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  • 1 Department of Inorganic and Analytical Chemistry, West Pomeranian University of Technology, Szczecin, al. Piastów 42, 71-065, Szczecin, Poland
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Abstract

A new compound in the Al–Sb–V–O system of the composition AlSbVO6 was successfully synthesized by a solid-state reaction and characterized by powder XRD diffraction. The structural and thermal properties of AlSbVO6 were investigated. The infra-red spectrum of the new phase is presented.

Abstract

A new compound in the Al–Sb–V–O system of the composition AlSbVO6 was successfully synthesized by a solid-state reaction and characterized by powder XRD diffraction. The structural and thermal properties of AlSbVO6 were investigated. The infra-red spectrum of the new phase is presented.

Introduction

Mixed metal oxides of rutile or rutile-like structure have been the subjects of increasing interest because of their potential use as catalysts of many industrial processes, in particular in direct synthesis of acrylonitrile from propane [14]. This reaction is an attractive alternative to the currently used industrial process of production of acrylonitrile from propylene, because propane is much cheaper than the olefin [5, 6]. Acrylonitrile is an important industrial chemical intermediate used in the production of acrylic and modacrylic fibers, rubbers, other important chemicals, and resins. Several papers have been published on the catalysts used for propane ammoxidation, but the major part of the reported work has been concentrated on two types of catalysts, the antimonates of rutile structure [7, 8] and molybdates [911]. Vanadium-antimony mixed oxides have exhibited high selectivity and activity as catalysts of this process [12, 13]. Better performance was obtained when alumina was incorporated into V–Sb–O oxide owing to the occurrence of specific structural effects [1416]. The active structure in the Al–Sb–V–O system is a bulk phase, which is directly formed in the catalyst synthesis. It is a trirutile-like phase Al1−xSbVxO4 (0 < x < 0.5), and the presence of excess of aluminum in the synthesis is critical for its formation [17, 18]. Thus, the aluminum is not only a catalysts support, but it is also a component of the active phase.

Our previous investigation and literature information have implied that there exist a series of new compounds of the general formula M′MSbO6 (where M′ = Cr, Rh, Fe and M = Ru, V, Ti, Te, Ge, Sn) of rutile-type structures [1922]. Hence, the aim of this investigation was to check on the formation of AlSbVO6 compound in the quaternary system Al–Sb–V–O. This compound can be a promising candidate for the development of a process of direct acrylonitrile synthesis from propane.

Another important objective of this study was an attempt to determine the structural and thermal properties of the compound obtained.

Experimental

In the experiments the following reactants were used: Al2O3, a.p. (POCh, Poland), V2O5, a.p. (POCh, Poland), and α-Sb2O4, obtained by oxidation of commercial Sb2O3 (Merck, Germany) in air, in the following stages: 500 °C (24 h) → 550 °C (72 h). The other compounds AlVO4, SbVO5, and AlSbO4 were obtained separately. These compounds were obtained by the solid-state reaction between appropriate mixtures of the oxides Al2O3, V2O5, and α-Sb2O4, under conditions described in literature [2325].

Mixtures of various reagents (Table 1) were weighed in suitable proportions, carefully homogenized by grinding and then shaped into tablets. The tablets were placed in porcelain crucibles and heated in air or argon atmosphere (at the flow rate of 10 dm3/h) until a monophase sample was obtained. All the samples were heated at a temperature range from 550 to 750 °C. On each heating stage the samples were gradually cooled down to room temperature, weighed (their mass changes and their color were recorded), and homogenised by triturating. Finally, all the samples were examined by differential thermal analysis DTA/TG and by X-ray diffraction method to determine their composition.

