanone) and 4 (4-hydroxyphenyl)(2H) phthalazin-1-one. The polymer was characterized by FTIR, 1HNMR, DSC,TG and X-ray analysis.
基金This work was supported by the National Natural Science Foundation.
文摘A novel soluble poly(aryl ether ketone) was prepared by the reaction of 4-(3-phenyl-4-hydroxyphenyl)phthalazinone with 4,4'-difluorobenzophenone. The polymer was characterized by DSC, TGA and X-ray diffraction.
文摘Poly( aryl ether ketone) copolymers containing 2,7-naphthylene and hydroquinone(HQ) moieties with various compositions were prepared by the reaction of 4,4'-difluorobenzophenone(DFB) 2,7-naphthylene and hydroquinone in the presence of sodium carbonate and potassium carbonate ( 19: 1, mass ratio) in diphenyl sulfone (DPS). The thermal analysis results of the copolymers show that the glass transition temperatures(Tgs) increase, while the melting temperatures(Tra) and tile 5.0% weight loss temperatures ( Td ) decrease with the increase of the 2,7-naphthalene moieties. For the copolymers synthesized at a molar fraction of 2,7-naphthalene in the difluoro monomers being over 0.30, no peaks corresponding to the cold crystallization temperature and the melting temperature could be detected, indicating that these copolymers are almost amorphous. The crystal structures of the copolymers with a molar fraction of 2,7-naphthalene being less than 0. 30 are rhombic.
基金This work was supported by the National Natural Science Foundation of China(No.50203008).
文摘A phosphrous-containing poly(aryl ether ketone) was synthesized derived from bisphenol-A and bis[4-(4- fluorobenzoyl)phenyl] phenyl phosphine oxide (FPPPO) by nucleophilic substitution reaction. The structure of the polymer was characterized by FT-IR, ^1H-NMR and ^31p-NMR. The thermal property of the PAEK was measured by DSC and TGA. The glass transition temperature (Tg) of the polymer was 205℃, and the 5% weight loss temperature under nitrogen was 475℃. Good solubility of the polymer in organic solvents, such as N-methylpyrrolidone, dimethylformamide, dimethylacetamide, dimethylsulfoxide and chloroalkanes was observed, flexible film was obtained from the polymer's CH2Cl2 solution. The limiting oxygen index (LOI) of the PAEK was 40, which indicated that organic phosphorus moiety can offer good flame retardant property to the polymer.
基金This work was supported by National Science Foundation of China (No. 20264001 ), National Science Foundation of Jiangxi Province, Innovation Fund for Technology Based Firms of China (No. 06C26213601342).
文摘A series of Poly(arly ether sulfone ether ketone)s containing pendant methyl groups were synthesized by the reaction of 4,4'-[sulfonylbis (1,4-phenylene)dioxy] dibenzoyl chloride (SODBC) with 4,4'- diphenoxy diphenylsulfone (DPODPS), 4,4'- di(2-methylphenoxy) diphenylsulfone (o-Me-DPODPS), 4,4'- di(3-methylphenoxy) diphenylsulfone (m-Me-DPODPS), 4,4'- di (2,6-bimethylphenoxy) biphenylsulfone(o-Me2-DPODPS) respectively, in a mixture of 1,2-dichloroethane (DCE) and N-methylpyrrolidone (NMP). These reactions were catalyzed by anhydrous aluminum chloride (AlCl). The characteristic of copolymers were studied by means of advanced analytical techniques such as FT-IR,1H-NMR, DSC, TGA and WAXD. The results show glass transition temperature (Tg) in the range of 193-206℃, thermally stable in excess of 434℃ and excellent solubility in polar solvents. Methyl-substituted Poly(aryl ether sulfone ketone)s had higher glass transition temperatures, lower initial decomposition temperatures than the unsubstituted ones.
基金the National Advanced Materials Committee of China (NAMCC) is gratefully acknowledged.
文摘The rheometries ARES rheometer was applied to determining the rheological behavior of a thermotropic liquid crystalline poly (aryl ether ketone). The viscosity of the material decreases with increasing temperature. reaching a minimum in the nematic state, then slightly increases with further raising the temperature in the biphase.
