• Title/Summary/Keyword: Solvent-free 조건

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Direct Preparation of Dichloropropanol from Glycerol over Acetin Catalyst (아세틴 촉매상에서 글리세롤로부터 디클로로프로판올의 직접 제조)

  • Song, Sun-Ho;Park, Dong-Ryul;Woo, Sung-Yul;Song, Won-Seob;Kwon, Myong-Suk;Song, In-Kyu
    • Clean Technology
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    • v.15 no.1
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    • pp.42-46
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    • 2009
  • Solvent-free direct preparation of dichloropropanol (DCP) from glycerol (by-product of bio-diesel production) and hydrochloric acid gas was carried out over acetin catalyst in a gas-liquid batch reactor. For this purpose, acetin mixture and triacetin were used as a homogeneous acetin catalyst. Performance in the acetin-catalyzed reaction was compared to that in the non-catalytic reaction under the same reaction conditions ($110^{\circ}C$, 3 bar, 3 h). Conversion of glycerol in the acetin-catalyzed reactions was ca. 3% higher than that in the non-catalytic reaction, and selectivity for dichloropropanol in the acetin-catalyzed reactions was ca. 50% higher than that in the non-catalytic reaction. It was also revealed that the catalytic performance of triacetin was ca. 2% higher than that of acetic mixture.

Free Radical Scavenging Effect and Extraction Condition of Ethanol Extracts and Fractions of Wild Grape Seed (Vitis coignetiea) (머루종자의 적정 추출조건 및 추출 분획물의 Free Radical 소거능 효과)

  • Kim, Nan-Young;Kim, Young-Kuk;Bae, Ki-Ja;Choi, Jae-Ho;Moon, Jea-Hak;Park, Geun-Hyung;Oh, Deog-Hwan
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.34 no.6
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    • pp.755-758
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    • 2005
  • Wild grape is a traditional medicine plant in north-eastern part of Asia and has been known to have healing properties for various illnesses. This study was to determine the optimum extraction condition and antioxidant activity of ethanol extracts of wild grape (V. coignetiae) seed. Also, organic solvent fractions of hexane, chloroform, ethyl acetate and butanol were obtained from the ethanol extract of wild grape seed at different temperatures. Total ethanol extraction yield of wild grape seed ranged from $4\%\;to\;12\%$ depending on the ethanol concentration, extraction temperature and time condition. The highest extraction yield of $11.9\%$ was obtained at $90\%$ ethanol condition for 12 hour at $70^{\circ}C$. However, the strongest free radical scavenging effect $(RC_{50})$ with $20.93\mu g/mL$ was observed in $70\%$ ethanol extract of wild grape seed extracted for 6 hour at $70^{\circ}C,\;while\;RC_{50}\;with\;40.42$\mu g/mL$ was observed in $90\%$ ethanol extract for 12 hour at $70^{\circ}C$. Antioxidant activity of ethanol extracts of wild grape seed increased as total phenol contents increased. Among each fraction obtained from organic solvents, ethyl acetate fraction was found to have the strongest $RC_{50}\;(8.6\mu g/mL)$ and 636.77 mg GAE/g phenol contents .

Free Radical Scavenging Effect and Extraction Condition of Ethanol Extracts of Epimedium Koreanum Nakai Containing Different Icariin Quantity (Icariin 함량에 따른 삼지구엽초 추출물의 추출조건 및 항산화 효과)

  • Kim, Seo-Jin;Oh, Deog-Hwan
    • Journal of Food Hygiene and Safety
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    • v.22 no.4
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    • pp.359-364
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    • 2007
  • This study was conducted to determine the optimum condition of extraction and antioxidant activity of ethanol extracts of Epimedium koreanum Nakai based on the icariin quantity. Also, further organic solvent fractions of hexane, chloroform, ethyl acetate and butanol were obtained from the ethanol extract of Epimedium koreanum Nakai at different temperatures. Total ethanol extraction yield of wild grape seed ranged from 11.8% to 39.3% depending on the concentration of icariin as well as different ethanol concentration, extraction temperature and time condition. Among different extraction temperatures and time, the highest extraction yield of 39.3% was obtained at 70% ethanol for 3 hour at $50^{\circ}C$ in the sample containing the 0.596% icariin (KE9412). In the meantime, the strongest free radical scavenging effect $(RC_{50})$ with $18.9{\mu}g/mL$ in the KE9412 sample was observed in 70% ethanol extract of Epimedium koreanum Nakai extracted for 7 hour at $70^{\circ}C$, while $RC_{50}$ with $35.2{\mu}g/mL$ was observed in the KE9405 (0.20% icariin content) sample at same condition. Also, antioxidant activity of ethanol extracts of Epimedium koreanum Nakai increased as icariin concentration increased. Among each fraction obtained from organic solvents, butanol fraction was found to have the strongest $RC_{50}\;(39.2{\mu}g/mL)$ and followed by ethylacetate $(49.0{\mu}g/mL)$, water $(118.8{\mu}g/mL)$, ethylacetate $(119.8{\mu}g/mL)$, and chloroform fraction $(138.5{\mu}g/mL)$ respectively.