Table 1

The composition of the initial mixtures and the conditions of synthesis all samples

No.Initial composition of samplesConditions of synthesis stage/temperature/time
1.33.33 mol% Al2O3

33.33 mol% V2O5

33.34 mol% α-Sb2O4
I 550 °C (24 h)

II 600 °C (24 h)

III 650 °C (24 h)

IV 700 °C (24 h)

IV 750 °C (24 h)
2.66.67 mol% AlSbO4

33.33 mol% V2O5
I 600 °C (24 h)

II 700 °C (24 h)

III 750 °C (24 h)
3.66.67 mol% AlVO4

33.33 mol% α-Sb2O4
I 600 °C (24 h)

II 700 °C (24 h)

III 750 °C (24 h)
4.66.67 mol% SbVO5

33.33 mol% Al2O3
I 600 °C (24 h)

II 700 °C (24 h)

III 750 °C (24 h)
5.33.34 mol% SbVO5

33.33 mol% AlVO4

33.33 mol% AlSbO4
I 600 °C (24 h)

II 650 °C (24 h)

III 700 °C (24 h)

The kind of phases contained in the samples was identified on the basis of X-ray phase analysis results (diffractometer HZG-4 (NRD) radiation Cu Kα/filter Ni) and the data found in PDF files [26] as well as in the works [23, 24, 27]. The powder diffraction pattern of AlSbVO6 was recorded at an angular range of 8.5° to 80° 2θ the step size 0.02° (2θ), time per step = 5 s. The intensity of a diffracted beam was recorded using a scintillation counter. The temperature of data collection was equal to 25 °C. The powder diffraction pattern of AlSbVO6 was indexed by means of POWDER program [28, 29].

The density of AlSbVO6 was determined by degassing sample and hydrostatic weighing in pycnometric liquid (CCl4) by the method described in article [30].

The DTA/TG investigations were performed using a Paulik–Paulik-Erdey derivatograph, a product of MOM (Budapest, Hungary). The measurements were conducted in air, in the temperature range 20–1,000 °C and at a constant heating rate of 10 °C/min. All investigations were performed in quartz crucibles. The mass of investigated samples always amounted to 500 mg. The accuracy of temperature reading determined on the basis of repetitions was established as ±5 °C. The DTA/TG measurements in the temperature range 20–1,300 °C were carried out, in inert atmosphere, with the use of an SDT 2960 (TA Instruments).

Initial mixtures and monophase samples were examined by IR spectroscopy. The IR spectra were recorded at wave numbers 1,200–250 cm−1, using a spectrometer of SPECORD M80 (Carl Zeiss, Jena, Germany). A technique used in the measurements was pressing pastilles with KBr at a weight proportion of 1:300.

Results and discussion

The research presented in this study was started with attempts to obtain the compound AlSbVO6 from stoichiometric mixtures of the oxides Al2O3, V2O5, and α-Sb2O4. Further investigation was aimed at preparation of AlSbVO6 from reacting mixtures that contained AlSbO4/V2O5, Al2O3/SbVO5, AlVO4/α-Sb2O4, and AlVO4/AlSbO4/SbVO5. The compositions of the initial mixtures and their heating conditions are presented in Table 1.

The XRD results for all samples after their final heating stage indicate that the initial compounds react with one another in the solid state according to the equations:
1
2
3
4
5

The diffraction patterns of the samples obtained after the last heating stage in air were identical with the diffractograms of the samples obtained in argon atmosphere. AlSbVO6 obtained according to the above reaction has a brownish color. The mass loss calculated on the basis of the reactions (2), (4), and (5) is compatible with the changes in the mass recorded after all the heating stages of samples and amounting to ∼2.5 ± 0.2 wt%, which finally confirms that this synthesis does not involve atmospheric oxygen.

Figure 1 presents the XRD pattern of: (a) an equimolar mixture of Al2O3 and V2O5 with α-Sb2O4, (b) a mixture of 66.67 mol% AlVO4 + 33.33 mol% α-Sb2O4, and (c) a mixture of 66.67 mol% SbVO5 + 33.33 mol% Al2O3 as well as the diffractogram pattern of compound AlSbVO6 (d) obtained from these mixtures. The diffraction patterns of the finally obtained samples show only the set of diffraction lines characteristic of compounds of rutile-type structure [1922, 27, 31, 32].

