PL219934B1 - Phases of continuous solid solution type in four-component system of vanadium, iron, magnesium and zinc oxides, and process for the preparation of phases of continuous solid solution type in four-component system of vanadium, iron, magnesium and zinc oxides - Google Patents
Phases of continuous solid solution type in four-component system of vanadium, iron, magnesium and zinc oxides, and process for the preparation of phases of continuous solid solution type in four-component system of vanadium, iron, magnesium and zinc oxidesInfo
- Publication number
- PL219934B1 PL219934B1 PL395018A PL39501811A PL219934B1 PL 219934 B1 PL219934 B1 PL 219934B1 PL 395018 A PL395018 A PL 395018A PL 39501811 A PL39501811 A PL 39501811A PL 219934 B1 PL219934 B1 PL 219934B1
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- PL
- Poland
- Prior art keywords
- phases
- oxide
- vanadium
- iron
- solid solution
- Prior art date
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims description 18
- 239000006104 solid solution Substances 0.000 title claims description 14
- 235000014692 zinc oxide Nutrition 0.000 title claims description 10
- 235000012245 magnesium oxide Nutrition 0.000 title claims description 9
- 229910052742 iron Inorganic materials 0.000 title claims description 8
- 229910052720 vanadium Inorganic materials 0.000 title claims description 8
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims description 7
- 235000013980 iron oxide Nutrition 0.000 title claims description 7
- 229910052749 magnesium Inorganic materials 0.000 title claims description 7
- 239000011777 magnesium Substances 0.000 title claims description 7
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical class [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 title claims description 7
- 238000000034 method Methods 0.000 title claims description 4
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title 2
- 150000001875 compounds Chemical class 0.000 claims description 8
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 7
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 claims description 6
- 239000011787 zinc oxide Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 229910002056 binary alloy Inorganic materials 0.000 claims description 2
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 claims description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 2
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- 150000002736 metal compounds Chemical class 0.000 claims description 2
- -1 vanadium (V) oxide - iron (III) oxide - magnesium oxide - zinc oxide Chemical group 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims 1
- 239000011651 chromium Substances 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical group [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
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Description
Opis wynalazkuDescription of the invention
Przedmiotem wynalazku są fazy typu ciągłych roztworów stałych w czteroskładnikowym układzie tlenków wanadu, żelaza, magnezu i cynku oraz sposób wytwarzania nowych faz typu ciągłych roztworów stałych w czteroskładnikowym układzie tlenków wanadu, żelaza, magnezu i cynku. Nowe fazy mogą znaleźć zastosowanie jako składniki katalizatorów procesów otrzymywania różnych organicznych związków nienasyconych.The subject of the invention is continuous solid solution phases in the four-component system of vanadium, iron, magnesium and zinc oxides, and the method of producing new phases of the continuous solid solution type in the four-component system of vanadium, iron, magnesium and zinc oxides. The new phases can be used as catalyst components for the production of various organic unsaturated compounds.
Nowe fazy według wynalazku nie były dotychczas opisywane w literaturze przedmiotu. Z polskiego opisu patentowego nr 193145 znane są inne fazy typu ciągłych roztworów stałych zawierające żelazo, chrom i wanad o ogólnym wzorze Fe2-xCrxV4O13, gdzie 0<x<2, tworzące się w trójskładnikowym układzie tlenków metali przejściowych, w którym układ trójskładnikowy oznacza tlenek wanadu(V) - tlenek żelaza(III) - tlenek chromu(III). Fazy te można otrzymać zarówno z tlenków V2O5, Fe2O3 i Cr2O3, jak i ze związków Fe2V4O13 i Cr2V4O13.The new phases according to the invention have not been described in the literature so far. Polish patent specification No. 193145 describes other phases of the type of continuous solid solutions containing iron, chromium and vanadium with the general formula Fe2-xCrxV4O13, where 0 <x <2, formed in the ternary transition metal oxide system, in which the ternary system is vanadium oxide (V) - iron (III) oxide - chromium (III) oxide. These phases can be obtained both from the oxides of V 2 O 5 , Fe 2 O 3 and Cr 2 O 3 , and from compounds of Fe 2 V 4 O 13 and Cr 2 V 4 O 13 .