Removal of Alkali Metal Ion using Inorganic Ion Exchanger (무기이온교환제를 이용한 알카리 금속이온 제거)

  • Ha, Ji-Won;Yi, Kwang Bok;Lee, Si Hyun;Rhee, Young-Woo;Kim, Jong-Nam
    • Korean Chemical Engineering Research
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    • v.46 no.2
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    • pp.423-429
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    • 2008
  • Currently, Ash-free clean coal producing process by solvent extraction is under development. The produced ash-free clean coal can be directly combusted in a gas turbine which results in substantial improvement of power generation efficiency. However, the clean coal produced by the solvent extraction still contain trace amount of alkali metal which may cause corrosion on turbine blades during the direct combustion. In present work ${\alpha},{\beta}$-metal (Zr and Ti) phosphates and H-Y zeolite were synthesized and their ion exchange characterizations were investigated for the application on alkali metal removal for clean coal production. $Na^+$ ion removal capacities of the metal phosphates and H-Y zeolite were measured and compared in both aqueous solution (100 ppmw, $Na^+$) and coal dissolved N-methyl-2-pyrrolidone (NMP, 12 ppmw $Na^+$) at elevated temperature. In aqueous solution, the ${\beta}$ form metal phosphates showed very high ion exchange capacities compared to ${\alpha}$ form. ${\beta}$ form metal phosphates also showed higher $Na^+$ removal capacities than H-Y zeolite. In ion exchange medium of NMP, all the ${\alpha}$ form metal phosphates showed over 90% of $Na^+$ ion removal efficiency in the temperature range of 200 to 400 while that of H-Y zeolite decreased as a half when the temperature was over 350. In addition, the regenerated metal phosphates by acid treatment showed no sign of degradation in $Na^+$ removal efficiency. Among the metal phosphates used, $Zr_{0.75}Ti_{0.25}(HPO_4)_2$ showed the best performance in $Na^+$ removal and is expected to be the most suitable inorganic ion exchanger for the alkali metal removal process.

Screening of Effective Extraction Conditions for Increasing Antioxidant Activities of Licorice Extracts from Various Countries of Origin (원산지별 감초추출물의 항산화활성 증가를 위한 효율적인 추출조건 탐색)

  • Ha, Ji Hoon;Lee, Hye Mi;Kwon, Soon Sik;Kim, Hae Soo;Kim, Moon Jin;Jeon, So Ha;Jeong, Yoo Min;Hwang, Jun Pil;Park, Jong-Ho;Choi, Yung-Key;Park, Jino;Park, Soo Nam;Park, Dong-Sik
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.39 no.4
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    • pp.259-269
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    • 2013
  • In this work, licorice extracts were prepared using various extraction conditions such as extraction solvent, temperature, and time from Glycyrrhiza uralensis (G. uralensis) produced in Korea and China and Glycyrrhiza glabra (G. glabra) in Uzbekistan. The optimum extraction condition was selected from the extraction yields and antioxidative activities of extracts. Korea licorice extracts showed the highest free radical (1,1-diphenyl-2-picrylhydrazyl, DPPH) scavenging activity (46.05%) under the extraction condition of 85% ethanol at $60^{\circ}C$ for 6 hours. The prominent ROS (reactive oxygen species) scavenging activity using luminol-dependent chemiluminescence assay and the cellular protective effect against $^1O_2$ induced cellular membrane damage were also shown from the extracts obtained from the same condition. Especially, Korea G. uralensis extracts exhibited the higher prominent protective effect (${\tau}_{50}$ = 116.4 min) than (+)-(+)-${\alpha}$-tocopherol (${\tau}_{50}$ = 28.5 min) and the extraction yield of Korea licorice extract was 18.75%, which is 1.2 times and 2.5 times higher than that of Uzbekistan and China, respectively. These results indicate that the extraction condition of 85% ethanol at $60^{\circ}C$ for 6 hours is optimal to prepare licorice extracts, which can be applicable as anti-oxidative cosmetic materials.

