• Title/Summary/Keyword: 1단계 합성

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Synthesis of Sol using acid Colloidal Silica and TMOS/MTMS (산성 Colloidal Silica와 TMOS/MTMS를 이용한 졸합성)

  • Kang, Dong-Pil;Park, Hoy-Yul;Ahn, Myeong-Sang;Myung, In-Hye;Lee, Tae-Hui;Lee, Tae-Ju
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2004.05b
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    • pp.154-157
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    • 2004
  • 산성 colloidal silica(CS) 1034A, HSA와 TMOS, MTMS 실란 간의 졸겔반응조건이 코팅도막의 특성에 미치는 영향을 조사하기 위하여 1034A CS계에 대해서는 1단계로 실란들을 첨가하고 동일한 MTMS에 대해 CS/TMOS의 함량비, 반응시간을 달리하여 졸을 합성하였다. HSA계에 대해서는 2단계로 분리하여 TMOS, MTMS 실란을 첨가하는데 실란 첨가순서와 실란 함량비, 반응시간을 달리하여 졸을 합성하였다. 합성된 졸은 slide glass에 함침 코팅한 후 $300^{\circ}C$에서 경화시킨 도막의 특성들을 조사하였다. 1034A CS계는 CS/TMOS의 비가 70/30일 때 50/50인 경우보다 반응시간에 따라서 표면조도가 우수하여 접촉각에 영향을 덜 주므로 효과적인 균일 반응상으로 진행되었다. HSA CS계는 1단계로 MTMS를 먼저 첨가하고 MTMS/TMOS 비를 25/75로 첨가하면 반응시간에 따라서 표면조도 거칠기에 크게 영향 받지 않고 접촉각을 안정화시킬 수 있다.

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The Formation Mechanism Synthesizing of $SrTiO_3$Fine Powders by Ultrasonic Spray Pyrolysis (초음파 분무 열분해법에 의한 $SrTiO_3$ 미분말 합성시 그 형성 과정에 관하여)

  • 허화범;이동주;신건철
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.2 no.2
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    • pp.11-19
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    • 1992
  • $SrTiO_3$powders were synthesized from the chloride and the nitrate aqueous solution by spray pyrolysis method using ultrasonic vibrator. The concentration of mother solution was prepared 0.05M and O.lM. The carrier gas flow rate was 0.5cm/sec and 1.5cm/sec, respectively. The formation processing was investigated in the 0.05M and 0.05cm/sec. The $SrTiO_3$powders could not be synthesized from chloride aqueous solution. The prepared powders from nitrate aqueous solution was SrTi03 with cubic structure and nearly sphere particle for all samples. Mean particle size was increased from $0.49{\mu}m$ to $0.67{\mu}m$ by changing the carrier gas flow rate from O.5cm/sec to 1.5cm/sec. Also, mean particle size increased from $0.49{\mu}m$to $0.55{\mu}m$by changing the concentration of mother solution from O.05M to O.1M. Atomizing droplet size was $14.3{\mu}m$. The shape of particles was very porous by evaporation of solvent at the initial step. But through the each step upwards, shape of particles was formed themselves into a nearly roundish.

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Development of the Efficient Synthetic Route for Itraconazole Antifungal Agent (이트라코나졸 항진균제의 효과적인 합성법 개발)

  • Baek, Du-Jong
    • Applied Chemistry for Engineering
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    • v.17 no.6
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    • pp.633-637
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    • 2006
  • In this study, the efficient large-scale synthetic route for itraconazole, triazole antifungal agent, was developed. The original synthetic route for medicinal chemistry reported by Janssen Pharmaceutica was linear (14 linear steps) starting from 2,4-dichloroacetophenone with the total yield of 1.4%, and potential hazardous materials such as methanesulfonyl chloride ($CH_{3}SO_{2}Cl$), hydrogen gas, and sodium hydride (NaH) were used. Furthermore, the expensive 1-acetyl-4-(4-hydroxyphenyl)piperazine and palladium were used in this medicinal chemistry route, thus the manufacturing cost would be practically high. In order to improve the commercial route, we developed the process of 12 step convergent synthesis combining two intermediates which are roughly halves of itraconazole with the total yield of 12.0%, and hazardous materials and expensive reagents were excluded in this process, thus the manufacturing cost could be cut down to a great extent.

