Facile solid-state chemical synthesis of novel ternary lanthanide complexes at room temperature

Article abstract of DOI:10.1080/15533174.2011.609225

This paper reports a facile one-step synthesis of two ternary lanthanide complexes via room temperature solid-state reactions of lanthanide chloride hydrates with two ligands, potassium sorbate (PS), and 8-hydroxyquinoline (8-hq). The structural features, composition, and the morphologies of two complexes are characterized by elemental analysis, UV-Vis, FT-IR, XRD, SEM, and EDX. The thermal property of two ternary lanthanide complexes was also investigated. UV-Vis and FT-IR results confirm the coordination of lanthanide ion with two ligands. XRD results show that signals of complexes are not from reactants, and are believed to originate from the corresponding ternary lanthanide complex.

Full text of DOI:10.1080/15533174.2011.609225

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Facile Solid-State Chemical Synthesis of Novel Ternary
Lanthanide Complexes at Room Temperature
a
b
a
a
Xiao-Fei Yang , Rong-Xian Zhang , Fan Yao & Wei-Meng Ouyang
a
School of Materials Science and Engineering, Jiangsu University, Zhenjiang, China
School of Chemistry and Chemical Engineering, Jiangsu University, Zhenjiang, P. R. China
b
Published online: 31 Jan 2012.
To cite this article: Xiao-Fei Yang , Rong-Xian Zhang , Fan Yao & Wei-Meng Ouyang (2012) Facile Solid-State Chemical
Synthesis of Novel Ternary Lanthanide Complexes at Room Temperature, Synthesis and Reactivity in Inorganic, Metal-Organic,
and Nano-Metal Chemistry, 42:1, 37-41, DOI: 10.1080/15533174.2011.609225
To link to this article: http://dx.doi.org/10.1080/15533174.2011.609225
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Synthesis and Reactivity in Inorganic, Metal-Organic, and Nano-Metal Chemistry, 42:37–41, 2012
Copyright ꢀC Taylor & Francis Group, LLC
ISSN: 1553-3174 print / 1553-3182 online
DOI: 10.1080/15533174.2011.609225
Facile Solid-State Chemical Synthesis of Novel Ternary
Lanthanide Complexes at Room Temperature
1
2
1
1
Xiao-Fei Yang, Rong-Xian Zhang, Fan Yao, and Wei-Meng Ouyang
1
School of Materials Science and Engineering, Jiangsu University, Zhenjiang, China
School of Chemistry and Chemical Engineering, Jiangsu University, Zhenjiang, P. R. China
2
also prevent lanthanide complexes from being further used in a
This paper reports a facile one-step synthesis of two ternary variety of areas.
lanthanide complexes via room temperature solid-state reactions
of lanthanide chloride hydrates with two ligands, potassium sor-
bate (PS), and 8-hydroxyquinoline (8-hq). The structural features,
composition, and the morphologies of two complexes are character-
ized by elemental analysis, UV-Vis, FT-IR, XRD, SEM, and EDX.
It has been confirmed that the room temperature solid-state
reaction is a facile and effective strategy to prepare a large
[19–28]
number of compounds and materials.
Solid state synthesis
at room temperature is known to have several advantages over
The thermal property of two ternary lanthanide complexes was conventional solution-phase synthesis, including solvent-free,
also investigated. UV-Vis and FT-IR results confirm the coordi- high yield, greener, and low energy consumption. To the best
nation of lanthanide ion with two ligands. XRD results show that
signals of complexes are not from reactants, and are believed to
ternary lanthanide complexes has been rarely reported so far.
originate from the corresponding ternary lanthanide complex.
of our knowledge, room temperature solid-state synthesis of
Preliminary work in our group aimed at solid-state synthe-
sis, characterization, and properties of binary and ternary lan-
thanide complexes by a room temperature chemical reaction
Keywords potassium sorbate, room temperature, solid state synthe-
sis, ternary lanthanide complexes
of lanthanide chloride hydrates with different hydroxybenzoate
sodium salts, and 8-hydroxyquinoline (8-hq).[
29–31]
As is well
known, potassium sorbate (PS) is used to inhibit molds and
yeasts in many foods and is also used in personal care products
to inhibit the development of microorganisma for shelf stability.
It is believed that the solid-state coordination reaction of lan-
thanide ion with PS and 8-hq leads to the development of novel
ternary rare earth complex-based antibacterial agents and mate-
rials. Herein we extended our previous approach and synthesized
two novel ternary lanthanide complexes at room temperature via
a rapid one-step solid-state coordination reaction of lanthanide
chloride hydrates with PS and 8-hq. Due to characteristics of
ternary lanthanide complexes and their wide applications, our
findings may have implications in the low-cost, environmentally
friendly scalable synthesis of functional materials derived from
ternary lanthanide complex.
INTRODUCTION
In the past decade, the synthesis of novel lanthanide com-
plexes and materials has been intensively developed not only for
its fundamental scientific interest but also for many technologi-
[
1–5]
cal applications, such as in catalysis,
organic light-emitting
diodes (OLEDs),[
6–8]
magnetic resonance imaging (MRI),
[9–13]
[
14–18]
and luminscent materials.
The coordination chemistry of
lanthanide ions plays an important role in the design, synthesis,
and application of novel functional materials. However, the over-
whelming majority of ternary lanthanide complexes reported
were prepared in alcohol/water co-solvent systems. The wet
chemical synthesis of lanthanide complexes often requires large
amounts of solvents to dissolve reactants, together with the use
of a base to neutralize acidic solution and initiate the coor-
dination. This may restrict the large-scale synthesis of novel
functional materials originating from lanthanide complexes and
EXPERIMENTAL
Materials
Received 11 February 2011; accepted 26 July 2011.
This work was financially supported by the National Natural Sci-
ence Foundation of China (Grant No. 51102116) and Natural Science
Foundation of Jiangsu (BK2011480).
Address correspondence to Xiao-Fei Yang, School of Materials
Science and Engineering, Jiangsu University, Zhenjiang 121013, P. R.
China. E-mail: xyang@ujs.edu.cn
Lanthanide (III) chloride hydrates (LaCl3· 6H2O,
YCl3·6H2O) were obtained by dissolving corresponding lan-
thanide oxide (La2O3, Y2O3, 99.99%, Shanghai Yuelong,
China) in 6 M HCl, and the resulting solution was evaporated and
dried in vacuum to give the product as a white solid. Potassium
sorbate (AR), 8-Hydroxyquinoline (AR), and absolute ethanol
37

