Thermal Decomposition Characteristics of NdCl3･6H2O

doi:10.12972/ksmer.2014.51.2.202

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2014 Vol.51, Issue 2 Preview Page Next Page

Research Paper

Thermal Decomposition Characteristics of NdCl3･6H2O NdCl3･6H2O의 열적 분해 특성에 관한 연구: 김정운·이원근·황인성·이진영·한춘
Joung Woon Kim, Wongeun Lee, Insung Hwang, Jin-young Lee,Choon Han

30 April 2014. pp. 202-210

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Abstract

Anhydride NdCl₃was prepared from NdCl₃·6H₂O and the anhydrous reaction mechanisms were identified by variables such as reaction temperature, reaction time and influent gas. Thermal decomposition reaction of NdCl_3·6H₂O was studied by 5 steps (130°C, 150°C, 190°C, 250°C, 400°C) using a differential thermal analysis (DTA). Results showed that stepwise dehydration proceeded with increasing temperature and completed at 400°C. Under HCl/Ar atmosphere, anhydride was completely prepared in 2 hour, whereas by-products were produced from Nd₂O₃ and Nd(OH)₂Cl after a 3 hour heat treatment. Meanwhile, anhydrous chlorides were produced under HCl/Ar atmosphere, whereas oxides were produced under Ar atmosphere. Optimally, NdCl₃was prepared from NdCl₃·6H₂O by a 2 hour heat treatment at 400°C under HCl/Ar atmosphere.

Keywords

NdCl₃

NdCl₃·6H₂O

Dehydration

Thermal decomposition

DTA

NdCl₃는 NdCl₃·6H₂O로부터 제조되고, 이 때의 무수화 반응 메커니즘은 반응 온도, 반응 시간, 유입되는 가스와 같은 실험변수에 의해 해석되었다. NdCl₃·6H₂O의 열적 분해 반응은 differential thermal analysis (DTA) 분석을 통해 130°C, 150°C, 190°C, 250°C, 400°C의 5단계로 연구가 수행되었다. 온도가 상승함에 따라 단계적으로 수화물이 제거 되는 결과를 확인하였고 400°C에서 무수화물을 제조하였다. HCl/Ar 분위기에서 2시간 반응시 완벽하게 무수화물이 제조되는 반면에 3시간 열처리 후,에는 Nd₂O₃와 Nd(OH)₂Cl이 부산물로 생성되었다. 한편, HCl/Ar 분위기에서는 무수 염화물이 제조 되는 반면에 Ar분위기에서 산화물이 생성되었다. 최종적으로 NdCl₃는 NdCl₃·6H₂O로부터 HCl/Ar 분위기하에서 400°C 온도에서 2시간의 열처리 과정을 거쳐 제조 되었다.