Fig. 1
Fig. 1

The XRD spectra of (a) initial mixture of 33.33 mol% Al2O3 + 33.33 mol% V2O5 + 33.34 mol% α-Sb2O4; (b) initial mixture of 66.67 mol% AlVO4 + 33.33 mol% α-Sb2O4; (c) initial mixture of 66.67 mol% SbVO5 + 33.33 mol% Al2O3; (d) AlSbVO6

Citation: Journal of Thermal Analysis and Calorimetry J Therm Anal Calorim 109, 2; 10.1007/s10973-012-2234-5

The results of indexing the powder diffraction pattern of AlSbVO6 are shown in Table 2. The calculated lattice parameters are the following: a = b = 0.44945 nm, c = 0.29498 nm, V = 0.0596 nm3, Z = 2. The X-ray calculated density amounts to drtg = 4.96 g/cm3, while the experimentally measured density is equal to d = 5.21 g/cm3.

Table 2

Indexing results for powder diffraction pattern of AlSbVO6

No.Miller indices hkldexp/nmdcalc/nmI/I0/%
1110 0.31880.3178100 
2101 0.24670.246669 
3200 0.22500.247217 
4111 0.21650.216218 
5210 0.20120.20107 
6211 0.16650.166175 
7220 0.15910.158924 
8002 0.14750.147512 
9310 0.14210.142114 
10112 0.13320.133736 

The powder diffraction pattern, parameters of the elementary cell of AlSbVO6, and the identical Miller indices (hkl) calculated for AlSbVO6 are similar to their correspondents typical of the rutile phase, which implies this type of structure for the new phase AlSbVO6. The structure proposed was confirmed by the similarity of the IR spectra which are presented in many articles [19, 20, 31, 32]. IR spectra of: an equimolar mixture Al2O3/V2O5/α-Sb2O4 (curve a), a mixture containing 66.67 mol% AlVO4 and 33.33 mol% α-Sb2O4 (curve b), a mixture containing 66.67 mol% SbVO5 + 33.33 mol% Al2O3 (curve c), and also the IR spectrum of the new compound AlSbVO6 (curve d) are shown in Fig. 2.

Fig. 2
Fig. 2

IR spectra of (a) initial mixture of 33.33 mol% Al2O3 + 33.33 mol% V2O5 + 33.34 mol% α-Sb2O4; (b) initial mixture of 66.67 mol% AlVO4 + 33.33 mol% α-Sb2O4; (c) initial mixture of 66.67 mol% SbVO5 + 33.33 mol% Al2O3; (d) AlSbVO6

Citation: Journal of Thermal Analysis and Calorimetry J Therm Anal Calorim 109, 2; 10.1007/s10973-012-2234-5

As follows from Fig. 2, the IR spectrum of the new compound differs essentially from the IR spectra of the initial mixtures, both in the number of the absorption bands, in their positions and intensities. In the vibration spectrum of AlSbVO6 two absorption bands can be distinguished. The first wide absorption band lying between 900 and 500 cm−1 displays absorption maxima at 720 and 570 cm−1. This band reflects the stretching vibrations of Sb–O bonds in SbO6 octahedron and those of Al–O bonds in AlO6 octahedron [3336]. The second absorption band lying over the wave-number range of 500–300 cm−1 with its absorption maxima at 420 and 380 cm−1, has been ascribed to the bending vibrations of O–M–O (O–Al–O, O–Sb–O, O–V–O) and V–O bonds in the distorted MO6 octahedra. It cannot be excluded that the absorption bands within this wave-number range correspond to the bending vibrations of Al–O–V or vibrations of a mixed character [3339].

At the next stage of the research, our investigation aimed at establishing the thermal properties of AlSbVO6 compound. Two endothermic effects were recorded on the DTA curve of AlSbVO6 up to 1,300 °C (Fig. 3). The first of them started at 820 ± 10 °C and reached its maximum at 1,125 °C. The other effect started at about 1,200 °C. With the view to establishing the nature of the effects recorded on DTA curve of AlSbVO6, the samples containing only this compound were heated for 3 h at the following temperatures: 820, 1125, and 1200 °C, then rapidly cooled to ambient temperature and investigated by XRD method. The diffractogram of the sample additionally heated at 820 °C shows a set of diffraction lines, which according to the PDF cards (PDF cards no. 35-1485, 04-0564) belong to the sets of both VSbO4 and AlSbO4. Location of the diffraction lines and the corresponding interplanar distances characterizing VSbO4 showed that this compound is a non-stoichiometric rutile-type phase Sb0.925+V0.283+V0.644+0.16O4. XRD analysis of the sample melted at 1,125 °C demonstrated the presence of AlSbO4 besides the phases α-Sb2O4 and V2O5 crystallizing from the liquid. The mass loss of sample recorded on the TG curve of AlSbVO6 at 1,000 °C as shown in Fig. 3, testifies to the simultaneous sublimation or decomposition of α-Sb2O4. Phase composition of the sample heated additionally at 1,200 °C confirmed the literature data on thermal stability of AlSbO4, which show that this compound melts incongruently at 1,200 °C with a deposition of solid Al2O3 [40]. The DTA curve of AlSbO4 was presented in Fig. 4.

