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Title: An Efficient, Solvent-Free Process for Synthesizing Anhydrous MgCl 2

Abstract

A new efficient and solvent-free method for the synthesis of anhydrous MgCl2 from its hexahydrate is proposed. Fluidized dehydration of MgCl 2·6H 2O feedstock at 200 °C in a porous bed reactor yields MgCl2·nH2O (0 < n < 1), which has a similar diffraction pattern as activated MgCl2. The MgCl 2·nH 2O is then ammoniated directly using liquefied NH 3 in the absence of solvent to form MgCl 2·6NH 3. Calcination of the hexammoniate complex at 300 °C then yields anhydrous MgCl 2. Both dehydration and deammoniation were thoroughly studied using in situ as well as ex situ characterization techniques. Specifically, a detailed understanding of the dehydration process was monitored by in situ PXRD and in situ FTIR techniques where formation of salt with nH 2O (n = 4, 2, 1, <1) was characterized. Given the reduction in thermal energy required to produce dehydrated feedstock with this method compared with current strategies, significant cost benefits are expected. Overall, the combined effect of activation, macroporosity, and coordinated water depletion allows the formation of hexammoniate without using solvent, thus minimizing waste formation.

Authors:
; ; ; ; ; ; ; ;
Publication Date:
Research Org.:
Pacific Northwest National Lab. (PNNL), Richland, WA (United States)
Sponsoring Org.:
USDOE
OSTI Identifier:
1422284
Report Number(s):
PNNL-SA-119379
Journal ID: ISSN 2168-0485; CJ0100000
DOE Contract Number:  
AC05-76RL01830
Resource Type:
Journal Article
Resource Relation:
Journal Name: ACS Sustainable Chemistry & Engineering; Journal Volume: 6; Journal Issue: 1; Related Information: 1048-1054
Country of Publication:
United States
Language:
English

Citation Formats

Motkuri, Radha K., Vemuri, Venkata Rama S., Barpaga, Dushyant, Schaef, Herbert T., Loring, John S., Martin, Paul F., Lao, David, Nune, Satish K., and McGrail, Bernard P. An Efficient, Solvent-Free Process for Synthesizing Anhydrous MgCl2. United States: N. p., 2018. Web. doi:10.1021/acssuschemeng.7b03366.
Motkuri, Radha K., Vemuri, Venkata Rama S., Barpaga, Dushyant, Schaef, Herbert T., Loring, John S., Martin, Paul F., Lao, David, Nune, Satish K., & McGrail, Bernard P. An Efficient, Solvent-Free Process for Synthesizing Anhydrous MgCl2. United States. doi:10.1021/acssuschemeng.7b03366.
Motkuri, Radha K., Vemuri, Venkata Rama S., Barpaga, Dushyant, Schaef, Herbert T., Loring, John S., Martin, Paul F., Lao, David, Nune, Satish K., and McGrail, Bernard P. Tue . "An Efficient, Solvent-Free Process for Synthesizing Anhydrous MgCl2". United States. doi:10.1021/acssuschemeng.7b03366.
@article{osti_1422284,
title = {An Efficient, Solvent-Free Process for Synthesizing Anhydrous MgCl2},
author = {Motkuri, Radha K. and Vemuri, Venkata Rama S. and Barpaga, Dushyant and Schaef, Herbert T. and Loring, John S. and Martin, Paul F. and Lao, David and Nune, Satish K. and McGrail, Bernard P.},
abstractNote = {A new efficient and solvent-free method for the synthesis of anhydrous MgCl2 from its hexahydrate is proposed. Fluidized dehydration of MgCl2·6H2O feedstock at 200 °C in a porous bed reactor yields MgCl2·nH2O (0 < n < 1), which has a similar diffraction pattern as activated MgCl2. The MgCl2·nH2O is then ammoniated directly using liquefied NH3 in the absence of solvent to form MgCl2·6NH3. Calcination of the hexammoniate complex at 300 °C then yields anhydrous MgCl2. Both dehydration and deammoniation were thoroughly studied using in situ as well as ex situ characterization techniques. Specifically, a detailed understanding of the dehydration process was monitored by in situ PXRD and in situ FTIR techniques where formation of salt with nH2O (n = 4, 2, 1, <1) was characterized. Given the reduction in thermal energy required to produce dehydrated feedstock with this method compared with current strategies, significant cost benefits are expected. Overall, the combined effect of activation, macroporosity, and coordinated water depletion allows the formation of hexammoniate without using solvent, thus minimizing waste formation.},
doi = {10.1021/acssuschemeng.7b03366},
journal = {ACS Sustainable Chemistry & Engineering},
number = 1,
volume = 6,
place = {United States},
year = {Tue Jan 02 00:00:00 EST 2018},
month = {Tue Jan 02 00:00:00 EST 2018}
}