왕겨 실리카와 VSB-5를 이용한 Biginelli 반응 및 크롬산음이온 흡착 = Biginelli Reaction and Chromate Sorption on the Rice-Husk Silica and VSB-5

다국어 초록 (Multilingual Abstract)

InCl3, CoCl2, FeCl3-impregnated microporous catalysts were prepared by impregnating InCl3, CoCl2, FeCl3 dissolved in acetonitrile to various microporous materials. Biginelli reactions under solvent-free conditions were investigated using microwave by the method of one-pot three-component condensation of urea, benzaldehyde and ethyl acetoacetate. Nanopore Silica was prepared by using Korean rice husk. The porous materials or Lewis acid modified porous materials, such as VSB-5, Nanopore Silica, InCl3/VSB-5, InCl3/Nanopore Silica, CoCl2/VSB-5, CoCl2/Nanopore Silica, FeCl3/VSB-5 and FeCl3/Nanopore Silica were used as catalysts. The Biginell reaction results of Nanopore Silica, InCl3/Nanopore Silica, CoCl2/Nanopore Silica and FeCl3/Nanopore Silica catalysts were compared. When Nanopore Silica was used as a catalyst, the yield of the Biginelli product was in the range of 65～68%.
The sorption of chromate anion was carried out using the CTABr modified Silica and VSB-5. Since cetyltrimethylammonium(CTA) ion is too large to enter into the internal surface of Silica, the sorption of CTA ion seems to be only occurred on the external and wide internal surfaces. However since the pore size of VSB-5 is too small, only externed surface of VSB-5 could be occupied by the cationic surfactant. While the unmodified Silica and VSB-5 had no affinity for the chromate anion, the surfactant modified porous materials showed the moderately enhanced sorption of the oxyanion from aqueous solution. The sorption of chromate seems to be due to entropic, Coulombic and hydrophobic effects.

목차 (Table of Contents)

• Ⅰ. 서론 = 1
• Ⅱ. 이론적 고찰 = 3
• 2.1 Green Chemistry와 촉매 화학 = 3
• 2.2 Porous Materials = 5
• 2.2.1 Nanoporus Materials = 5
• 2.2.1.1 VSB-5의 특성 = 5
• 2.2.1.2 왕겨 Silica = 7
• 2.3 Microwave의 특성 = 11
• 2.4 Biginelli Reaction과 DHPM(dihydropyrimidinone)의 합성 = 13
• 2.5 흡착 = 15
• 2.6 계면활성제에 의한 다공성 물질 표면의 변형 = 17
• Ⅲ. 실험 방법 = 19
• 3.1 Nanoporous 물질의 합성 = 19
• 3.1.1 VSB-5의 합성 = 19
• 3.1.2 Nanopore Silica의 제조 = 20
• 3.2 여러 가지 촉매에 Lewis acid의 Impregnation = 20
• 3.3 Microwave를 이용한 DHPM(dihydropyrimidinone)의 무용매 합성 = 21
• 3.4 X-선 회절 분석 = 23
• 3.5 전자 현미경 분석 = 23
• 3.6 CTABr로 변형된 Silica와 VSB-5의 크롬산음이온의 흡착 = 24
• 3.6.1 계면활성제 CTABr에 의한 제올라이트 분자체 표면 변형 = 24
• 3.6.2 Silica와 VSB-5의 크롬산음이온 제거 반응 = 24
• 3.6.3 Silica와 VSB-5의 시간에 따른 크롬산음이온 제거 반응 = 25
• Ⅳ. 결과 및 고찰 = 26
• 4.1 합성한 촉매의 SEM 사진 = 26
• 4.1.1 Silica와 VSB-5의 SEM 사진 = 26
• 4.1.2 Silica와 VSB-5의 원소분석 = 31
• 4.2 촉매의 X-선 회절 분석 결과 = 33
• 4.3 마이크로파를 이용한 촉매의 DHPM의 합성 수득률 = 33
• 4.3.1 DHPM의 합성 = 33
• 4.3.2 합성한 DHPM의 확인 = 35
• 4.4 CTABr로 변형된 Silica와 VSB-5의 크롬산음이온 흡착 = 36
• 4.4.1 CTABr 처리 = 36
• 4.4.2 크롬산음이온의 제거 = 38
• 4.4.2.1 Nanopore Silica = 39
• 4.4.2.2 VSB-5 = 40
• 4.4.3 시간에 따른 크롬산음이온의 흡착 = 42
• 4.4.3.1 Nanopore Silica = 42
• 4.4.3.2 VSB-5 = 42
• Ⅴ. 결론 및 제언 = 44
• Ⅵ. 참고 문헌 = 46