• Title/Summary/Keyword: Acid anhydride

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Polyimide Films Using Dianhydride Containing Ester Linkages and Various Amine Monomers (에스터기를 가지는 무수물과 다양한 아민 단량체를 이용한 폴리이미드 필름)

  • Choi, Chang Hwon;Chang, Jin-Hae
    • Polymer(Korea)
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    • v.37 no.5
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    • pp.618-624
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    • 2013
  • Hydroquinone bis(trimellitic anhydride) (HQ-TA) was synthesized from trimellitic anhydride chloride and hydroquinone. Poly(amic acid)s (PAAs) were synthesized by reacting a HQ-TA with six different diamines, which were cyclized to yield polyimides (PIs) containing ester linkages by chemical- and thermal-imidization methods. The various PIs were synthesized from structurally different aromatic diamines. The glass transition temperatures ($T_g$) were in the range of 167-$215^{\circ}C$, and the decomposition temperatures (${T_D}^i$) were in the range of $364-451^{\circ}C$. The maximum improvements in coefficient of thermal expansion (CTE) and barrier to oxygen permeation were observed in PIs using TFB (3.23 $ppm/^{\circ}C$) and 4,4-ODA (< $10^{-2}cc/m^2/day$), respectively. The PI films possessed a transmittance of 65-89% at 500 nm and had a yellowish color with a yellow index (YI) of 3.01-69.52.

Preparation of 2,3,4,5-Tetrafluorobenzoic Acid (2,3,4,5-Tetrafluorobenzoic Acid의 합성)

  • Li, Hua;Wang, Hongkai;Zhao, Ruiju;Liu, Juan;Zhao, Zhengui;Hu, Guoqin;Liang, Zhengyong
    • Journal of the Korean Chemical Society
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    • v.54 no.6
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    • pp.744-748
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    • 2010
  • 2,3,4,5-Tetrafluorobenzoic acid, an important intermediates of fluoroquinolone antibiotics, was synthesized from tetrachloride phthalic anhydride through imidation, fluorination, hydrolysis and decarboxylation. The effects of phase transfer catalyst on imidation and fluorination reaction and the effects of surfactants on the hydrolysis reaction were studied, respectively. Experimental results showed that the imidation reaction time was greatly reduced in the presence of a phase transfer catalyst, hexadecyltrimethyl, resulting in imidation yield as high as 98.2%. The fluorination yield reached 81.3% when tetrabutylammonium bromide was chosen as a phase transfer catalyst. The hydrolysis reaction time was also decreased by adding hexadecyltrimethyl while increasing the yield to 88.6%. In the post-processing, the sublimation method was used to purify the product, and ideal effect was obtained. In the decarboxylation reaction, tetrafluoride phthalic acid was obtained by decarboxylation in the solvent of tri-n-butyl amine and decarboxylation yield reached 81.6%. Compared with the literature method, the overall reaction time of the improved method decreased from 53 h to 20.5 h and the total yield increased from 47.3% to 57.4%.

A Study on the Acid Property and the Activity of Xylene Oxidation Catalyst (자일렌 산화반응 촉매의 산특성과 반응성에 관한 연구)

  • Kim, Taek-Joong;Kim, Young-Ho;Lee, Ho-In
    • Applied Chemistry for Engineering
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    • v.2 no.4
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    • pp.330-339
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    • 1991
  • The acid properties of $V_2O_5-TiO_2/SiO_2$ catalysts and the partial oxidation of o-xylene into phthalic anhydride had been investigated in order to relate the acid property of catalyst to the catalytic activity. $V_2O_5$ had both weak (V=O) and strong (V-O-V) acid sites which gave pyridine desorption peaks at $230^{\circ}C$ and $300^{\circ}C$, respectively, and the amount of weak acid sites at $230^{\circ}C$ decreased with the increase of calcination temperature. On the other hand, the amount of weak acid sites increased considerably by increasing the amount of $TiO_2$ to the $V_2O_5-TiO_2/SiO_5$, and the maximum value was shown at 20 and higher mole % of $TiO_2$ with respect to $SiO_2$. In the oxidation of o-xylene, $V_2O_5-TiO_2/SiO_2$ enhandced more the total conversion and the selectivity to phthalic anhydride than $V_2O_5/SiO_2$, and the higher $TiO_2$ ratio to $V_2O_5$ increased the total conversion but could not change the selectivity to phthalic anhydride. Weak acid sites (V=O) led o-xylene to partial oxidation producing phthalic anhydride by adsorbing o-xylene weakly, while acid sites (V-O-V) led it to total oxidation producing CO and $CO_2$ by adsorbing it strongly.

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Hydrolytic Stability of Sulfonic Acid-Containing Polyimides for Fuel Cell Membranes

  • Kim Hyoung-Juhn;Litt Morton H.;Shin Eun-Mi;Nam Sang Yong
    • Macromolecular Research
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    • v.12 no.6
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    • pp.545-552
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    • 2004
  • The long-term stability of sulfonic acid-containing polyimides has been investigated. The hydrolytic degradation of homopolyimide and the block copolyimide comprising $27\;mol\%$ of 2,2'-bis(trifluoromethyl)benzidine and $9\;mol\%$ of m-phenylenediamine (BTFMB27mPl0[7/(3+1)]), was quantified through viscosity measurements and FT-IR spectroscopic analyses. The viscosity decrease with respect to time and the degradation rate were similar. The degrees of degradation with respect to time under ambient conditions and at elevated temperature in water were monitored by FT-IR spectroscopy. A new absorption peak was observed at $1786\;cm^{-1},$ which we corresponds to the presence of anhydride end groups formed by hydrolytic scission of the imide rings.

