• Journal of the Korean Applied Science and Technology
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• v.25 no.2
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• pp.144-150
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• 2008

The polyamide-amide-imide (PAAI) was synthesized by reacting 4,4'-diaminobenzanilide (DBA) with trimellitic anhydride chloride using a two-stage heating. The precursor of polyamide-acids was formed at first stage and followed by the formation of imide of PAAI. Two polyamide-imides (PAIs) were prepared from benzidine (BZ) or 4,4'-diaminodiphenylether (DPE) with trimellitic anhydride chloride. These three polymers had glass transition temperature in the temperature range of $240-250^{\circ}C$. X-ray data were obtained on thin film specimens cured at $250^{\circ}C$. There was a minimal kind of short-range order consisting of the most probable distances between neighboring chains. The average segmental spacing of short-range order decreased in the order of polymers obtained from 4,4'-diaminobenzanilide (DBA), polyamide-imide, and 4,4'-diaminodiphenylether (DPE). The imidization of three polyamide-imides was confirmed by $^{15}N$ MAS NMR and FT-IR spectroscopy. $^{15}N$ NMR spectrum of cured polyamide-imide showed imide $^{15}N$ peak, thereby providing an evidence for the imidization of three polyamide-imides.

• Applied Chemistry for Engineering
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• v.10 no.1
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• pp.138-142
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• 1999

Imide-containing diamine and dicarboxylic acid monomers, N-(4-aminophenyl)-4-aminophthalimide(APAP), N-(4-carboxyphenyl)-4-carboxyphthalimide(CPCP), N,N'-oxydiphenylenebis(4-aminophthalimide)(ODPAP) and N,N'-oxydiphenylenebis(4-carboxyphthalimide)(ODPCP) were prepared. Poly(amide-imide)s were prepared by condensation reaction of the diamine and the dicarboxylic acid monomers. Poly(amide-imide)s were also prepared from the diamine monomers and aromatic acid chlorodes such as terephthaloyl chloride and isophthaloyl chloride. The polymers possess inherent viscosity of 0.18~0.67 dL/g and brittle films were cast from NMP/LiCl solution. The poly(amide-imide)s are easily soluble in NMP/LiCl and also partially soluble in polar aprotic solvents such as DMF, DMSO, NMP and DMAc even at $80^{\circ}C$. DSC traces of polymers showed no glass transition temperature and melting temperature, and TGA traces showed a 10% weight loss at $500^{\circ}C$.

• Applied Chemistry for Engineering
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• v.10 no.5
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• pp.767-771
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• 1999

Poly(ester-imide)(PEI) for the electrical insulation coating was synthesized and evaluated with one-step method as well as two-step method. For the synthesis of poly(ester-imide), imide repeat unit of N,N'-(4,4'-diphenylmethane) bistrimellitimide(DID) was initially made from trimellitic anhydride(TMA) and methylene dianiline(MDA), followed by the second stage reaction of esterification. One-step reaction was performed by reaction of TMA, MDA, dimethyl terephthalate(DMT), ethylene glycol(EG), and 1,3,5-tris-(2-hydroxy ethyl) isocyanurate(THEIC) in m-cresol solvent at a time. The synthesized poly(ester-imide) was cured with xylene, P-5030K(phenol-formaldehyde resin), TK-8(TDI type blocked polyisocyanate) and tetrapropyltitanate(TPT). It was found that the content of hydroxyl group, amount of DMT, and imide repeat unit played important role for the properties of electrical insulation coating film.