基金We thank the national "Ninth 5-year Plan" key project for the financial support.
文摘Soluble reacitve copoly (aryl ether ketone ketone) was synthesized from the condensation of 2.2 ' .3.3 ' .6.6 ' -hexaphenyl-4.4 ' -diphenol. 2.2-p-hydroxyphenl 1-tso-propane. and 1-methyl-cyclohex-1-ene-4.5-diyl-bis) (4-fluorophenyl methanone). FT-IR. DSC and TGA were used to characterize the novel polymer.
基金Supported by the National High Technology Research and Development Program of China(No.2006AA03Z543).
文摘High performance polymers have received considerable attention over the past decade owing to their increased demands as replacements for metals or ceramics in automotive, aerospace, and microelectronic industries. Poly(aryl ether ketone)s(PAEKs) are a class of important high-performance aromatic polymers with excellent mechanical properties, good solvent resistance, size-accuracy, electrical characteristics, and superior thermal stability. However,
基金Thanks to the "Ninth 5-year Plan" key project of the state.
文摘A novel poly (aryl ether ketone) (PPEK) containing phthalazinone and naphthalene moieties was prepared by the nucleophilic displacement reaction of 4-(4-hydroxyphenyl) (2H) phthalazin-1-one with 1-chloro-4-(4-chlorobenzoyl) naphthalene. The polymer was characterized by FTIR, H-1-NMR, DSC, TGA and WAXD.
基金This project was supported by the National Ninth Five-Year-Plan Key Project "The pilot-scale production and the applied development of polyaryl ether concerning phthalazinone moiety" (No. 97-564-01-07).
文摘A kind of novel heat-resistant, high performance engineering thermoplastic phthalazinone poly(aryl ether sulfone ketone) (PPESK) containing a carboxyl group in its side chain was prepared by the nucleophilic displacement reaction of 4-(4-hydroxylphenyl)- 1 (2H)-phthalazinone with di(4-chlorophenyl) sulfone, 4,4'-difluoro-benzophenone and phenolphthalin in sulfolane in the presence of K2CO3 to produce high molecular weight polymers which can be dissolved in some polar solvents such as chloroform and nitrobenzene at room temperature and can be easily cast into flexible, yellowish and transparent films. PPESK is an amorphous polymer having a decomposition temperature above 400degreesC, which indicates that it has high thermal stability. At the same time, the thermal properties of PPESKs with dicyandiamide (DICY) as curing agent indicated that the heat-resistance properties of the PPESKs are improved after curing. The apparent activation energy (A-E) of the cross-linking reaction and the reaction order (n) of PPESK/DICY were found to be 52.2 kJ/mol and ca. 1.0, respectively. Therefore, the cross-linking reaction is approximately a first order reaction.
基金This work is sponsored by the National Natural Science Foundation of China (No. 59473901).
文摘A new monomer of 4, 4-biphenyl-bis[4-phthalazin-1(2H)-one] was synthesized from biphenyl and phthalic anhydride, and a novel copoly(aryl ether ketone) (PPEK) was synthesized from 2, 2-bis(4-hydroxyphenyl)-propane (BPA), 4, 4'-biphenyl-bis-[4-phthalazin-1(2H)-one], 4, 4- difluorodiphenylketone (DFK). The monomer and copolymer were characterized by FT-IR and 1H-NMR. DSC and TGA were used to the novel polymer.
文摘In a facile procedure, 2-(1, 3-dithian-2-ylidene)-l-aryl ketones 1 vere reduced with magnesium in methanol to give α-aryl-β -(1, 3-dithane) alcohols 2 in good to high yields.
文摘A new poly (aryl ether ketone) was successfully synthesized by nucleophilic substitution of bis-1,4-(4-chlorobenzoyl) benzene (BCBB) by 1,2-dihydro-4-(4-hydroxy phenyl) (2H)phthatazin-1-one (DHPZ) in appropriate condition. The polymer was characterized by FT-IR, H-1-NMR, DSC and TGA etc.
文摘Two kinds of macrocyclic oligomers containing aromatic sulfide linkages have been synthesized by the solution polycondensation in high yield. The cyclic compounds were characterized by H-1 and C-13 NMR, by and MALDI - TOF MS.