A Facile Reduction of Acid Anhydrides with Borane in the Presence of Lithium Chloride in Tetrahydrofuran

  • Yoon, Nung-Min;Lee, Whee-Seong
    • Bulletin of the Korean Chemical Society
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    • v.7 no.4
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    • pp.296-298
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    • 1986
  • Carboxylic acid anhydrides are rapidly reduced with borane-lithium chloride (1:0.1) system to give corresponding alcohols (diols in the case of cyclic anhydride) quantitatively in tetrahydrofuran at room temperature. This reagent tolerates aromatic acid ester, nitro, and halide functional groups, however competitively reduces aliphatic ester and nitrile groups.

Improvement on the Reactivity Properties with Tannic Acid of Yellowfin Sole Skin Gelatin by Succinylation (숙시닐화에 의한 각시가자미껍질 젤라틴의 탄닌산과의 반응성 개선)

  • Cho, Soon-Yeong;Ha, Jin-Hwan;Lee, Jung-Suck;Lee, Eung-Ho;Kim, Jin-Soo
    • Applied Biological Chemistry
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    • v.38 no.5
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    • pp.393-397
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    • 1995
  • With a view to utilizing fish skin gelatin as a clearifier or chewing gum base, yellowfin sole skin gelatin was succinylated. Up to 10% succinic anhydride to gelatin, the succinylation degree of gelatin was increased linear and above this concentration a nearly constant value was reached. The succinylated gelatin treated with 15% succinic anhydride to gelatin was examined on the reactivity properties with tannic acid in the experiment. Succinylation degree of the gelatin was about 80%. Succinylation shifted the apparent isoelectric point from pH 5.54 in untreated gelatin to pH 4.08 in succinylated gelatin. The proximate composition and amino acid composition of succinylated gelatin were similar to those of untreated gelatin. However Lysine composition for succinylated gelatin was lower than for untreated gelatin. The ratio of precipitated gelatin and tannic acid became maximum at pH 4.8 in untreated gelatin, at pH 4.0 in succinylated gelatin. Regardless of the difference between untreated and succinylated gelatins, the ratio of precipitated gelatin decreased with concentration of gelatin. The ratio of precipitated tannic acid was the highest by adding $2{\sim}4$ times in succinylated gelatin to tannic acid weight, by adding $2{\sim}3$ times in untreated gelatin. The ratios of precipitated succinylated gelatin and tannic acid were scarcely affected by the presence of sucrose, however, were affected by the presence of ethyl alcohol.

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Synthesis and Properties of Photocurable Dipentaerythritol Modified Polymethacrylates (광경화형 Dipentaerythritol 변성 폴리메타아크릴레이트의 합성과 물성)

  • Kim, Dong Kook;Lim, Jin Kyu;Kim, Woo Geun;Haw, Jung Rim
    • Applied Chemistry for Engineering
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    • v.16 no.1
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    • pp.101-106
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    • 2005
  • Photocurable modified 6 functional polyacrylate(PA-1) were prepared from dipentaerythritol derivatives (DPET) and acrylic acid, and 12 functional polymethacrylate(PA-2) were prepared from dipentaerythritol derivatives (DPET), trimellitic anhydride, and glycidyl methacrylate. And physical properties of photocurable modified poly(meth)acrylate were increased with increasing functionality of (meth)acrylate. Thermal stability of UV cured film obtained by using TGA was shifted to higher temperature as the increasing of functionality. Hardness, abrasion resistance and tensile strength of UV cured film were increased with increasing functionality of (meth)acrylate. Values of yellow index were increased with increasing functionality of (meth)acrylate.

Effects of acid-anhydride hardener and postcuring heat-treatments on dielectric properties of epoxy composites (에폭시 복합체의 유전특성에 미치는 산무수물 경화제와 후경화 열처리의 영향)

  • 왕종배;이성일;이준웅
    • Electrical & Electronic Materials
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    • v.7 no.3
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    • pp.187-199
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    • 1994
  • In order to find an effect of structural changes due to variation of addition ratio of anhydride hardener and postcuring herat-treatments upon electrical properties of epoxy composites, the dielectric properties over a frequency range from 30[Hz] to l[MHz] were investigated in the temperature range of 20-180[.deg. C]. From the dielectric properties, the a peaks related with glass-transition phenomena of epoxy network appeared near 130[.deg. C], the conduction loss in high temperature region above 150[.deg. C] due to thermal dissociation of hardener started off with the low frequency side and the .betha. peak concerned with contribution of movable unreacted terminal epoxy groups and curing agents in the glass states concurred with the high-frequency side below 20[.deg. C]. And an effect of an hydride hardener upon structural changes and of postcuring heat treatments upon structural stability in epoxy composites would be explained through the estimation of the distribution of relaxation times and the activation energy for a .alpha. peak according to the WLF equations.

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