38
X.-F. YANG ET AL.
(AR) were purchased from Sinopharm Chemical Reagent Co.,
Ltd, and used as received without further purification.
Preparation of Ternary Lanthanide Complexes
In a typical synthesis, accurately weighed potassium sor-
bate (PS, 1.5 g, 10 mmol) and 8-hydroxyquinoline (8-hq, 2.9 g,
20 mmol) were first ground separately in the agate mortar to
give fine powders, and two ligands were then mixed and ground
gently for 30 min at room temperature. Consequently, the ap-
propriate amount of lanthanide chloride (3.53 g for LaCl3·6H2O
and 3.03 g for YCl3 ·6H2O, 10 mmol) was added to the mixture
of two ligands. The color of the mixture changed gradually from
light yellow to deep yellow with continuous grinding for 2 h,
indicating the coordination of lanthanide ion with ligands. The
resulting mixture was kept on grinding at room temperature for
a further 30 min before washing with deionized water and al-
cohol for three times. The obtained powders were then dried in
◦
FIG. 1. UV-Vis spectra of two ligands and as-synthesized ternary lanthanide
complexes (color figure available online).
vacuum at 60 C overnight to give the product as yellow solids.
Characterization
thanide complexes and two ligands were examined by solid-state
UV-Vis spectroscopy and the results are shown in Figure 1.
It is clearly shown in Figure 1 that the spectrum of 8-hq
shows two peaks at 243 nm and 317 nm, corresponding to
Elemental analyses of two ternary lanthanide complexes
were carried out using a Flash 111A elemental analyzer. UV-Vis
spectra were recorded within 200–600 wavelength range using a
Shimadzu UV2450 spectrometer. FT-IR spectra were recorded
∗
π-π transition from quinoline ring while the spectrum of PS
−1
within 4000–400 cm wave number range using a Nicolet
Nexus 470 IR spectrometer with the KBr pellet technique. X-ray
diffraction (XRD) patterns were collected on a Bruker AXS D8
Superseed X-ray diffractometer using Ni-filtered Cu Kα radia-
tion (40 Kv, 250 mA). The morphologies of the as-synthesized
products were examined by field-emission scanning electron
microscopy (FESEM; JEOL, JSM-7001F). The elemental com-
positions of ternary lanthanide complexes were analyzed with
energy-dispersive X-ray spectroscopy (EDX) attached to FE-
SEM instrument. Thermogravimetry properties (TGA) of two
∗
exhibits a peak at 244 nm assigned to come from π-π transition
from –C C-C C-.[ Obvious red shifts were observed in UV-
Vis spectra of two ternary lanthanide complexes where two
main peaks are found around 260 nm and 380 nm, respectively,
suggesting the coordination of lanthanum ion with PS and 8-
hq. The red shift is caused by the decrease of energy between
two energy levels because of the redistribution of energy in
the bigger system after the coordination. The similarity in the
spectra of SSR001 and SSR002 was observed.
32]
ternary lanthanide complexes were measured under nitrogen on IR Spectra
◦
a Netzsch STA 449C simultaneous thermal analyzer from 25 C
to 1000 C.
Due to the similarity of two ternary lanthanide complexes,
SSR 001 and SSR 002, only the IR spectrum of SSR 001 was
chosen and is shown in Figure 2. Not all of the spectrum has to
be identified and there only four characteristic peaks appearing
in the IR spectra of 8-hq that need to be identified, two peaks
◦
RESULTS AND DISCUSSION
Elemental Analysis Results
−1
−1
at 3140 cm and 1223 cm are attributed to O-H stretching
−1
For the ternary lanthanum complex SSR001, Anal. Calc. and bending vibrations, and two peaks at 1093 cm and 1578
−1
LaC30H26O6N2: C, 55.48; H, 4.04; N, 4.31; Found C, 55.15; cm correspond to C-O and C N stretching vibrations, re-
H, 3.95; N, 4.48. For the ternary yttrium complex SSR002, spectively. For the same reason, three main peaks presenting
Anal. Calcd. YC30H26O6N2: C, 60.11; H, 4.37; N, 4.67; Found in the IR spectra of PS were observed and analyzed, in which
C, 59.74; H, 4.25; N, 4.74. According to elemental analysis peaks at 1398 cm and 1558 cm are assigned to symmetric
results, two ternary lanthanide complexes are suggested to have and asymmetric stretching vibrations of COO group, while the
−1
−1
−1
[33]
general formula of Ln(PS)2(hq)2 (Ln = La, Y).
peak at 1008 cm belongs to the bending vibration of C-H.
In the IR spectrum of ternary lanthanum complex SSR 001,
UV-Vis Spectra
the sharp peaks corresponding to symmetric (ν ), asymmetric
s
The chelation of rare earth ion with unsaturated conjugated stretching (νas) vibrations of COO group and stretching (νC N)
−
−1
1
functional ligands frequently leads to changes in the absorbance vibration of O-H exhibit obvious shifts, from 1398 cm , 1558
−1
−1
of the chromophore. In order to investigate the coordination cm , and 1578 cm , to lower frequency 1315 cm , 1464
−1
−1
of lanthanide ions with two different ligands, two ternary lan- cm , and 1568 cm , indicating the chelation of the lanthanum