A Study on the Extraction of Monasil PCA using Liquid CO2 (액체 이산화탄소 이용한 Monasil PCA 추출에 대한 연구)

  • Cho, Dong Woo;Oh, Kyoung Shil;Bae, Won;Kim, Hwayong;Lee, Kab-Soo
    • Korean Chemical Engineering Research
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    • v.50 no.4
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    • pp.684-689
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    • 2012
  • Poly(acrylic acid) (PAA) microspheres is one of the widely-used polymeric materials for the bio-field application and the electric materials. For the synthesis of PAA microspheres, the polymerization technique using surfactants is applied. After the synthesis, the purification and separation processes are required for the removal of surfactant. When general organic solvents were used, many problems, such as huge amount of waste solvent, additional separation processes, and the possibility of residual media, were occurred. Thus, High-pressure Soxhlet extraction using liquid $CO_2$ was developed to solve these problems. In this study, High-pressure Soxhlet extraction of the synthesized PAA microspheres using liquid $CO_2$ was conducted for the removal of Monasil PCA which is used for the dispersion polymerization of acrylic acid in compressed liquid Dimethyl ether (DME). The morphology of the extracted PAA particles was checked by field emission scanning electron microscopy (FE-SEM) and the residual concentration of Monasil PCA was analyzed by inductively coupled plasma - Optical Emission Spectrometer (ICP-OES). For studying the effect of the solvent effect, Soxhlet extraction was conducted using n-hexane, liquid DME, and liquid $CO_2$. In case of n-hexane, some extracted PAA microspheres were produced. However, deformation was also occurred due to the high thermal energy of n-hexane vapor. Liquid DME could not remove Monasil PCA. When using liquid $CO_2$, the extracted PAA microspheres which were free for the residual solvent were produced without deformation. For finding the optimum operating condition, high-pressure Soxhlet extraction was conducted for 8 hours with changing the temperature of reboiler and condenser. When the extractor temperature is $19.6{\pm}0.2^{\circ}C$ and the pressure is $51.5{\pm}0.5$ bar, the best removal efficiency was obtained.

Comparison of Chemical Characteristics of Korean Mountain Ginseng Different Parts According to Extract Conditions (장뇌삼의 부위별 추출조건에 따른 이화학적특성 비교)

  • Kim, Jun-Han;Lee, Gee-Dong;Lee, In-Seon;Kim, Jong-Kuk
    • Food Science and Preservation
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    • v.13 no.6
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    • pp.720-725
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    • 2006
  • This study was conducted to investigate extracting solution effect on the chemical compositions in different parts of Korean mountain Ginseng. Water, 80% EtOH and 80% MeOH are used as extraction solutions, and extracting conditions were 2 hr at $85^{\circ}C$ in water bath. The Brix(%) of the extract were ranged from $0.42{\sim}22.58%$, 80% EtOH extract for leaf is the highest level as 22.58%. The pH ranges of the extracts were $4.43{\sim}7.41$ and brown color of the extract was the highest with 1.803 in 80% EtOH extract for leaf, respectively. In case of hunter's color value of the extract, L value is the highest with 24.35 in 80% EtOH extract of seed, a and b value were the highest with 0.41 in 100% water extract of leaf and 3.69 in 80% MeOH extract of stem. Sucrose is the major free sugar of the extinct it highest content with 3673 mg% in 80% MeOH extract of mot and fructose is the highest with 1897 mg% in 80% MeOH extract of leaf, Major organic acids are identified as malic, tartaric and citric acid, and total organic acid content is the highest with 5,254 mg% in 80% MeOH extract of leaf and 1,527 mg% in 80% EtOH extract of leaf, The extracted major minerals ate P and K, P content highest with 15,563 ppm in 100% water extract of stem, K is 4,952 ppm in 80% MeOH extract of leaf, and Ca is the highest with 3,052 ppm in 1011% water extract of leaf. These results suggest that extracting solvent (80% MeOH) is concerned with the extract preparation of Korea Mountain Ginseng.

