초임계 CO<sub>2</sub>를 이용한 RESS 공정으로부터 안식향산 미세입자의 제조 및 그 특성

김병목; 천재기; 이석희; 이민규; 주창식; Byung Mok Kim; Jae Kee Cheon; Seok Hee Lee; Min Gyu Lee; Chang Sik Ju

HWAHAK KONGHAK, Vol.38, No.3, 387-392, June, 2000

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초임계 CO₂를 이용한 RESS 공정으로부터 안식향산 미세입자의 제조 및 그 특성

Preparation and Characterization of Benzoic Acid Fine Particles by RESS Process with Supercritical CO₂

김병목, 천재기 , 이석희 , 이민규 , 주창식 ^†

부경대학교 화학공학부, 부산 608-739

Byung Mok Kim, Jae Kee Cheon , Seok Hee Lee , Min Gyu Lee , and Chang Sik Ju^†

School of Chemical Engineering, Pukyong National University, Pusan 608-739, Korea

E-mail:

초록

초임계 CO₂를 이용한 RESS 공정으로 안식향산의 미세 입자를 제조하는 실험을 행하여, 공정의 조작변수들이 생성되는 입자의 물성에 미치는 영향을 실험적으로 조사하였다. 팽창관으로 모세관 판을 사용하면, 비교적 넓은 조작조건 범위에서 안식향산 미세 입자를 얻을 수 있었다. 추출온도가 증가할수록, 추출압력이 감소할수록 그리고 초임계 CO₂에 의한 희석 정도가 증가할수록 초임계 용액 중의 안식향산 농도가 감소하여 입자가 크고 입도분포가 넓은 안식향산 입자가 생성되었다. 팽창관 입구온도가 증가할수록 생성되는 입자는 그 크기가 증가하고, 입도분포가 넓어졌다. 수집조에 baffle을 사용한 경우에는 nozzle과 baffle 사이의 거리가 증가할수록 입자 크기가 증가하고 입도분포가 넓어지나, 이 거리가 9cm 이상이 되면 그 영향은 무시되었다.

Experimental researches on the preparation of benzoic acid fine particles by RESS process with supercritical CO₂ have been performed and the effects of operating condition on the physical properties of particles prepared were examined. Benzoic acid fine particles were prepared with orifice disk as an expansion device in wide range of operation conditions. The particle size and particle size distribution increased with the increase in the extraction temperature, the extent of dilution of supercritical benzoic acid solutions with supercritical CO₂, and pre-expansion temperature. However, they decreased with extraction pressure. The distance between orifice nozzle and baffle had no effect on the particle size and particle size distribution if it was longer than 9 cm.

Keywords:Supercritical;RESS Process;Benzoic Acid Fine Particles

[References]

Goldstein AN, "Handbook of Nanophase Materials," Marcel Dekker Inc., New York (1997)
Sugimoto T, Adv. Colloid Interface Sci., 28, 65 (1987)
Ju CS, Lee HG, Jeong YO, Chyn JK, Hwang DK, HWAHAK KONGHAK, 33(4), 437 (1995)
Hannay JB, Hogarth J, Proc. Roy. Soc., London, A29, 324 (1879)
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Peirico NM, Matos HA, de Azevedo EG, da Ponte MN, Proc. 5th Supercri. Fluids, Nice, 313 (1998)
Dobbs JM, Wong JM, Johnston KP, J. Chem. Eng. Data, 31, 303 (1986)
Steckel H, Thies J, Muller BW, Int. J. Pharm., 152, 99 (1997)
Tavana A, Chang J, Randolph AD, AIChE J., 35(4), 645 (1989)
Tavana A, Randolph AD, AIChE J., 35(10), 1625 (1989)
Domingo C, Berends EM, van Rosmalen GM, J. Cryst. Growth, 166, 989 (1996)
Schmitt WJ, Reid RC, J. Chem. Eng. Data, 31, 208 (1986)
Liu GT, Nagahama K, J. Chem. Eng. Jpn., 30(2), 293 (1997)

[Related Articles]

[1] Goldstein AN, "Handbook of Nanophase Materials," Marcel Dekker Inc., New York (1997)

[2] Sugimoto T, Adv. Colloid Interface Sci., 28, 65 (1987)

[3] Ju CS, Lee HG, Jeong YO, Chyn JK, Hwang DK, HWAHAK KONGHAK, 33(4), 437 (1995)

[4] Hannay JB, Hogarth J, Proc. Roy. Soc., London, A29, 324 (1879)

[5] Mohamed RS, Debenedetti PG, Prud'homme RK, AIChE J., 35(2), 325 (1989)

[6] Subramaniam B, Rajewski RA, Snavely K, J. Pharm. Sci., 86(8), 885 (1997)

[7] Chou YH, Tomasko DL, 14th Intern'l Symp. on Supercritical Fluids, May 11-14, Sendai, Jpn (1997)

[8] Kim JH, Paxton TE, Tomasko DL, Biotechnol. Prog., 12(5), 650 (1996)

[9] Peirico NM, Matos HA, de Azevedo EG, da Ponte MN, Proc. 5th Supercri. Fluids, Nice, 313 (1998)

[10] Dobbs JM, Wong JM, Johnston KP, J. Chem. Eng. Data, 31, 303 (1986)

[11] Steckel H, Thies J, Muller BW, Int. J. Pharm., 152, 99 (1997)

[12] Tavana A, Chang J, Randolph AD, AIChE J., 35(4), 645 (1989)

[13] Tavana A, Randolph AD, AIChE J., 35(10), 1625 (1989)

[14] Domingo C, Berends EM, van Rosmalen GM, J. Cryst. Growth, 166, 989 (1996)

[15] Schmitt WJ, Reid RC, J. Chem. Eng. Data, 31, 208 (1986)

[16] Liu GT, Nagahama K, J. Chem. Eng. Jpn., 30(2), 293 (1997)