• 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.

• 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.

• 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 $500^{\circ}C$.

• Fibers and Polymers
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• v.2 no.2
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• pp.92-97
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• 2001

New film forming aromatic poly(amide-imide)s containing isoindoloquinazolinedione (IQ) unit in the backbone chain (polymer XIV) have been successfully synthesized by preparing prepolymers of poly(amic acid-carbonamide). followed by subsequent thermal cyclization of the prepolymers. 4,4-Diamino-3-carbamoylbenzanilide (DACB) V has been synthesized by reduction of 3-carbamoyl-4-amino-4-nitrobenzanilide IV. The prepolymers of poly(amic-acid-carbonamide) (polymers VII and VIII) which exhibit viscosities ranging from 1.4 to 1.7 dl/g have been prepared by a condensation polymerization of monomers such as BPDA, ODA, and DACB. Polymer XIV has been obtained by thermal cyclization of the polymers VII and VIII. During the thermal cyclization reaction, imide ring structure was first introduced and then transformed to the structure of IQ unit. The thermal degradation rate of the resultant polymers were influenced by the cleavage of amide bond but the final char yield was comparable to that of poly(BPDA-ODA).

• 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.

• 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.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.20 no.1
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• pp.35-40
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• 2007

The new PEI(poly(epoxy-imide))-nano Silica film has been synthesized via in situ CS sol process, and the chemical bonding and microstructure of nano silica dispersed in resin were examined by FT-IR, TAG and SEM. The dielectric properties of these hybrid films over a given temperature and frequency ranges have been studied in a point of view of stable chemical bonding of nano Silica filler. The results from IR spectra and SEM photograph indicated that PEI-Silica hybrid film prepared with nano CS sol process has been synthesized in uniform and chemical bonding. The decrease property of dielectric constant with CS content, tangent loss consistent of given frequency and temperature has been explained in terms of the chain movement of polymer through chemical bonging and size effect of nano silica. The new PEI-CS sol hybrid film with such stable chemical and dielectric properties was expected to be used as a high functional coating application in ET, IT and electric power products.

• Polymer(Korea)
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• v.36 no.4
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• pp.427-433
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• 2012

A series of poly(imide-aramid-sulfone)s with alternatingly introduced imide/aramid groups were prepared by reacting divinyl sulfone (DVS) and $N^1,N^4$-bis(4-(vinylsulfonyl)phenyl)terephthalamide (2) with pyromellitic diimide. Three model compounds, N-[2-(p-aminophnenylsulfonyl)ethyl]phthalimide (3), 2,2'-(2,2'-sulfonylbis(ethane-2,1-diyl))diisoindoline-1,3-dione (4), and N,N-bis(4-(2-(1,3-dioxoisoindolin-2-yl)ethylsulfonyl)phenyl)terephthalamide (5), resembling polymers were prepared with good yields by reacting p-aminophenyl vinyl sulfone, DVS, and 2 with phthalimide. Condensation polymerization was carried out by Michael-type addition reaction of the difunctional phthalimide group with the DVS group in the presence of tetrabutylammonium hydroxide (TBAH), resulting in poly(imide-aramid-sulfone)s 6-12 with moderate molecular weights and good yields. They were highly soluble in polar solvents such as N,N-dimethylformamide, dimethylsulfoxide, N-methylpyrrolidinone and tetrahydrofuran. The ratios of DVS/2 were 1/0, 3/1, 2/1, 1/1, 1/2, 1/3, and 0/1. Molecular weight and physical properties such as solubility, viscosity, and thermal properties of the polymers were examined.

• Korean Membrane Journal
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• v.6 no.1
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• pp.16-23
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• 2004

The silica containing carbon (C-SiO$_2$) membranes were fabricated using poly(imide siloxane) (PIS) having -CO- swivel group. The characteristics of porous C-SiO$_2$ structures prepared by the pyrolysis of poly(imide siloxane) were related with the micro-phase separation between the imide block and the siloxane block. Furthermore, the nitrogen adsorption isotherms of the CMS and the C-SiO$_2$ membranes were investigated to define the characteristics of porous structures. The C-SiO$_2$ membranes derived from PIS showed the type IV isotherm and possessed the hysteresis loop, which was associated with the mesoporous carbon structures, while the CMS membranes derived from PI showed the type I isotherm. For the molecular sieving probe, the C-SiO$_2$ membranes pyrolyzed at 550, 600, and 700$^{\circ}C$ showed the O$_2$ permeability of 924, 1076, and 367 Barrer (1 ${\times}$ 10$\^$-10/㎤(STP)cm/$\textrm{cm}^2$$.$s$.$cmHg) and O$_2$/N$_2$ selectivity of 9, 8, and 12.