세척탑(Wash Column)을 이용한 인산 결정의 정제

김광주; 심경재; 한명완; Kwang-Joo Kim; Gyeong-Jae Sim; Myung-Wan Han

Journal of the Korean Industrial and Engineering Chemistry, Vol.15, No.1, 75-80, February, 2004

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세척탑(Wash Column)을 이용한 인산 결정의 정제

Purification of Phosphoric Acid Crystals by Wash Column

김광주 ^†, 심경재, 한명완 ¹

한국화학연구원 응용화학연구부 결정화공정연구실, 대전 305-343
¹충남대학교 공과대학 화학공학과, 대전 305-764

Kwang-Joo Kim^†, Gyeong-Jae Sim, and Myung-Wan Han¹

Crystallization Process & Engineering Lab., Korea Research Institute of Chemical Technology, Daejeon 305-343, Korea
¹Department of Chemical Engineering, Chungnam National University, Daejeon 305-764, Korea

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초록

연속식 세척탑(Wash column)에 의하여 인산결정 내에 존재하는 불순물의 분리정제에 관한 연구가 수행되었다. 관의 정제부의 농도 및 온도분포를 측정하여 세척탑의 성능이 조사되었고, 회분식 결정화기의 정제도와 세척탑의 정제성능이 비교되었다. 세척탑의 정제부에서 역혼합 정도는 이전의 관결정화기에서 얻어진 것의 1/5이었다. 세척탑의 정제도는 환류비가 증가함에 따라 증가하였으며 환류비가 20 이상일 때 일정하였다. 불순물의 농도는 현탁밀도가 증가함에 따라 감소하였으며, 분배계수가 변하지 않는 최적의 체류시간은 54 min이었다. 세척탑을 이용하여 결정에 존재하는 불순물은 1/10 ~ 1/20배로 감소되었다.

The impurities included in phosphoric acid crystals were removed by wash column. The performance of purification section in the column was investigated from experimental determinations made of concentration and temperature profiles. The performance of purification section in the wash column were compared with that of the batch crystallization. The product purity increased with increasing reflux ratio. The higher suspension density leads to the lower impurity concentration in crystals. The impurity concentration of products decreases with increasing the residence time. The back-mixing of purification section in the wash column was a fifth times lower than that in the column crystallizer. Impurity content included in the crystals can be reduced to the 1/10 ~ 1/20 of the original sample by wash column.

Keywords:wash column;melt crystallization;suspension density;reflux ratio

[References]

U.S. Patent, 4,665,789 (1987)
J.P. Patent, 026,111 A (2000)
J.P. Patent, 239,008 A (2000)
U.S. Patent, 4,299,804 (1981)
J.P. Patent, 14,692 (1969)
U.S. Patent, 2,540,083 (1951)
Matsuoka M, Takiyama H, Soutome O, Trans. IChemE, 75, 206 (1997)
Kim KJ, Lee JM, Ryu SK, J. Korean Ind. Eng. Chem., 8(3), 389 (1997)
Kim KJ, Lee CH, Koh JC, HWAHAK KONGHAK, 31(2), 160 (1993)
Albertins R, Powers JE, AIChE J., 15, 554 (1969)
Matsuoka M, Kiyomura M, BIWIC, 90, 50 (1990)
Funakoshi K, Uchida H, Takiyama H, Matsuoka M, Chem. Eng. Trans., 1, 1017 (2002)
Jansens PJ, Ph.D. Thesis, TU Delft (1994)

[Related Articles]

[1] U.S. Patent, 4,665,789 (1987)

[2] J.P. Patent, 026,111 A (2000)

[3] J.P. Patent, 239,008 A (2000)

[4] U.S. Patent, 4,299,804 (1981)

[5] J.P. Patent, 14,692 (1969)

[6] U.S. Patent, 2,540,083 (1951)

[7] Matsuoka M, Takiyama H, Soutome O, Trans. IChemE, 75, 206 (1997)

[8] Kim KJ, Lee JM, Ryu SK, J. Korean Ind. Eng. Chem., 8(3), 389 (1997)

[9] Kim KJ, Lee CH, Koh JC, HWAHAK KONGHAK, 31(2), 160 (1993)

[10] Albertins R, Powers JE, AIChE J., 15, 554 (1969)

[11] Matsuoka M, Kiyomura M, BIWIC, 90, 50 (1990)

[12] Funakoshi K, Uchida H, Takiyama H, Matsuoka M, Chem. Eng. Trans., 1, 1017 (2002)

[13] Jansens PJ, Ph.D. Thesis, TU Delft (1994)