1070-4272/03/7604-0661 $25.00 C 2003 MAIK [Nauka/Interperiodica]
Russian Journal of Applied Chemistry, Vol. 76, No. 4, 2003, pp. 661!662. Translated from Zhurnal Prikladnoi Khimii, Vol. 76, No. 4, 2003,
Original Russian Text Copyright + 2003 by Gordina, Prokof’ev, Il’in.
Synthesis of NaA Zeolite by Mechanochemical Methods
N. E. Gordina, V. Yu. Prokof’ev, and A. P. Il’in
Ivanovo State University of Chemical Technology, Ivanovo, Russia
Received September 13, 2002
Abstract-A method for obtaining NaA zeolite by mechanochemical activation of a raw material is proposed.
The method produces no wastewater in the course of zeolite synthesis.
It is known that synthesis of zeolites by their pre-
cipitation from solutions leads to formation of a con-
siderable amount of wastewater . Therefore, devel-
opment of new methods for production of zeolites is
a promising direction of research in the field of syn-
thesis of these compounds.
In the present study, it is proposed to synthesize
a NaA zeolite by mechanochemical treatment of raw
materials, which yields the product without any li-
To carry out mechanochemical synthesis under
[mild] conditions [2, 3], it is preferable to use com-
pounds containing constitution water. This is the
reason why aluminum hydroxide Al(OH)
lite), sodium silicate Na
O and silica gel
O with n = 0.875 were chosen as raw ma-
terial. The component ratio corresponds to the stoi-
chiometry of the reaction producing NaA zeolite:
O) + 12Al(OH)
O . 6Al
The synthesis was performed in a VM-4 roller vib-
rating mill with impact-shear loading, vibration fre-
quency of 930 min
, and energy load of 5.4 kW kg
in the course of 30 min. Then a sample obtained was
calcined at 450oC for 4 h. The resulting zeolite was
identified by comparing its characteristics with pub-
lished data  and parameters of a commercial NaA
zeolite [TU (Technical Specifications) 38-83-047388].
An X-ray phase analysis was made on a DRON-3M
diffractometer with Cu
radiation, and a differen-
tial-thermal analysis, on a Q-1500D derivatograph
(Hungary) in air at sample heating rate of 5 deg min
IR spectra of samples compacted with KBr in 5% dilu-
tion were measured on a Nicolet AVATAR 360 FT-IR
IR spectrometer in the 40031250 cm
As shown by the experimental data obtained (Fig. 1),
the X-ray diffraction pattern of the starting mixture
used to synthesize the A zeolite contains diffraction
peaks of hydrargillite and sodium silicate. After dis-
pergation of the mixture for 30 min the reflections as-
sociated with sodium silicate disappear, and the inten-
sity of reflections corresponding to hydrargillite de-
creases substantially (by approximately a factor of 3).
New peaks appear at diffraction angles 2q 14.0o,
24.3o, 34.4o, 42.7o, and 52.0o. Comparison of the
X-ray diffraction pattern with published data suggests
Fig. 1. X-ray diffraction patterns (Cu
radiation) of mix-
tures used to synthesize NaA zeolite. (2q) Bragg angle.
HG stands for hydrargillite, and SS, for sodium silicate.
Time of dispergation (min): (a) 0 and (b) 30; (c) calcined