• Macromolecular Research
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• 제13권1호
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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.

• 공업화학
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• 제10권5호
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• pp.767-771
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• 1999

내열성 전기 절연 coating에 사용되는 기본 수지인 poly(ester-imide) (PEI)의 1단계 및 2단계 합성법을 비교하였으며 촉매의 영향도 조사하였다. Poly(ester-imide) 수지의 합성에 있어서 trimellitic anhydride(TMA)와 methylene dianiline(MDA)으로부터 imide 반복 단위를 구성하는 N,N'-(4,4'-diphenylmethane)bistrimellitimide(DID)를 먼저 합성하고 에스테르화 반응을 시키는 2단계법과 TMA, MDA, dimethyl terephthalate(DMT) 및 ethylene glycol(EG), 1,3,5-tris-(2-hydroxy ethyl)isocyanurate(THEIC)를 모두 m-cresol 용매에 넣고 반응시키는 1단계법이 동등한 PEI 수지를 생성함을 확인할 수 있었다. 합성된 poly(ester-imide) 수지 용액에 xylene, phenol-formaldehyde 수지인 P-5030K, TDI type blocked isocyanate인 TK-8 및 tetrapropyltitanate(TPT)를 첨가하여 경화 반응을 시키고 생성된 피막의 유연성 및 투명도를 조사한 결과 히드록실기의 함량, DMT의 첨가 및 imide 반복 단위의 함량이 내열성 절연 코팅의 물성에 중요한 인자로 작용함을 알 수 있었다.

• 공업화학
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• 제10권1호
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• pp.138-142
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• 1999

Imide 단위를 포함하는 diamine과 dicarboxylic acid 단량체들, N-(4-aminophenyl)-4-aminophthalimide(APAP), N-(4-carboxyphenyl)-4-carboxyphthalimide(CPCP), N,N'-oxydiphenylenebis(4-aminophthalimide)(ODPAP), 그리고 N,N'-oxydiphenylenebis(4-carboxy-phthalimide)(ODPCP)를 합성하였다. 상기 디아민을 포함한 단량체들과 디카르복시산을 포함한 단량체들을 서로 축합반응하여 imide 단위가 교대로 치환된 poly(imide-amide)s를 합성하였다. 또한 imide단위를 포함하는 diamine 단량체들과 terephthaloyl chloride, 그리고 isophthaloyl chloride를 축합하여 poly(imide-amide)s들도 합성하였다. 이렇게 합성된 중합체들은 NMP/LiCl용액에 매우 잘 용해하였으나 그밖에 극성 비양자성 극성 용매인 DMF, DMSO, 그리고 DMAc 등에는 $80^{\circ}C$에서도 작은 용해도를 보여주었다. 그밖에 고유점도는 0.18~0.67 dL/g를 보여주었으며 NMP/LiCl 용액으로부터 단단하고 부서지기 쉬운 막이 형성되었다. 중합체들은 $500^{\circ}C$ 이하에서 유리 전이 온도 및 융점은 관찰되지 않았으며 열 중량 분석에서 10% 중량 감량은 $500^{\circ}C$ 부근에서 나타나 우수한 열적 성질을 보여주었다.

• Fibers and Polymers
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• 제2권2호
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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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• 제3권2호
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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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• 제12권3호
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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.

• 한국응용과학기술학회지
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• 제27권2호
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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.

• 한국전기전자재료학회논문지
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• 제20권1호
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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.

• 폴리머
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• 제36권4호
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• pp.427-433
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• 2012

이미드/아라미드/설폰기가 교대로 도입된 poly(imide-aramid-sulfone)s을 divinyl sulfone(DVS)과 $N^1,N^4$-bis(4-(vinylsulfonyl)phenyl)terephthalamide (2)를 pyromellitic diimide와 반응하여 높은 수율로 제조하였다. 또한 고분자를 닮은 3가지 모델 화합물인 N-[2-(p-aminophnenylsulfonyl)ethyl]phthalimide (3), 2,2'-(2,2'-sulfonylbis(ethane-2,1-diyl))diisoindoline-1,3-dione (4), 및 N,N-bis(4-(2-(1,3-dioxoisoindolin-2-yl)ethylsulfonyl)phenyl)terephthalamide (5)을p-aminophenyl vinyl sulfone, DVS, 2와 phthalimide와 반응하여 얻었다. 축합 중합은 phthalimide 기와 DVS의 마이클 첨가 반응에 의하여 균일 용액으로 진행되며 tetrabutylammonium hydroxide (TBAH)가 촉매로 작용하여 poly(imide-aramid-sulfone)s 6-12의 분자량이 큰 중합체를 얻을 수 있었다. DVS/2의 구성비는 1/0, 3/1, 2/1, 1/1, 1/2, 1/3, 및 0/1이다. 얻어진 고분자들은 극성 용매인 N,N-dimethylformamide, dimethylsulfoxide, N-methylpyrrolidinone 및 tetrahydrofuran에 잘 용해하였다. 그 밖에 분자량, 점도 그리고 열적 성질을 평가하였다.

• Korean Membrane Journal
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• 제6권1호
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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.