• Macromolecular Research
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• v.13 no.1
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• pp.14-18
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• 2005

Under irradiation in a microwave oven, six novel poly(amide-imide)s containing tetrahydropyrimidinone, tetrahydro-2-thioxopyrimidine moieties and trimellitic rings in their main chains were synthesized through the polycondensation reaction of N,N'-(4,4'-diphenylether)bis(trimellitimide) diacid chloride with six different derivatives of tetrahydropyrimidinone and tetrahydro-2-thioxopyrimidine in the presence of a small amount of a polar organic medium, such as o-cresol. The polycondensation proceeded rapidly and completed within 7-9 min, producing a series of new poly(amide-imide)s in high yield that showed inherent viscosities in the range 0.33-0.52 dL/g. These poly(amide-imide)s were characterized by elemental analysis, viscosity measurement, thermal gravimetric analysis, solubility test, and FT-IR spectroscopy. All of the polymers were soluble at room temperature in polar solvents such as N,N-dimethylacetamide, N,N-dimethylformamide, dimethylsulfoxide, tetrahydrofuran, and N-methyl-2-pyrrolidone.

• Korean Membrane Journal
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• v.3 no.1
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• pp.24-31
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• 2001

Ultrafiltration membranes base on copoly(amide-imide) derivatives were prepared by the phase inversion method and the factors determining the permeation characteristics of membrane were investigated. The permeation behavior was observed by the relative ratio of permeate flux (J$\_$t/)/pure water flux (J$\_$o/). The characteristics through membrane were measured using aqueous solution of poly(ethyleneglycol) (MW 2.0$\times$10$\^$4/) over a temperature range of 10∼90$\^{C}$. With increasing the operating temperature, the relative ratio of flux became high. All the membranes had good chemical stability. Copoly(amide-imide) membranes having various Permeation properties could be obtained. Further, it was proved that the membrane performances could be determined from the preparation conditions as well as various operating conditions.

• Korean Chemical Engineering Research
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• v.48 no.1
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• pp.45-52
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• 2010

Two different imide oligomers(6FDA-ODA/APA and 6FDA-MDA/MA) having crosslinkable end groups were prepared by using a solution imidization method and their properties were investigated. Also, semi-interpenetrating polymer networks(semi-IPN) were prepared using the blends of imide oligomers with polyetherimide $Ultem^{(R)}$, which is used in dual-ovenable packaging materials. The characteristic properties of semi-IPN films were interpreted by using TGA, Thin Film Diffusion Analyzer, and WAXD. Molecular weights of imide oligomers were successfully controlled utilizing 2-aminophenylacetylene(APA) and maleic anhydride(MA) as an endcapping agent. Exotherm reactions by crosslinking appeared and the amount of exthotherm heat was linearly increased as the content of imide oligomers was increased. For semi-IPNs of $Ultem^{(R)}$ and imide oligomers, 5% and 10% weight loss temperatures increased as the contents of imide oligomers were increased. Diffusion coefficient and water uptake of semi-IPNs decreased as the content of imide oligomers was increased, which might be resulted from hydrophobic fluorine group and high packing density. It was concluded that relatively low thermal stability and hydrolytic stability of polyetherimide $Ultem^{(R)}$ were improved by incorporating new developed imide oligomers.

• Rapid Communication in Photoscience
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• v.1 no.1
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• pp.19-20
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• 2012

Novel star-shaped imide compounds containing electron-donating triphenylamine and/or electron-withdrawing bis(trifluoromethyl)phenyl side groups were synthesized via a two-step process. First, 3,6-dibromo-benzene-1,2,4,5-tetracarboxylic acid (2B4BA) was reacted with 4-aminophenyl (diphenylamine) (ATPA) or 3,5-bis(trifluoromethyl)aniline (6FA) by imide reaction. Then, Suzuki coupling reaction was carried out on these compounds with 4-(N,N-diphenylamino)-1-phenyl boronic acid (BTPA) or 3,5-bis(trifluoromethyl)phenyl boronic acid (6FBB), resulting in 3,6-bis[4-(diphenylamino)phenyl]-N,N'-bis[4-(diphenylamino) phenyl]-pyromellitimide (TPTPPI), 3,6-bis[3,5-bis(trifluoro methyl) phenyl]-N,N'-bis[3,5-bis(trifluoromethyl) phenyl]-pyro mellitimide (6F6FPI) or 3,6-bis[4-(diphenylamino)phenyl]-N,N'-bis[3,5-bistrifluoromethyl)phenyl]-pyromellitimide (6FTPPI). The imide compounds obtained were characterized by NMR, FT-IR, DSC, TGA, melting point analyzer, EA, and solubility measurements. In addition, their optical and electrical properties were evaluated by fluorescence spectroscopy, UV-vis spectroscopy, and cyclic voltammetry (CV). 6F6FPI exhibited deep blue emission (443 nm), along with high $T_m$ ($382^{\circ}C$) and relatively high $T_g$ ($148^{\circ}C$).