Fig. 3
Fig. 3

The DTA/TG curves of AlSbVO6

Citation: Journal of Thermal Analysis and Calorimetry J Therm Anal Calorim 109, 2; 10.1007/s10973-012-2234-5

Fig. 4
Fig. 4

The DTA curve of AlSbO4

Citation: Journal of Thermal Analysis and Calorimetry J Therm Anal Calorim 109, 2; 10.1007/s10973-012-2234-5

As follows from the above-discussed, AlSbVO6 decomposes in the solid state, at 820 °C with release of the solid VSbO4 and AlSbO4. The first effect, recorded on the DTA curve of AlSbVO6 is related to VSbO4 decomposition. According to literature data, the compound VSbO4 decomposes at 820 °C [41]. On the basis this part of the investigation, it was also found that the other effect recorded on the DTA curve of AlSbVO6, is linked to the thermal properties of the solid product of its decomposition, AlSbO4.

Conclusions

A new compound of the formula of AlSbVO6 was prepared by the conventional solid-state reactions from stoichiometric mixtures of the oxides Al2O3, V2O5, and α-Sb2O4 as well as from the reacting mixtures containing AlSbO4/V2O5, Al2O3/SbVO5, AlVO4/α-Sb2O4 or AlVO4/AlSbO4/SbVO5. The obtained compound crystallizes in the tetragonal system, in the rutile-type structure. The unit cell parameters are the following: a = b = 0.44945 nm, c = 0.29498 nm, V = 0.0596 nm3, Z = 2. AlSbVO6 in inert atmosphere is stable up to ∼820 °C, after it undergoes decomposition to VSbO4 and AlSbO4.

The author is grateful to Professor Elżbieta Filipek (West Pomeranian University of Technology) for fruitful discussions.

References

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  • 1. Roussel, H, Mehlomakulu, B, Belhadj, F E van Stehen Millet, MM 2002 Active sites characterization in mixed vanadium and iron antimonate oxide catalysts for propane ammoxidation. J Catal 205:97106 .

    • Crossref
    • Search Google Scholar
    • Export Citation
  • 2. Kuo-Tseng, L, Chin-Shyu, Y, Ni-Shen, S 1997 Mixed-metal oxide catalysts containing iron for selective oxidation of hydrogen sulfide to sulfur. Appl Catal 156:117130 .

    • Crossref
    • Search Google Scholar
    • Export Citation
  • 3. Ballarini, N, Cavani, F, Marion, P, Tonielli, N, Trifiro, F 2009 The role of V in rutile-type Sn/V/Nb/Sb mixed oxides, catalysts for propane ammoxidation to acrylonitrile. Catal Today 142:170174 .

    • Crossref
    • Search Google Scholar
    • Export Citation
  • 4. Ballarini, N, Cavani, F, Ghisletti, D, Catani, R, Cornaro, U 2003 Cr/V/Sb mixed oxide catalysts for the ammoxidation of propane to acrylonitrile. Part I. Nature of the V species. Catal Today 78:237245 .

    • Crossref
    • Search Google Scholar
    • Export Citation
  • 5. Bettahar, MM, Costentin, G, Savary, L, Lavalley, JC 1996 On the partial oxidation of propane and propylene on mixed metal oxide catalysts. Appl Catal 145:148 .

    • Crossref
    • Search Google Scholar
    • Export Citation
  • 6. Cimini, M, Millet, JMM, Ballarini, N, Cavani, F, Ciardelli, C, Ferrari, C 2004 Synthesis, characterization and evaluation as catalysts for propane ammoxidation of VMoSbO systems with rutile-type structure. Catal Today 91:259264 .