Fazy typu ciągłych roztworów stałych w czteroskładnikowym układzie tlenków metali, w którym układ czteroskładnikowy oznacza tlenek wanadu(V) - tlenek żelaza(III) - tlenek magnezu tlenek cynku, według wynalazku, posiadają wzór ogólny Zn2-xMgxFeV3O11, gdzie 0<x<2. Układ Zn2FeV3O11-Mg2FeV3O11 jest jednym z rzeczywistych układów składowych czteroskładnikowego układu tlenków V2O5-Fe2O3-MgO-ZnO, przy czym w przeliczeniu na składniki układu czteroskładnikowego tlenków zawartość tlenku wanadu(V) w procentach molowych wynosi 37,50% mol i jest stała dla całej serii tworzących się nowych faz typu ciągłych roztworów stałych oraz w przeliczeniu na składniki układu czteroskładnikowego tlenków zawartość tlenku żelaza(III) w procentach molowych wynosi 12,50% mol i jest stała dla całej serii tworzących się nowych faz typu ciągłych roztworów stałych, natomiast suma zawartości tlenku magnezu i tlenku cynku wynosi zawsze 50,00% mol. Nowe fazy tworzą się w układzie dwuskładnikowym związków Zn2FeV3O11-Mg2FeV3O11 w całym zakresie stężeń jego składników.Continuous solid solution phases in a four-component metal oxide system, in which the four-component system is vanadium (V) oxide - iron (III) oxide - magnesium oxide, zinc oxide, according to the invention, have the general formula Zn2-xMgxFeV3O11, where 0 <x <2. The Zn2FeV3O11-Mg2FeV3O11 system is one of the real constituent systems of the four-component V2O5-Fe2O3-MgO-ZnO oxide system, where the content of vanadium (V) oxide in mole percent is 37.50 mol% and is constant for the whole in a series of new phases formed in the continuous solid solution type, and in terms of the components of the four-component oxide system, the content of iron (III) oxide in mol percent amounts to 12.50 mol% and is constant for the entire series of new phases formed in the continuous solid solution type, while the sum of of magnesium oxide and zinc oxide is always 50.00 mol%. New phases are formed in the binary system of Zn2FeV3O11-Mg2FeV3O11 compounds in the entire concentration range of its components.
Sposób wytwarzania faz typu ciągłych roztworów stałych w układzie tlenków wanadu, żelaza, magnezu i cynku, według wynalazku, polegający na mieszaniu i ujednorodnianiu związków metali, charakteryzuje się tym, że miesza się związki Zn2FeV3O11 i Mg2FeV3O11. Związki Zn2FeV3O11 i Mg2FeV3O11 miesza się w stosunku molowym takim, że suma zawartości Zn2FeV3O11 i Mg2FeV3O11 w procentach molowych jest zawsze równa 100 i zależna od wartości x występuj ącego we wzorze ogólnym nowych faz Zn2-xMgxFeV3O11. Otrzymaną mieszaninę ujednorodnia się przez ucieranie, a następnie wygrzewa w temperaturach od 760 do 830°C w ciągu 60 godzin, korzystnie w trzech etapach, przy czym po każdym etapie próbki ochładza się wolno do temperatury pokojowej i rozciera, otrzymując produkt o ogólnym wzorze Zn2-xMgxFeV3O11, gdzie x mieści się w przedziale 0<x<2. Temperatura topnienia Zn2-xMgxFeV3O11 stopniowo wzrasta wraz ze wzrostem wartości x i mieści się w granicach od 865°C do 1005°C.The method of producing continuous solid solution phases in the system of vanadium, iron, magnesium and zinc oxides according to the invention, which consists in mixing and homogenizing metal compounds, is characterized by mixing Zn2FeV3O11 and Mg2FeV3O11 compounds. The compounds Zn2FeV3O11 and Mg2FeV3O11 are mixed in a molar ratio such that the sum of Zn2FeV3O11 and Mg2FeV3O11 in mol percent is always equal to 100 and depends on the x value of the new Zn2-xMgxFeV3O11 phases present in the general formula. The obtained mixture is homogenized by rubbing, and then annealing at temperatures from 760 to 830 ° C for 60 hours, preferably in three stages, after each stage the samples are slowly cooled to room temperature and rubbed to obtain a product of the general formula Zn2- xMgxFeV3O11, where x is in the range 0 <x <2. The melting point of Zn2-xMgxFeV3O11 gradually increases as the value of x increases, and ranges from 865 ° C to 1005 ° C.