• Journal of the Korean Applied Science and Technology
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• v.27 no.2
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• pp.129-136
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• 2010

A series of noble poly(amide-imide)s and copoly(amide-imide)s bearing 1,2-bis(4-phenoxy)benzene units were synthesized by the direct polycondensation of 1,2-bis(4-trimellitimidophenoxy)benzene[1,2-PTPB] with a combination of commercially available aromatic diamines and diacids such as m-phenylene diamine, p-phenylene diamine(PPD), isophthalic acid and terephthalic acid(TA) in N-methyl-2-pyrrolidone(NMP) using triphenyl phosphite and pyridine as a condensing agent in the presence of dehydrating agent ($CaCl_2$). The resulting polymers had inherent viscosities in the range of 0.37~0.78 dL/g and most of them were soluble m common organic solvents including NMP, dimethylacetamide, dimethylsulfoxide, dimethylformamide, and m-cresol. Wide-angle X-ray diffractograms revealed that the copoly(amide-imide) derived from PPD with mixed acids of 1,2-BTPB and TA, showed crystalline nature, whereas all of the other polymers were found to be amorphous. The glass transition temperatures of the polymers occurred over the temperature range of $270{\sim}323^{\circ}C$ in their differential scanning calorimetry curves and their 10% weight loss temperature, determined by thermogravimetric analysis in air and nitrogen atmosphere, were in the range $465{\sim}535^{\circ}C$, $500{\sim}550^{\circ}C$, respectively, indicating their good thermal stability.

• Fibers and Polymers
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• v.3 no.2
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• pp.55-59
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• 2002

The thermal reaction of acetoacetanilide in the presence of aniline or phenol yielded carbanilide in quantitative yields. This reaction was applied to the synthesis of polyurea. Bisacetoacetamides were prepared from diamines and diketene in DMF. They were thermally polymerized in the presence of phenol or a diamine (6FDA) to yield polyureas of low molecular weights. The polymers were soluble in DMSO and NMP. $^1{H-NMR}$ analysis showed that they had amino group terminated structures. Poly(urea-imide) was synthesized by the reaction of an oligourea diamine with pyromellitic dianhydride in NMP. The concentration of terminal amino groups was determined by an acid-base titration. The thermal property of poly(urea-imide) was evaluated by thermogravimetric analysis (TGA). Initial decompisition took place at 332-$350^{\circ}C$.

• Macromolecular Research
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• v.12 no.3
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• pp.258-262
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• 2004

We have developed facile and rapid polycondensation reactions of N-trimellitylimido-L-leucine diacid chloride 1 with eight different derivatives of hydantoin compounds 2a-h, in the presence of a small amount of a polar organic medium, such as Ο-cresol, by using a domestic microwave oven. The polycondensation reactions proceeded rapidly-they were complete within 7-9 min-to produce a series of novel optically active poly(amide-imide)s (3a-h) in high yield with inherent viscosities of 0.33-0.51 dL/g. We characterized the resulting poly(amide-imide)s by elemental analysis, thermal gravimetric analysis (DSC, TGA, and DTG), and FTIR spectroscopy, and by measuring their viscosities, specific rotations, and solubilities. All of the polymers were soluble at room temperature in polar solvents such as N ,N-dimethylacetamide, N,N-dimethylformamide, dimethylsulfoxide, tetrahydrofuran, and N-methyl-2-pyrrolidone.