Preparation Nanosized TPA-Silicalite-1 with Different Silica Sources and Promoters (다양한 실리카 원과 결정화 촉진제를 이용한 나노크기의 TPA-Silicalite-1 제조)

  • Jung, Sang-Jin
    • Applied Chemistry for Engineering
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    • v.25 no.3
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    • pp.286-291
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    • 2014
  • In this study, nanosized TPA-silicalite-1 was synthesized with a suitable molar composition of TPAOH: $SiO_2$: $H_2O$ for the development of zeolite ceramic membranes to utilize as gas separation. As silica sources, TEOS, LUDOX AS-40 and CAB-O-SIL were used with the starting material of TPAOH. $NaH_2PO_4$, and a variety of acids and bases were used as promoters after TPAOH, $SiO_2$, $H_2O$ gel synthesis. To decrease synthesis time, a two step temperature change method was applied to the synthesis of TPA-silicalite-1 at a low temperature. TPA-silicalite-1 synthesized was analyzed with XRD, SEM, BET and TGA. As a result, TPA-silicalite-1 powders with a particle size of 100 nm and a specific surface area of $416m^2/g$ were obtained as optimum synthesis conditions when the two stage temperature change method was used with $NaH_2PO_4$ as promoter.

Process Development of 4,4'-Bis(2-benzoxazolyl)stilbene from Recyclable Source MFB (재사용이 가능한 MFB로부터 4,4'-Bis(2-benzoxazolyl)stilbene의 합성 공정 개발)

  • Ryu, Young;Kim, Jong Cheon;Ham, Mi Jeong;Kim, Seok Chan
    • Applied Chemistry for Engineering
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    • v.27 no.2
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    • pp.195-198
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    • 2016
  • A total four-step synthetic process of high quality optical brightening agent 4,4'-bis(2-benzoxazolyl)stilbene (BBS) from methyl 4-formylbenzoate (MFB) was developed with 73% total yield. MFB is one of the main by-products in dimethyl terephthalate (DMT) production process. Our process involves the formation of 4,4'-stilbenedicarboxylate (2) obtained from the reaction of an aldehyde in MFB with ethyl 4-((diethoxyphosphoryl)methyl)benzoate (1) and the subsequent transformation to 4,4'-stilbenedicarbonyl chloride (3). In order to prepare benzoxazole ring in BBS, various solvents and catalysts were studied. The best solvent and catalyst were found to be 1,2,4-trichlorobenzene and boric acid, respectively suitable for mass production of BBS.

Synthesis and Application of Melamine-Type Superplasticizer at the Different Synthetic Conditions (멜라민계 고유동화제의 다양한 조건에서의 합성 및 응용)

  • Yoon Sung-Won;Shin Kyoung-Ho;Rho Jae-Seong
    • Journal of the Korea Concrete Institute
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    • v.17 no.5 s.89
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    • pp.811-818
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    • 2005
  • It is well known that the fluidity and the fluidity loss of fresh concrete are affected by the kind of organic admixtures. Organic admixture can improve the properties of concrete. Sulfonated Naphthalene-Formaldehyde(SNF) Superplasticizer is used representatively, but has a problem in fluidity loss. In this study, we synthesized the Sulfonated Melamine-Formaldehyde(SMF) superplasticizer at the various synthetic conditions and compared the physical properties with SMF superplasticizer. SW superplasticizer is synthesized with four synthetic steps. Step 1 is hydroxymethylation, Step. 2 is Sulfonation, Step. 3 is Polymerization and Step. 4 is Stabilization. Synthesis of SMF superplasticizer depends on pH, temperature and reaction time. In this reaction, we changed the mole ratio of melamine to formaldehyde at 1:3, 1:4, and the amount of acid catalyst at Step. 3. After application of SMF superplasticizer and its mixture with SNF superplasticizer to cement pastes and mortars, we measured the physical properties of them at the different dosages(0.5, 1.0, 1.5 wt%) to cement. All samples including superplasticizer showed higher compressive strengths and slump, smaller pore size and porosity than CEM