Przedmiot wynalazku bliżej objaśnia poniższy przykład.The subject of the invention is illustrated in the following example.
P r z y k ł a dP r z k ł a d
Mieszaniny osobno otrzymanych związków Zn2FeV3O11 i Mg2FeV3O11, których składy, w procentach molowych, podano w tabeli 1, ujednorodnia się przez ucieranie. Otrzymane próbki ogrzewa się w atmosferze powietrza w trzech etapach: w pierwszym etapie próbki wygrzewa się w temperaturze 760°C w ciągu 20 godzin, w drugim etapie próbki wygrzewa się 20 godzin w temperaturze 830°C, w trzecim etapie próbki wygrzewa się w temperaturze 830°C w ciągu 20 godzin. Po każdym etapie próbki chłodzi się powoli do temperatury pokojowej i rozciera.Mixtures of the separately prepared Zn2FeV3O11 and Mg2FeV3O11 compounds, the compositions of which, in mole percentages, are given in Table 1, are homogenized by grinding. The obtained samples are heated in air in three stages: in the first stage, the samples are heated at 760 ° C for 20 hours, in the second stage, the samples are heated for 20 hours at 830 ° C, in the third stage, the samples are heated at 830 ° C ° C for 20 hours. After each step, the samples are slowly cooled to room temperature and triturated.
T a b e l a 1T a b e l a 1
PL 219 934 B1 cd. tabeli 1PL 219 934 B1 cont. table 1
Nowe fazy typu ciągłych roztworów stałych o wzorze ogólnym Zn2-xMgxFeV3O11, których przykładowe wzory zamieszczono w tabeli 1, są trwałe w stałym stanie skupienia w powietrzu w zakresie temperatur od 885°C do 990°C, po czym ulegają stopieniu.New phases of the continuous solid solution type of the general formula Zn2-xMgxFeV3O11, the exemplary formulas of which are presented in Table 1, are stable in a solid state in air in the temperature range from 885 ° C to 990 ° C, and then they melt.
Nowe fazy posiadają strukturę zarówno Zn2FeV3O11, jak i Mg2FeV3O11, co oznacza, że krystalizują w układzie trójskośnym. Charakterystykę rentgenowską przykładowej fazy typu Zn2-xMgxFeV3O11, gdzie x = 1, co odpowiada wzorowi ZnMgFeV3O11, przedstawiono w tabeli 2.The new phases have the structure of both Zn2FeV3O11 and Mg2FeV3O11, which means that they crystallize in a triclinic pattern. The X-ray characteristics of an exemplary phase of the Zn2-xMgxFeV3O11 type, where x = 1, which corresponds to the formula ZnMgFeV3O11, are presented in Table 2.
T a b e l a 2.T a b e l a 2.
Zastrzeżenia patentowePatent claims
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PL395018A PL219934B1 (en) | 2011-05-27 | 2011-05-27 | Phases of continuous solid solution type in four-component system of vanadium, iron, magnesium and zinc oxides, and process for the preparation of phases of continuous solid solution type in four-component system of vanadium, iron, magnesium and zinc oxides |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PL395018A PL219934B1 (en) | 2011-05-27 | 2011-05-27 | Phases of continuous solid solution type in four-component system of vanadium, iron, magnesium and zinc oxides, and process for the preparation of phases of continuous solid solution type in four-component system of vanadium, iron, magnesium and zinc oxides |
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| Publication Number | Publication Date |
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| PL395018A1 PL395018A1 (en) | 2012-12-03 |
| PL219934B1 true PL219934B1 (en) | 2015-08-31 |
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| PL395018A PL219934B1 (en) | 2011-05-27 | 2011-05-27 | Phases of continuous solid solution type in four-component system of vanadium, iron, magnesium and zinc oxides, and process for the preparation of phases of continuous solid solution type in four-component system of vanadium, iron, magnesium and zinc oxides |
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| PL395018A1 (en) | 2012-12-03 |
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