FACILE SOLID-STATE CHEMICAL SYNTHESIS
39
FIG. 3. XRD patterns of reactants and as-synthesized ternary lanthanide com-
plexes (color figure available online).
FIG. 2. FT-IR spectra of two ligands and the ternary lanthanide complex
SSR001 (color figure available online).
ion with both two ligands, PS and 8-hq. In comparison with the
−
1
difference between symmetric (νs, 1398 cm ) and asymmetric
−1
stretching (νas, 1558 cm ) vibrations of the COO group (ꢀν
−
1
−
1
=
160 cm , PS), the gap between symmetric (νs, 1315 cm )
−1
and asymmetric stretching (νas, 1464 cm ) vibrations of COO
−1
group (ꢀν = 149 cm , SSR 001) is indicative of bidentate
[
34]
chelating coordination of lanthanum ion with PS. In the IR
−1
spectrum of SSR001, the stretching (νO-H, 8-hq, 3140 cm )
and bending vibrations (δO-H, 8-hq, 1223 cm ) disappear and
the stretching vibration (νC N, 8-hq) at 1093 cm moves to
higher frequency (1103 cm ), also suggesting the coordination
of lanthanum ion with 8-hq.
−
1
−1
−1
XRD Analysis
Figure 3 exhibits the XRD patterns of three reactants, lan-
thanide chloride hydrates, 8-hq, PS, and as-prepared ternary
lanthanum complexes SSR001 and SSR002. It is clearly shown
that no signal from three reactants was detected in the XRD pat-
terns of as-synthesized ternary lanthanide complexes SSR001
and SSR002, and new diffraction peaks were found, although
the intensities are relatively weak, suggesting the completion of
solid-state reactions of three reactants at room temperature and
confirming room temperature is insufficient for the formation of
crystalline ternary lanthanide complexes. The similarity in the
XRD patterns of two complexes indicates that solid-state reac-
tions of different lanthanide chloride hydrates with 8-hq and PS
result in the generation of lanthanide complexes with similar
structures.
SEM and EDX Results
Further characterizations have been performed to confirm
the morphology and the composition of the ternary lanthanide
complex. SEM image and EDX analysis of SSR001 are shown in
FIG. 4. SEM image (a) and EDX analysis (b) of the ternary lanthanide complex
Figure 4, in which the obtained lanthanide complex is observed SSR001 (color figure available online).

40
X.-F. YANG ET AL.
◦
the ternary lanthanide complex in the range of 550–1000 C.
The total mass loss of SSR001 is 40.9% including 5.4% loss
of remaining water and solvents in the first stage, mass loss of
24.1% in the second stage, and 11.4% weight loss in the final
stage. The mass loss of SSR002 in first step is 8.2%, followed by
the weight loss of 21.6 in second step and a mass loss of 8.2% in
final step. In brief, as-synthesized ternary lanthanide complexes
showed better thermal stability than that of two ligands, 8-hq
and PS.
On the basis of previous results, general structure of the as-
synthesized two ternary lanthanide complexes is proposed and
shown in Figure 6.
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