• Title/Summary/Keyword: acid-catalyst

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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%.

1,4-Dioxane Decomposition by Catalytic Wet Peroxide Oxidation using Cu Wire Catalysts (Cu wire 촉매를 이용한 촉매습식과산화공정에 의한 1,4-다이옥산의 분해)

  • Lee, Dong-Keun;Kim, Dul Sun
    • Clean Technology
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    • v.22 no.4
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    • pp.281-285
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    • 2016
  • Cu wire catalyst was highly reactive toward catalytic wet peroxide oxidation of the highly refractory 1,4-dioxane. While complete removal of 1,4-dioxane could be achieved with the catalyst, the removed 1,4-dioxane could not totally mineralized into $CO_2$ and $H_2O$. In accordance with the disappearance of 1,4-dioxane, formaldehyde and oxalic acid were formed gradually with reaction time and they went through maxima. At around the time of maximum concentrations of these two intermediates acetaldehyde concentration was increased drastically and showed maximum value. With the disappearance of these three intermediates, formic acid together with ethylene glycol diformate began to increase gradually. The Cu wire catalyst was proved also to be highly stable against deactivation during the reaction.

The reaction of isatin with monocarboxylic acids (Isatin과 일염기산의 반응)

  • 민윤식
    • YAKHAK HOEJI
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    • v.18 no.1
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    • pp.74-76
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    • 1974
  • Oh heating isatin with aromatic monocarboxylic acids having .alpha.-hydrogen atoms such as p-nitrophenylacetic acid, p-methoxyphenyl acetic acid and .alpha.-naphthylacetic acid in the presence of anhydrous sodium acetate functioning as a catalyst, p-nitrobenzylidene-3-oxindole, p-methoxybenzylidene-3-oxindole and ${\alpha}$-naphthobenzylidene-3-oxindole are obtained, respectively. The results of these experiments show that isatin may be used as the carbonyl component in the condensation reaction.

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A Method for Suppression of Active Metal Leaching during the Direct Synthesis of H2O2 by Using Polyelectrolyte Multilayers (고분자 전해질 다층박막을 이용한 과산화수소 직접제조 반응 중 활성금속 용출 억제 방법)

  • Chung, Young-Min
    • Korean Chemical Engineering Research
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    • v.53 no.2
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    • pp.262-268
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    • 2015
  • In this study, two types of catalysts were prepared via conventional metal supporting method and encapsulation of metal nanoparticles in the polyelectrolyte multilayers constructed on support. The resulting catalysts were applied to the direct synthesis of hydrogen peroxide, and the effect of catalyst preparation method on the catalyst life as well as hydrogen peroxide productivity was investigated. The catalytic activity was strongly dependent upon the acid strength of support regardless of the catalyst preparation methods and HBEA (SAR=25) with strong acidity was superior to other supports to promote the reaction. In the case of metal supported catalyst, while hydrogen peroxide productivity was higher than that of polyelectrolyte multilayered counterpart, the reaction performance was sharply decreased during catalyst recycling due to the metal leaching. On the other hand, construction of polyelectrolyte multilayers on support weakened the influence of acid support on the reaction medium and therefore resulted in the decrease of catalytic activity and the increase of hydrogen peroxide decomposition as well. It is noted, however, that the catalytic activity was maintained after 5 recycles, which suggests that the introduction of polyelectrolyte multilayers on the support is very effective to suppress the unfavorable metal leaching phenomenon during a reaction.

Preparation and Thermal Degradation Behavior of WO3-TiO2 Catalyst for Selective Catalytic Reduction of NOx (NOx 제거용 WO3-TiO2 계 SCR 촉매 제조 및 열적열화거동연구)

  • Shin, Byeongkil;Kim, Janghoon;Yoon, Sanghyeon;Lee, Heesoo;Shin, Dongwoo;Min, Whasik
    • Korean Journal of Metals and Materials
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    • v.49 no.8
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    • pp.596-600
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    • 2011
  • Thermal degradation behavior of a $WO_3-TiO_2$ monolithic catalyst was investigated in terms of structural, morphological, and physico-chemical analyses. The catalyst with 4 wt.% $WO_3$ contents were prepared by a wet-impregnation method, and a durability test of the catalysts were performed in a temperature range between $400^{\circ}C$ and $800^{\circ}C$ for 3 h. An increase of thermal stress decreased the specific surface area, which was caused by grain growth and agglomeration of the catalyst particles. The phase transition from anatase to rutile occurred at around $800^{\circ}C$ and a decrease in the Brønsted acid sites was confirmed by structural analysis and physico-chemical analysis. A change in Brønsted acidity can affect to the catalytic efficiency; therefore, the thermal degradation behavior of the $WO_3-TiO_2$ catalyst could be explained by the transition to a stable rutile phase of $TiO_2$ and the decrease of specific surface area in the SCR catalyst.