키워드

NdCl₃

NdCl₃·6H₂O

탈수

열적 분해

DTA

References

Amundsen, K., Eklund, H.R. and Schmidt, R., 2000, “Process for producing anhydrous MgCl2,” U. S. patent, US 6,042,794.
Ashcroft, S.J. and Mortimer, C.T., 1968, “The thermal decomposition of lanthanide(III) chloride hydrates,” J. of the Less-Common Metals, Vol. 14, pp. 403-406.
Eom, H.-C., Park, H. and Yoon, H.-S., 2010, “Preparation of anhydrous magnesium chloride from ammonium magnesium chloride hexahydrate,” Advanced Powder Technology, Vol. 21, pp. 125-130.
Haeseler, G. and Matthes, F., 1965, “Uber den thermischen abbau dek chloridhydrate der elemente der deltenen erden,” J. of the Less-Common Metals, Vol. 9, pp. 133-151.
Hedrick, J.B., 2000, Rare earth, U. S. Geological survey minerals yearbook, 2000, p. 62.1-62.10.
Huang, Q., Lu, G., Wang, J. and Yu, J., 2011, “Thermal decomposition mechanisms of MgCl₂·6H₂O and MgCl₂·H₂O,” J. of Analytical and Applied Pyrolysis, Vol. 91, pp. 159-164.
Kashani-Nejad, S., NG, K.W. and Harris, R., 2004, “Preparation of MgOHCl by Controlled Dehydration of MgCl₂·6H₂O,” Metallurgical and Materials Transactions B, Vol. 35B, pp. 405-406.
Kim, S., Yoon, H., Kim, C., Kim, J. and Eom, H., 2005, “Pr epar ation of Cer ium Car bonate fr om Leaching Solution of Oxidation Roasted Bastnasite,” J. of the Korean Society for Geosystem Engineers, Vol. 42, No. 1, pp. 28-34.
Kipouros, G.J. and Sadoway, D.R., 2001, “A thermochemical analysis of the production of anhydrous MgCl₂,” J. of Light Metals, Vol. 1, pp. 111-117.
Kipouros, G.J. and Sharma, R.A., 1990, “Characterization of neodymium trichloride hydrates and neodymium hydroxychloride,” J. of the Less-Common Metals, Vol. 160, pp. 85-99.
Komiyama, M., Matsumura, K. and Matsumoto, Y., 1992, “Unprecedentedly Fast Hydrolysis of the RNA Dinucleoside Monophosphates ApA and UpU by Rare Earth Metal Ions,” J. of the Chemical Society, Chemical Communications, No. 8, pp. 640-641.
Mostashari, S.M. and Moafi, H.F., 2008, “Thermal decomposition pathway of a cellulosic fabric impregnated by magnesium chloride hexahydrate as a flame-retardant,” J. of Thermal Analysis and Calorimetry, Vol. 93, No. 2, pp. 589-594.
Munhwa Ilbo, 2013.10.23, www.munhwa.com/news/view. html?no= 2013102301070132256002.
Park, J., An, Ki., Han, C., Lee, J., Kim, S., Yoon, H. and Kim, J., 2003, “Separation of Heavy Rare Earth Elements (Dy, Ho, Er) by the Extraction Chromatography Method using P₅₀₇ Resin,” J. of the Korean Society for Geosystem Engineers, Vol. 40, No. 4, pp. 248-257.
Rard, J.A., Oakes, C.S. and Archer, D.G., 2004, “Enthalpies of Dilution of NdCl₃(aq) at Temperatures from 297.89 K to 372.08 K and an Extended Pitzer Ion-Interaction Model for the NdCl₃ + H₂O System,” J. of Chemical and Engieering Data, Vol. 49, pp. 313-325.
Saito, Y., Kawabata, K. and Okuda, M., 1995, “Single- Layered Carbon Nanotubes Synthesized by Catalytic Assistance of Rare-Earths in a Carbon Arc,” J. of Physical Chemistry, Vol. 99, pp. 16076-16079.
Saito, Y., Okuda, M. and Yoshikawa, T., 1994, “Correlation between Volatility of Rare Earth Metals and Encapsulation of Their Carbides in Carbon Nanocapsules,” J. of Physical Chemistry, Vol. 98, No. 27, pp. 6696-6698.
Schob, O. and Parthe, 1965, “AB Compounds with Se, Y and Rare Earth Metals I. Scandium and Yttrium Compounds with CrB and CsCI Structure,” Acta Crystallographica, Vol. 19, pp. 214-224.
Shin, H., Kim, J. and Kim, J., 2013, “Feasibility Study on the Recovery for Valuable Minerals in Beach Sand,” J. of the Korean Society of Mineral and Energy Resources Engineers, Vol. 50, No. 4, pp. 534-542.
Skriver, H. and Mertig, I., 1990, “Electron-phonon coupling in the rare-earth metals,” Physical Review B, Vol. 41, No. 10, pp. 6553-6557.
Taylor, S.R., 1964, “Abundance of chemical elements in the continental crust: a new table,” Geochimica et Cosmochimica Acta, Vol. 28, pp. 1273-1285.
Wu, Y.-L., Huang, X.-F., Yang, M.-D., Zou, S.-P., Dang, J. and Hu, H.-S., 2008, “Study on the mechanisms and kinetics of complex’'s thermal decomposition getting anhydrous magnesium chloride,” J. of Analytical and Applied Pyrolysis, short communication, Vol. 81, pp. 133-135.
Yadav, T., Longmont and CO (US), 2007, “Nanoparticles of rare earth oxides,” U. S. patent, US 7,229,600 B2.

Information

Publisher :The Korean Society of Mineral and Energy Resources Engineers
Publisher(Ko) :한국자원공학회
Journal Title :Journal of the Korean Society of Mineral and Energy Resources Engineers
Journal Title(Ko) :한국자원공학회지
Volume : 51
No :2
Pages :202-210
DOI :https://doi.org/10.12972/ksmer.2014.51.2.202

[1] Amundsen, K., Eklund, H.R. and Schmidt, R., 2000, “Process for producing anhydrous MgCl2,” U. S. patent, US 6,042,794.

[2] Ashcroft, S.J. and Mortimer, C.T., 1968, “The thermal decomposition of lanthanide(III) chloride hydrates,” J. of the Less-Common Metals, Vol. 14, pp. 403-406.

[3] Eom, H.-C., Park, H. and Yoon, H.-S., 2010, “Preparation of anhydrous magnesium chloride from ammonium magnesium chloride hexahydrate,” Advanced Powder Technology, Vol. 21, pp. 125-130.

[4] Haeseler, G. and Matthes, F., 1965, “Uber den thermischen abbau dek chloridhydrate der elemente der deltenen erden,” J. of the Less-Common Metals, Vol. 9, pp. 133-151.

