천연 Zeolite를 이용한 1.1-nm Tobermorite의 수열합성

임굉

HWAHAK KONGHAK, Vol.37, No.2, 235-242, April, 1999

Export Citation

천연 Zeolite를 이용한 1.1-nm Tobermorite의 수열합성

Hydrothermally-Synthesized 1.1-nm Tobermorite using Natural Zeolite

임굉

초록

1.1-nm tobermorite의 수열합성에 SiO₂원으로 천연산 제올라이트를 사용하여 소석회와 Ca/(Si+Al)몰비 0.8-1.0으로 150-230 ℃, 8-48시간 동안 포화증기압하에서 수열반응시킨 결과, 반응초기단계에서 tobermorite가 생성되었고 고결정성 1.1-nm tobermorite의 최적합성조건은 0.8몰, 230℃, 48시간이었다. 출발물질 중 Al의 존재로 tobermorite는 0.8몰이 1.0몰보다 결정화가 급속히 이루어지고 있으나 Al을 함유치 않은 경우에는 1.0몰이 0.8몰보다 결정화가 빠르게 진행되었다. 1.1-nm tobermorite는 700 ℃에서 일주일간 가열처리하여도 저면간격이 변화하지 않는 열적거동이 이상형임을 보여주었다. 특히 출발물질 중 Al의 존재가 1.1-nm tobermorite의 결정화와 안정화를 촉진시켜주며 Al이온이 tobermorite 구조 중의 Si이온과 동형치환을 한다.

SiO₂ source on the hydrothermal synthesis of 1.1-nm tobermorite was studied by using natural zeolite. The mixtures of calcium hydroxide and natural zeolite with the Ca(Si+Al) ratio of 0.8-1.0 were reacted hydrothermally under saturated steam pressure, at 150-230 ℃ for 8-48 hour. In result natural zeolite yielded tobermorite at the initial stage of the reaction. The highly crystalline tobermorite was formed at 0.8 mole and 230 ℃ for 48 hour as optimum conditions of hydrothermal synthesis. In the presence of Al in starting, tobermorite was crystallized more rapidly at 0.8 mole than 1.0, but in the absence of Al, crystallization was faster at 1.0 mole than 0.8. Tobermorite showed anomalous thermal behaviour without any significant change in the basal spacing of a heated sample at 700 ℃ for a week. In particular the presence of aluminum in the starting accelerates the crystallization and stabilization of tobermorite, and that the aluminum ion substitutes for the silicon ion in the tobermorite structure.

Keywords:Starting Materials;Natural Zeolite;Hydrothermal Synthesis;1.1-nm Tobermorite;Autoclaved Materials

[References]

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[2] Komarneni S, Roy R, Roy DM, Fyfe CA, Kennedy GJ, Bothner-By AA, Dadok J, Chesnick AS, J. Mater. Sci., 20, 4209 (1985)

[3] El-Hemaly SAS, Mitsuda T, Taylor HFW, Cem. Conc. Res., 7, 429 (1977)

[4] Abe M, Gypsum Lime, 204, 3 (1986)

[5] Suzuki T, Gypsum Lime, 204, 58 (1986)

[6] Komarneni S, Roy DM, Roy R, Cem. Conc. Res., 12, 773 (1982)

[7] Komarneni S, Roy DM, J. Mater. Sci., 20, 2930 (1985)

[8] Komarneni S, Roy DM, U.S. Patent, 4,537,710 (1985)

[9] Komarneni S, Breval E, Miyake M, Roy R, Clays Clay Min., 35, 385 (1987)

[10] Komarneni S, Breval E, Roy DM, Roy R, Cem. Conc. Res., 18, 204 (1988)

[11] Shrivastava OP, Komarneni S, Breval E, Cem. Conc. Res., 21, 83 (1991)

[12] Yasue T, Kojima Y, Inoue H, Arai Y, Gypsum Lime, 228, 18 (1990)

[13] Yasue T, Kojima Y, Inoue H, Arai Y, J. Ceram., 98, 483 (1990)

[14] Yasue T, Shioya Y, Arai Y, J. Ceram., 99, 780 (1991)

[15] Ochiai T, Gypsum Lime, 242, 22 (1993)

[16] Mumpton FA, "Natural Zeolite Occurrence, Properties, Use," Pergamon Press, New York (1978)

[17] Minato H, Ceramics, 10, 17 (1975)

[18] Kim JT, Sohn JR, Choi WH, Kim HW, HWAHAK KONGHAK, 17(5), 331 (1979)

[19] Seo G, Kim K, Moon H, Park H, HWAHAK KONGHAK, 19(5), 349 (1981)

[20] Ha KS, Korean J. Chem. Eng., 4(2), 149 (1987)

[21] Hwang UC, Nam IS, Kim YG, HWAHAK KONGHAK, 28(1), 104 (1990)

[22] Hwang EY, Choi JK, Kim KH, Park DW, Woo HC, Korean J. Chem. Eng., 15(4), 434 (1998)

[23] Negishi T, J. Jap. Assoc. Min. Petr. Econ. Geol., 67, 29 (1972)

[24] Torii K, Hotta M, Onodera Y, Asaka M, Kogyo-Kagaku Zasshi, 74(11), 2012 (1971)

[25] Oinuma K, Hayashi H, J. Toyo Univ. Nat. Sci., 8, 1 (1967)

[26] Harada K, Tomita K, Am. Mineral., 52, 1438 (1967)

[27] Tomita K, Yamashita H, Oba N, J. Jap. Assoc. Min. Petr. Econ. Geol., 63, 16 (1970)

[28] Claringbull GF, Hey MH, Min. Mag., 29, 960 (1952)

[29] McConnell JDC, Min. Mag., 30, 293 (1954)

[30] Kalousek GL, J. Am. Ceram. Soc., 40(3), 74 (1957)

[31] Mitsuda T, Hikichi Y, Cemento Gijutsu Nenpo, 24, 82 (1970)

[32] Mitsuda T, hikichi Y, Murachi M, Cemento Gijutsu Nenpo, 24, 76 (1970)

[33] Mitsuda T, Gypsum Lime, 214, 3 (1988)

[34] Diamond S, White JL, Dolch WL, Am. Mineral, 51, 388 (1966)

[35] Roy DM, Johnson AM, Am. Mineral, 50, 114 (1965)

[36] Mitsuda T, Ceramics, 9, 38 (1974)

[37] Barnes MW, Sheetz BE, Mater. Res. Soc. Symp. Proc., 179, 243 (1991)

[38] Hara N, Inoue N, Yogyo-Kyokai-Shi, 88, 515 (1980)

[39] Mitsuda T, Sasaki K, Ishida H, J. Am. Ceram. Soc., 75(7), 1858 (1992)

[40] Gard JA, Taylor HFW, Min. Mag., 31, 361 (1957)

[41] Mitsuda T, Taylor HFW, Min. Mag., 42, 229 (1978)

[42] Kalousek GL, Prebus AF, J. Am. Ceram. Soc., 41, 124 (1958)

[43] Ikeda Y, Yasuike Y, Takashima Y, J. Ceramics, 99, 423 (1991)