Synthesis and Lubricating Properties of Dimer Acid Derivatives Based on Used Vegetable Oil (폐식물유 기반 다이머산 유도체의 합성 및 경유의 윤활성능)

  • Lee, Sang Jun;Kim, Young-Wun;Yoo, Seung-Hyun;Kim, Nam-Kyun;Shin, Ji Hoon;Yoon, Byung-Tae
    • Applied Chemistry for Engineering
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    • v.24 no.5
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    • pp.530-536
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    • 2013
  • Vegetable oil-based dimer acid derivatives were prepared through a two-step procedure and their lubricating properties for diesel fuel were evaluated using high frequency reciprocating ring (HFRR) method to investigate wear scar diameter (WSD). Diels-Alder reaction at an elevated temperature transformed fatty acid to dimer acid, subsequently converted into dimer acid derivatives by esterification with methanol. It should be noted that the derivatives were dissolved well in diesel oil up to 1 wt%. After adding 120 ppm of the derivatives to pure diesel, the WSD significantly decreased to $300{\sim}05{\mu}m$, compared to $552{\mu}m$ of WSD in pure diesel. Dimer acid derivatives having carboxylic acid show superb in lubricating property which does not depend on the alkyl group in the derivatives.

Studies on the Synthesis of Etodolac Derivatives as Potential Anti-inflammatory Agents (항염증제인 Etodolac 유도체의 합성에 관한 연구)

  • Cho, Hoon;Chung, Yong Seog;Jang, Hang Dong;Ryu, Seong Ryual
    • Applied Chemistry for Engineering
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    • v.10 no.1
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    • pp.135-137
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    • 1999
  • For the synthesis of new anti-inflammatory agents as indol derivatives, we have synthesized ${\alpha}$-benzoyl-1-ethyl-1,3,4,9-tetrahydro-8-ethyl-9-(N-benzoyl)pyrano[3,4-b]indole-1-acetic acid methyl ester. It was a new method for ${\alpha}$-substituted etodolac carboxylic acid. The synthetic process was composed of four steps, and 7-ethylindole and oxalyl chloride were used as starting materials. The third step, cyclization was carried out by addition of borontrifluoride diethyl etherate in 66% yield. The step of reduction and cyclization were simplified successfully. The final product, ${\alpha}$-benzoyl-1-ethyl-1,3,4,9-tetrahydro-8-ethyl-9-(N-benzoyl)pyrano[3,4-b]indole-1-acetic acid methyl ester was obtained in 66% yield by the reaction of methyl 1,8-dimethyl-1,3,4,9-tetrahydropyrano[3,4-b]indole-1-acetate (etodollic acid methyl ester) and benzoyl chloride.

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Preparation of nanosized TPA-silicalite-1 with various crystallization promoters (다양한 결정화 촉진제를 이용한 나노크기의 TPA-silicalite-1 제조)

  • 김호동;정상진;김명훈;김영희;김수룡;이영무
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2003.03a
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    • pp.48-48
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    • 2003
  • 미세기공(microporous)을 가진 제올라이트는 다양한 유기질 분리의 촉매제 및 광학, 화학 센서, 기체 분리 등의 고기능 소재로서 크게 주목받고 있으며, 비표면적의 증가, 새로운 기능의 발현 둥으로 최근 들어 나노크기를 갖는 제올라이트 합성에 관한 연구가 활발히 진행되고 있다. 본 연구에서는 기체 분리에 응용하기 위한 제올라이트 분리막 개발에 앞서 분리막 제조에 유리할 것으로 판단되어지는 적합한 크기와 형상을 갖춘 나노크기의 제올라이트를 합성하였으며 그 특성을 분석하였다. 출발물질로서 실리카 원으로는 TEOS, LUDOX AS-40, Cab-O-SIL 등을 사용하였으며, 템프레이트(TPAOH)와 함께 특정조성의 TPAOH/SiO$_2$,/$H_2O$ 겔을 만들었다. 합성시간을 단축할 수 있는 방법의 연구로서 저온하의 2단계 온도 변화법을 적용하였으며, 결정성장속도의 향상을 목적으로 NaH$_2$PO$_4$, H$_2$SO$_4$, NH$_4$OH 등의 결정화 촉진제로 사용하여 수열합성법으로 Silicalite-1를 합성하였다.

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