Removal Characteristics of Dichloroacetic Acid at Different Catalyst Media with Advanced Oxidation Process Using Ozone/Catalyst (담지체를 달리한 오존/촉매 AOP공정에서 디클로로아세트산의 제거 특성)

  • Park, Jin Do;Lee, Hak Sung
    • Applied Chemistry for Engineering
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    • v.20 no.1
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    • pp.87-93
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    • 2009
  • Pd/activated carbon (Pd/AC) and Pd/alumina (Pd/AO) catalysts were prepared by the impregnation of palladium into activated carbon and alumina. The catalytic characteristics according to the kinds of support materials were compared. The decomposition efficiencies of ozone according to kinds of support materials are about the same when these were compared by adding 10 g of catalysts into the water saturated with ozone. The decomposition efficiencies and the oxidation characteristics (TOC, $COD_{Cr}$) of dichloroacetic acid were compared with the ozone only process and the catalytic ozonations using Pd/activated carbon and Pd/alumina catalysts. The decomposition efficiencies of dichloroacetic acid by catalytic ozonations were better than the one by ozone only process, but there was slight difference of the one between Pd/activated carbon and Pd/alumina catalyst. The decomposition efficiency of dichloroacetic acid was increased with increasing ozone dose at a constant concentration of dichloroacetic acid, but the one was little increased with increasing ozone dose at more than 1.0 L/min of ozone dose. It was seemed that the bicarbonate and the chloric ion formed throughout the decomposition of dichloroacetic acid acted as the scavenger of hydroxyl radical.

Preparation of Calcium Sulfate Hemihydrate Using Stainless Refinery Sludge and Waste Sulfuric Acid

  • Eun, Hee-Tai;Ahn, Ji-Whan;Kim, Hwan;Kim, Jang-Su;Sung, Ghee-Woong
    • Proceedings of the IEEK Conference
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    • 2001.10a
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    • pp.432-436
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    • 2001
  • In this study, calcium sulfate(gypsum) powder was obtained using waste sulfuric acid and stainless refinery sludge by- produced from chemical reagent and the iron industry, by the neutralization of waste sulfuric acid. As variables for the experiment the mole ratio of the H$_2$SO$_4$ : Ca(OH)$_2$, the pH, the reaction temperature and time, the amount of catalyst were used. The crystal shape and microstructure of obtained powder were observed by XRD and SEM, and the thermal property was investigated by DTA. As the NaCl is added 0~20wt% as a catalyst to the H$_2$SO$_4$ : Ca(OH)$_2$, system it can be found that the crystal shape goes through the processes as follows : gypsum dihydratlongrightarrowgypsum hemihydrate+gypsum dihydratelongrightarrowgypsum hemihydrate. And gypsum hemihydrate is $\beta$-type as the result of DTA. As waste sulfuric acid and stainless refinery sludge were used, the pH of reacted solution (which was 0.8) was rapidly raised up to 8~9 by the addition of stainless sludge and gypsum dihydrate was produced as a by-product. Therefore, it was found that stainless refinery sludge is sufficiently applicable for the neutralization of waste sulfuric acid.

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Efficient Microwave-assisted Deoxydehydration (DODH) Reactions: Synthesis of Adipic Acid from Galactose (마이크로웨이브를 이용한 효율적인 탈산소탈수(DODH) 반응: 갈락토스 유래 아디픽산의 합성)

  • Shin, Nara;Kwon, Sohyun;Kim, Young Gyu
    • Applied Chemistry for Engineering
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    • v.28 no.2
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    • pp.165-170
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    • 2017
  • An efficient synthetic process for bio-based adipic acid, a monomer for nylon 66, was developed from galactose. Galactaric acid, prepared from a mild oxidation of galactose using a Pt catalyst, was successfully converted to muconate, a key intermediate for adipic acid, by an efficient microwave-assisted DODH (deoxydehydration) reaction. The high efficiency of the microwave-assisted reaction greatly reduced the overall reaction time to 30 min. and resulted in an excellent yield of 97% of muconate. The catalytic hydrogenation of muconate followed by the acidic hydrolysis successfully produced the desired adipic acid in high purity after recrystallization.

Changes in Fatty Acid Composition During Partial Hydrogenation of Soybean Oil (콩기름의 수소첨가 반응시 지방산 조성의 변화)

  • Kwon, Hye-Soon;Yum, Cho-Ae
    • Journal of the Korean Applied Science and Technology
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    • v.10 no.2
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    • pp.57-63
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    • 1993
  • This study investigated the reaction and variation of fatty acid composition of soybean oil when it is partially hydrogenated until its iodine value(IV) shifts from 134 to 110. Experment was conducted under he outlined reactiion conditions of temperatures(170, 190 and $210^{\circ}C$), pressure(1.3, 2.8 and 4.2atm) and nickel(Ni) catalyst concentraons(0.005, 0.01, 0.05, and 0.1%) with a fixed agitation(350rpm). Further investigation was also made to see the effect of added lecithin on hydrogenation. When reaction temperature was gradually raised and catalyst concentration increased, the content of linolenic acid progressively decreased while the increase amount of stearic acid reduced(P<0.05). On he other hand when pressure gradually increased, the contents of stearic acid and linolenic acid increased(P<0.05). Meanwhile when lecithin was added, reaction time increased by two to six times more than when no addition was made.

Selective Synthesis of Butene-1 Through Double-bond Migration of Butene-2 over η-Alumina Catalysts

  • Jeon, Jong-Ki;Kim, Do Heui;Park, Young-Kwon
    • Bulletin of the Korean Chemical Society
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    • v.35 no.9
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    • pp.2669-2672
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    • 2014
  • Double bond migration of butene-2 to butene-1 over ${\eta}$-alumina was investigated. The effects of calcination temperature on catalytic properties were analyzed by applying BET surface area, XRD, $NH_3$-TPD, and FT-IR of adsorbed pyridine techniques. The highest activity of the ${\eta}$-alumina catalyst calcined at $600^{\circ}C$ could be attributed not only to the highest amount of weak and medium strength acid sites, but also to the highest ratio of medium to weak strength Lewis acid sites.