Use of Ethylamine, Diethylamine and Triethylamine in the Synthesis of Zn,Al Layered Double Hydroxides

Abstract

Amines with two carbon atoms in the organic chain [ethylamine (EA), diethylamine (DEA), triethylamine (TEA)] have been used as precipitant agents to obtain a hydrotalcite-like compound with Zn (II) and Al (III) as layered cations and with nitrate anions in the interlayered region to balance the charge. This Layered Double Hydroxide was prepared following the coprecipitation method, and the effect on the crystal and particle sizes was studied. Also, the effect of submitting the obtained solids to hydrothermal post-synthesis treatment by conventional heating and microwave assisted heating were studied. The obtained solids were exhaustively characterized using several instrumental techniques, such as X-ray diffraction, Thermal Analysis (DTA and TG), Chemical Analysis, Infrared Spectroscopy (FT-IR), determination of Particle Size Distribution and BET-Surface area. Well crystallized solids were obtained showing two possible LDH phases, depending on the orientation of the interlayer anion with respect to the brucite-like layers. The results indicated that there is a certain influence of the amine, when used as a precipitating agent, and as a consequence of the degree of substitution, on the crystallinity and particle size of the final solid obtained. The LDHs obtained using TEA exhibited higher crystallinity, which was improved after a long hydrothermal treatment by conventional heating. Regarding the shape of the particles, the formation of aggregates in the former solid was detected, which could be easily disintegrated using ultrasound treatments, producing solid powder with high crystallinity and small particle size, with homogeneous size distribution.

Keywords

• LDHs
• hydrotalcite
• amines
• coprecipitation method
• hydrothermal treatment
• crystallinity