    • Crossref
    • Search Google Scholar
    • Export Citation
  • 7. Bowker, M, Bicknell, CR, Kerwin, P 1996 Ammoxidation of propane to acrylonitrile on FeSbO4. Appl Catal 136:205229 .

  • 8. Sokolovskii, VD, Davydov, AA, Ovsitser, OY 1995 Mechanism of selective paraffin ammoxidation. Catal Rev Sci Eng 37:425459 .

  • 9. Delmon, B 2007 Preparation of heterogeneous catalysts. Synthesis of highly dispersed solids and their reactivity. J Therm Anal Calorim 9:4965 .

    • Crossref
    • Search Google Scholar
    • Export Citation
  • 10. Guerrerro-Perez, MO, Al-Saeedi, JM, Guliants, VV, Banares, MA 2004 Catalytic properties of mixed Mo–V–Sb–Nb–O oxides catalysts for the ammoxidation of propane to acrylonitrile. Appl Catal 260:9399 .

    • Crossref
    • Search Google Scholar
    • Export Citation
  • 11. Sydorchuk V , Makota O, Khalameida S, Bulgakova L, Skubiszewska-Zięba J. Physical-chemical and catalytic properties of deposited MoO3 and V2O5. J Therm Anal Calorim. 2011. doi: .

    • Crossref
    • Search Google Scholar
    • Export Citation
  • 12. Nilsson, R, Lindblad, T, Andersson, A 1994 Ammoxidation o propane over antimony–vanadium-oxide catalysts. J Catal 148:501513 .

  • 13. Ballarini, N, Berry, FJ, Cavani, F, Cimini, M, Ren, X, Tamoni, D, Trifiro, F 2007 The synthesis of rutile-type V/Sb mixed oxides, catalysts for the ammoxidation of propane to acrylonitrile. Catal Today 128:161167 .

    • Crossref
    • Search Google Scholar
    • Export Citation
  • 14. Guerrerro-Perez, MO, Pena, MA, Fierro, JLG, Banares, MA 2006 A study about propane ammoxidation to acrylonitrile with an alumina-supported Sb–V–O catalyst. Ind Eng Chem Res 45:45374543 .

    • Crossref
    • Search Google Scholar
    • Export Citation
  • 15. Zanthoff, HW, Schaefer, S, Wolf, GU 1997 Ammoxidation of propane over modified V–Sb–Al-oxides—the role od acidity and redox properties of the catalysts. Appl Catal 164:105117 .

    • Crossref
    • Search Google Scholar
    • Export Citation
  • 16. Catani, R, Centi, G, Trifiro, F 1992 Kinetics and reaction network in propane ammoxidation to acrylonitrile on V–Sb_Al based mixed oxides. Ind Eng Chem Res 31:107119 .

    • Crossref
    • Search Google Scholar
    • Export Citation
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  • Impact Factor (2019): 2.731
  • Scimago Journal Rank (2019): 0.415
  • SJR Hirsch-Index (2019): 87
  • SJR Quartile Score (2019): Q3 Condensed Matter Physics
  • SJR Quartile Score (2019): Q3 Physical and Theoretical Chemistry
  • Impact Factor (2018): 2.471
  • Scimago Journal Rank (2018): 0.634
  • SJR Hirsch-Index (2018): 78
  • SJR Quartile Score (2018): Q2 Condensed Matter Physics
  • SJR Quartile Score (2018): Q2 Physical and Theoretical Chemistry

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Journal of Thermal Analysis and Calorimetry
Language English
Size A4
Year of
Foundation
1969
Volumes
per Year
4
Issues
per Year
24
Founder Akadémiai Kiadó
Founder's
Address
H-1117 Budapest, Hungary 1516 Budapest, PO Box 245.
Publisher Akadémiai Kiadó
Springer Nature Switzerland AG
Publisher's
Address
H-1117 Budapest, Hungary 1516 Budapest, PO Box 245.
CH-6330 Cham, Switzerland Gewerbestrasse 11.
Responsible
Publisher
Chief Executive Officer, Akadémiai Kiadó
ISSN 1388-6150 (Print)
ISSN 1588-2926 (Online)