페촉매로부터의 니켈 추출 및 이를 이용한 유지경화용 수소화 촉매의 제조

김태진; 차익수; 이희철; 안화승

Journal of the Korean Industrial and Engineering Chemistry, Vol.5, No.6, 925-934, December, 1994

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페촉매로부터의 니켈 추출 및 이를 이용한 유지경화용 수소화 촉매의 제조

A Study on the Preparation of Oil Hydrogenation Catalysts Using Nickel Extracted from the Spent Catalysts

김태진, 차익수, 이희철, 안화승

초록

유지 수소화용 폐촉매로부터 니켈을 추출 분리하여 수소화 촉매로 재생하였다. 입수한 폐촉매로부터는 약 21.8% Ni, 0.7% Mg 및 소량의 Al, Fe와 Zn이 검출되었다. 폐촉매로부터 무기산을 이용하여 니켈 성분을 추출할 때는 염산>질산>황산의 순서로 추출률이 감소하였으며, 질산으로 추출할 경우 3N의 농도로 3시간 정도 추출하는 것이 적합하였다. 용해도차를 이용한 금속 불순물의 침전 분리 제거에 있어서 니켈 회수율을 최대화 하려면 pH 6.5∼9.0의 조건이 좋으나 부분적으로 불순물 공침이 생긴다. 니켈의 회수율이 약간 떨어지더라도 pH 7.0∼9.0에서 니켈을 분리하여 금속 불순물의 대부분을 제거하면 촉매 제조에 효과적이었다. 폐촉매로부터 추출 처리하여 얻은 nickel을 규조토에 담지시켜 습식환원법으로 제조한 촉매는 촉매 내 금속 불순물의 제거율이 높은 경우, 시약으로 실험실에서 제조한 촉매와 대동소이한 대두유 경화반응 특성을 나타내었다. 이 때 담체의 비표면적은 반응에 영향을 미치지 않았다.

Nickel recovered from the spent oil-hydrogenation catalysts was used in hydrogenation catalyst preparation. The spent catalyst contains approximately 21.8% Ni, 0.7% Mg, and small quantities of Al, Fe, and Zn. Nickel recovery was obtained by inorganic acid digestion in the order of HCl> HNO₃> H₂SO₄. For HNO₃, 3hour extraction with 3N solution was satisfactory. In the PH range of 6.5 ∼9.0, Ni recovery was higher, but metallic impurities were found to be coprecipitated. The PH in the range of 7.0∼9.0 seems to be the optimum condition for separation to obtain acceptable Ni precipitates without the decrease of purity. The catalysts prepared with reclaimed nickel by wet reduction methods showed catalytic activities close to those prepared using reagent nickel in the oil hydrogenation reaction. The surface areas of the support do not seem to affect the catalytic activity.

[References]

Allen RR, "World Conference on Soya Processing and Utilization," JAOCS, 166-169 (1981)
Allen RR, Formo MW, Krishnamurthy RG, McDermott GM, Norris FA, Sonntag NOV, "Bailey's Industrial Oil and Fat Products," 2, 62-65 4th Ed. John Wiley and Sons (1982)
Coenen JWE, Ind. Eng. Chem. Fundam., 25, 43 (1986)
Coenen JWE, JAOCS, 53, 382 (1976)
Patterson HBW, "Hydrogenation of Fats and Oils," 126, Applied Science Publishers, London (1990)
Grau RJ, Cassano AE, Baltanas MA, Catal. Rev.-Sci. Eng., 30, 1 (1988)
Kim HW, Kim JS, shim JH, Park SJ, ahn TH, Park KM, Choi CU, Korean J. Food Sci. Technol., 22, 681 (1990)
Satterfield CN, "Heterogeneous Catalysis in Practice," 80-83, McGraw-Hill Book Company, New York (1980)
Drozdowski B, Zajac M, JAOCS, 149 (1980)
Shukla A, Maheshwari PN, Vasishtha AK, JAOCS, 65, 1816 (1988)
Massoumi A, Kajbaf MA, JAOCS, 56, 565 (1979)
Orficial & Tentative Method of the American Oil Chemist's Society, ed. W.E. Links, 1, AOCS, Champaign, IL (1976)
Jeffery GH, Bassett J, Mendham J, Denny RC, "Vogel's Testbook of Quantitative Inorganic Analysis," 5th Edition, 384-393, Longman Scientific & Technical Co. (1989)
Freedman B, Kwolek WR, Pryde EH, JAOCS, 63, 13 (1986)
Watanabe S, JAOCS, 50, 360 (1973)
Mork PC, JAOCS, 53, 506 (1973)
Bard AJ, "Chemical Equilibrium," 40-60, Harper & Row Publishers, New York, Evanston and London (1966)

[Referenced By]

[1] Allen RR, "World Conference on Soya Processing and Utilization," JAOCS, 166-169 (1981)

[2] Allen RR, Formo MW, Krishnamurthy RG, McDermott GM, Norris FA, Sonntag NOV, "Bailey's Industrial Oil and Fat Products," 2, 62-65 4th Ed. John Wiley and Sons (1982)

[3] Coenen JWE, Ind. Eng. Chem. Fundam., 25, 43 (1986)

[4] Coenen JWE, JAOCS, 53, 382 (1976)

[5] Patterson HBW, "Hydrogenation of Fats and Oils," 126, Applied Science Publishers, London (1990)

[6] Grau RJ, Cassano AE, Baltanas MA, Catal. Rev.-Sci. Eng., 30, 1 (1988)

[7] Kim HW, Kim JS, shim JH, Park SJ, ahn TH, Park KM, Choi CU, Korean J. Food Sci. Technol., 22, 681 (1990)

[8] Satterfield CN, "Heterogeneous Catalysis in Practice," 80-83, McGraw-Hill Book Company, New York (1980)

[9] Drozdowski B, Zajac M, JAOCS, 149 (1980)

[10] Shukla A, Maheshwari PN, Vasishtha AK, JAOCS, 65, 1816 (1988)

[11] Massoumi A, Kajbaf MA, JAOCS, 56, 565 (1979)

[12] Orficial & Tentative Method of the American Oil Chemist's Society, ed. W.E. Links, 1, AOCS, Champaign, IL (1976)

[13] Jeffery GH, Bassett J, Mendham J, Denny RC, "Vogel's Testbook of Quantitative Inorganic Analysis," 5th Edition, 384-393, Longman Scientific & Technical Co. (1989)

[14] Freedman B, Kwolek WR, Pryde EH, JAOCS, 63, 13 (1986)

[15] Watanabe S, JAOCS, 50, 360 (1973)

[16] Mork PC, JAOCS, 53, 506 (1973)

[17] Bard AJ, "Chemical Equilibrium," 40-60, Harper & Row Publishers, New York, Evanston and London (1966)