[5] Hedrick, J.B., 2000, Rare earth, U. S. Geological survey minerals yearbook, 2000, p. 62.1-62.10.

[6] Huang, Q., Lu, G., Wang, J. and Yu, J., 2011, “Thermal decomposition mechanisms of MgCl₂·6H₂O and MgCl₂·H₂O,” J. of Analytical and Applied Pyrolysis, Vol. 91, pp. 159-164.

[7] Kashani-Nejad, S., NG, K.W. and Harris, R., 2004, “Preparation of MgOHCl by Controlled Dehydration of MgCl₂·6H₂O,” Metallurgical and Materials Transactions B, Vol. 35B, pp. 405-406.

[8] Kim, S., Yoon, H., Kim, C., Kim, J. and Eom, H., 2005, “Pr epar ation of Cer ium Car bonate fr om Leaching Solution of Oxidation Roasted Bastnasite,” J. of the Korean Society for Geosystem Engineers, Vol. 42, No. 1, pp. 28-34.

[9] Kipouros, G.J. and Sadoway, D.R., 2001, “A thermochemical analysis of the production of anhydrous MgCl₂,” J. of Light Metals, Vol. 1, pp. 111-117.

[10] Kipouros, G.J. and Sharma, R.A., 1990, “Characterization of neodymium trichloride hydrates and neodymium hydroxychloride,” J. of the Less-Common Metals, Vol. 160, pp. 85-99.

[11] Komiyama, M., Matsumura, K. and Matsumoto, Y., 1992, “Unprecedentedly Fast Hydrolysis of the RNA Dinucleoside Monophosphates ApA and UpU by Rare Earth Metal Ions,” J. of the Chemical Society, Chemical Communications, No. 8, pp. 640-641.

[12] Mostashari, S.M. and Moafi, H.F., 2008, “Thermal decomposition pathway of a cellulosic fabric impregnated by magnesium chloride hexahydrate as a flame-retardant,” J. of Thermal Analysis and Calorimetry, Vol. 93, No. 2, pp. 589-594.

[13] Munhwa Ilbo, 2013.10.23, www.munhwa.com/news/view. html?no= 2013102301070132256002.

[14] Park, J., An, Ki., Han, C., Lee, J., Kim, S., Yoon, H. and Kim, J., 2003, “Separation of Heavy Rare Earth Elements (Dy, Ho, Er) by the Extraction Chromatography Method using P₅₀₇ Resin,” J. of the Korean Society for Geosystem Engineers, Vol. 40, No. 4, pp. 248-257.

[15] Rard, J.A., Oakes, C.S. and Archer, D.G., 2004, “Enthalpies of Dilution of NdCl₃(aq) at Temperatures from 297.89 K to 372.08 K and an Extended Pitzer Ion-Interaction Model for the NdCl₃ + H₂O System,” J. of Chemical and Engieering Data, Vol. 49, pp. 313-325.

[16] Saito, Y., Kawabata, K. and Okuda, M., 1995, “Single- Layered Carbon Nanotubes Synthesized by Catalytic Assistance of Rare-Earths in a Carbon Arc,” J. of Physical Chemistry, Vol. 99, pp. 16076-16079.

[17] Saito, Y., Okuda, M. and Yoshikawa, T., 1994, “Correlation between Volatility of Rare Earth Metals and Encapsulation of Their Carbides in Carbon Nanocapsules,” J. of Physical Chemistry, Vol. 98, No. 27, pp. 6696-6698.

[18] Schob, O. and Parthe, 1965, “AB Compounds with Se, Y and Rare Earth Metals I. Scandium and Yttrium Compounds with CrB and CsCI Structure,” Acta Crystallographica, Vol. 19, pp. 214-224.

[19] Shin, H., Kim, J. and Kim, J., 2013, “Feasibility Study on the Recovery for Valuable Minerals in Beach Sand,” J. of the Korean Society of Mineral and Energy Resources Engineers, Vol. 50, No. 4, pp. 534-542.

[20] Skriver, H. and Mertig, I., 1990, “Electron-phonon coupling in the rare-earth metals,” Physical Review B, Vol. 41, No. 10, pp. 6553-6557.

[21] Taylor, S.R., 1964, “Abundance of chemical elements in the continental crust: a new table,” Geochimica et Cosmochimica Acta, Vol. 28, pp. 1273-1285.

[22] Wu, Y.-L., Huang, X.-F., Yang, M.-D., Zou, S.-P., Dang, J. and Hu, H.-S., 2008, “Study on the mechanisms and kinetics of complex’'s thermal decomposition getting anhydrous magnesium chloride,” J. of Analytical and Applied Pyrolysis, short communication, Vol. 81, pp. 133-135.

[23] Yadav, T., Longmont and CO (US), 2007, “Nanoparticles of rare earth oxides,” U. S. patent, US 7,229,600 B2.

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