Enhancement of cyanoacrylate-developed marks using p-dimethylaminobenzaldehyde (DMAB) on semi-porous surfaces and analysis of the influence factors on fluorescence intensity (반다공성 재질에 유류된 지문의 CA 훈증 후 p-dimethylaminobenzealdehyde(DMAB) 형광시약 적용 시 표면적과 주변 온도, 기압이 형광착색에 미치는 효과에 관한 연구)

  • Yu, Je-Sul;Kim, Ju-Hah
    • Analytical Science and Technology
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    • v.27 no.4
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    • pp.187-195
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    • 2014
  • It is very important to minimize the damage of latent fingerprints at enhancing the contrast. This study proves the enhancement effects of cyanoacrylate-fumed latent fingerprints using p-dimethylaminobenzealdehyde (DMAB) on semi-porous surfaces and the influence factors. The latent fingerprints in experiment were developed for cyanoacrylate treatment in a vacuum chamber and used after drying at room temperature for 24 hours. For fluorescence staining, the cyanoacrylate-developed marks using DMAB were sublimated during 48 hours under the different conditions of surface area, temperature, atmospheric pressure. First experiment showed how surface area effects on the sublimation rate and fluorescence intensity by DMAB of particle size and container size. In addition, the fluorescence staining using DMAB with solvent-free contact method had the greatest fluorescence intensity after 36 hours and a low fluorescence intensity over a certain size of surface area. Second experiment showed that the evaporation of DMAB solid crystals got a satisfying result in a temperature of $20^{\circ}C$ and reduced time to get the greatest fluorescence intensity. It took a long time to get a optimum level of fluorescence intensity at $30^{\circ}C$ or more and it was less effective in fluorescence intensity. Third experiment on the pressure indicated that the fluorescence intensity of vacuum was weaker than nonvacuum but it was inapplicable to very high variations in pressure.

A Study on the Effect of Surfactants in Acrylic Emulsion Polymerization (아크릴 에멀젼 중합에서의 계면활성제 영향에 관한 연구)

  • Song, Ju-Ho;Park, Sang-Joon;Park, Sang-Kwon;Lee, Myung-Cheon;Lim, Jong-Choo
    • Applied Chemistry for Engineering
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    • v.10 no.4
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    • pp.523-530
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    • 1999
  • Acrylic pressure-sensitive adhesive has been made utilizing organic solvents, but nowadays it is made by solvent-free system due to environmental problems. In this study, emulsion polymerization were carried out at $40^{\circ}C$ with methacrylic acid(MAA), n-butyl acrylate(n-BA) and 2-ethylhexyl acrylate(2-EHA) as monomers in the presence of anionic(sodium dodecyl sulfate, SDS) and nonionic(ethylene oxide types) surfactant mixtures. The overall conversion of the polymerization reaction in a mixed surfactant system was found to be higher than that in a single surfactant system. Emulsion stability in mixed or anionic surfactant systems was found to be over 12 week, which was better than that in nonionic surfactant system. Emulsion particle size decreased as surfactant content increased. The Tg and molecular weight of emulsion polymer were inependent of the type, the amount and the mixing ratio of surfactant. Based on the results of stability and peel strength, the optimum nonionic surfactant ratio in total 4 g of surfactant mixture systems is found to be 40~60% by weight where the nonionic surfactant has 50 ethylene oxide groups and 16~18 carbon atoms in hydrophobic alkyl chain.

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The Physical and Thermal Properties Analysis of the VOC Free Composites Comprised of Epoxy Resin, and Dicyandiamide (VOC Free Epoxy Resin/Dicyandiamide 경화물의 배합비 변화에 따른 물리적 특성 및 열적특성 분석)

  • Kim, Daeyeon;Kim, Soonchoen;Park, Young IL;Kim, Young Chul;Lim, Choong-Sun
    • Clean Technology
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    • v.21 no.1
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    • pp.76-82
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    • 2015
  • Volatile organic compounds (VOC) free adhesives have been interested by many scientists and engineers due to environmental regulations and the safety of industrial workers. In this work, a series of composites composed with bisphenol A epoxy resin used as solvent, dicyandiamide, and promoter were prepared to investigate the most appropriate molar ratio for steel-steel adhesion. The cured test specimen of each composite were measured with universal testing machine (UTM) to figure out mechanical properties such as tensile strength, Young’s modulus, and elongation. Furthermore, the lap shear strength of the specimen was tested with UTM while impact resistance was measured with Izod impact tester. The composite whose molar ratio of epoxy resin to curing agent is 1 : 0.9 (sample 3), showed better tensile strength, coefficient of elastic modulus, elongation, and impact strength than other composites did. The highest tanδ from dynamic mechanical analysis (DMA) was observed from sample 2 (epoxy resin: dicy = 1 : 0.7) while sample 3 showed slightly lower tanδ than that of 2. The morphology of the fracture surface of the cured composites from SEM showed that the number of subtle lines on the surface caused by impact increase as the contents of amine curing agent accrete. Furthermore, the viscosity change of sample 5 (epoxy resin: dicy = 1 : 1.3) was observed to confirm its storage stability.