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Composite material composed of nanoparticles of transition metal and magnetic ferric oxide, a methode of preparing the same, and uses of the same

Патентный поиск по классам МПК-8:

Класс B01J21/00 Катализаторы, содержащие элементы, оксиды или гидроксиды магния, бора, алюминия, углерода, кремния, титана, циркония или гафния

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Классы МПК:B01J21/00 Катализаторы, содержащие элементы, оксиды или гидроксиды магния, бора, алюминия, углерода, кремния, титана, циркония или гафния
Автор(ы): Wang, Yuan (Beijing, CN)
Zhang, Junling (Beijing, CN)
Liang, Minghui (Beijing, CN)
Wang, Xiaodong (Beijing, CN)
Wei, Yongge (Beijing, CN)
Gui, Linlin (Beijing, CN)
Патентообладатель(и): Peiking University (Beijing, CN)
Приоритеты:
подача заявки
12.10.2005
публикация патента
24.05.2011

РЕФЕРАТ (Abstract)

A composite material composed of nanoparticles of transition metal(s) and magnetic ferric oxide, a method of preparing the same, and uses of the same are provided. The composite material is substantially composed of nanoparticles of transition metal(s) or alloy thereof and nanoparticles of magnetic ferric oxide, the size of nanoparticles of transition metal(s) or alloy thereof is in the range of 0.7 to 5 nm, the size of nanoparticles of magnetic ferric oxide is in the range of 5 to 50 nm, and the amount of transition metal(s) or alloy thereof is in the range of 0.1 to 30 wt %, based on the total weight of composite material, the magnetic ferric oxide is gamma-Fe2O3, Fe3O4, complex obtained from gamma-Fe2O3 by partial reduction, or complex obtained from Fe3O4 by partial reduction. The composite material has a high reactivity and an extreme selectivity for industrial reaction of hydrogenating halogeno-nitro-aromaticics to obtain halogeno-arylamine, and has important industrial applicability because the problem such as hydrogenolysis-dehalogenation during preparing halogeno arylamine by hydrogenating halogeno-nitro-aromatics is fully resolved by using the composite materials.
Полный текст Патента US 7947191 + PDF


ФОРМУЛА ИЗОБРЕТЕНИЯ (CLAIMS)

We claim:

1. Transition metals-magnetic iron oxides nanocomposite materials consisting of a composite of transition metals or alloys thereof nanoparticles having a diameter ranging from 0.7 to 5 nm and magnetic iron oxides nanoparticles having a diameter ranging from 5 to 50 nm, the total content of the transition metals or the alloys thereof in the nanocomposite materials ranging from 0.1 to 30 wt. %, the magnetic iron oxides including γ-Fe2O3 and Fe3O4, the composite made from part reduction of the γ-Fe2O3 and part oxidation of Fe3O4.

2. The nanocomposite materials according to claim 1, wherein the composite derived from part reduction of γ-Fe2O3 is obtained by partly reducing the transition metal-γ-Fe2O3 nanocomposite at 278-473 K in the presence of a reductant selected from the group consisting of hydrogen, glycolic acid, alcohol, aldehyde and mixtures thereof.

3. The nanocomposite materials according to claim 1, wherein the composite derived from part oxidation of Fe3O4 is obtained by partly oxidizing the transition metal-Fe3O4 nanocomposite at 313-523 K in the presence of oxygen.

4. The nanocomposite materials according to claim 1, wherein the transition metals are selected from the group consisting of Pt, Ru, Rh, Os and Ir; and the transition metal alloys are composed of at least two metal elements selected from the group consisting of Pt, Pd, Ru, Rh, Os and Ir.

5. The nanocomposite materials according to claim 1, wherein the diameter of the magnetic iron oxide nanoparticles ranges from 5 to 25 nm.

6. A method for producing the nanocomposite materials of claim 1 comprising the steps of: 1) preparing a transition metal colloid by dissolving at least one soluble salt or acid containing a transition metal into an alcohol solution or alcohol/water mixture to form transition metal compound solution with a concentration of 0.01-100 g/l; mixing an alcohol solution, or aqueous solution, or alcohol/water containing an alkali metal hydroxide or alkaline-earth metal hydroxide into the transition metal compound solution; heating the obtained mixture at 343-473 K to produce a colloidal solution of transition metal nanoclusters, the colloidal solution of transition metal nanoclusters having a molar ratio of alkali metal hydroxides or alkaline-earth metal hydroxides to the salt or acid containing the transition metal from between 3 to 30; wherein the alcohols are selected from the group consisting of alcohols containing 1-8 carbon atoms and one, two, or three hydroxyl groups, and their derivatives containing one methoxyl or ethoxyl group; and the typical volume content of water in the alcohol/water mixtures is between 0-50%; 2) preparing a ferric hydroxide colloid by forming a precipitate of ferric hydroxide by adding an alkaline solution into a solution containing an Fe3+ salt and adjusting the pH value to between 4-12; peptizing the obtained precipitate in a peptizing agent to produce a colloidal solution of ferric hydroxide with a concentration of 1-300 g/l; wherein the said peptizing agents are selected from the group consisting of ferric chloride solution, ferric nitrate solution and hydrochloric acid; 3) preparing a nanocomposite material having transition metal nanoclusters and magnetic iron oxide nanoparticles by mixing the transition metal colloidal solution prepared in step 1) and the ferric hydroxide colloidal solution prepared in step 2) at a mass ratio of metal colloidal solution to ferric hydroxide colloidal solution between 1:3-1:13400; heat treating the mixture at 313-523 K between 1-200 h; and drying the mixture at 313-523 K for the purpose of providing a nanocomposite material having transition metal nanoclusters and magnetic iron oxide nanoparticles.

7. The preparation method according to claim 6, wherein the soluble salt or acid containing the transition metal in step 1) is selected from the group consisting of a salt or acid containing Pt, Pd, Ru, Rh, Os or Ir.

8. The preparation method according to claim 6, wherein the concentration of the Fe3+ salt in the solution of step 2) is between 0.01-4 mol/l; the alkali metal hydroxide or alkaline-earth metal hydroxide is selected from the group consisting of ammonia, potassium hydroxide, sodium hydroxide, lithium hydroxide, tetramethylammonium hydroxide, and butylamine; the temperature for precipitating ferric hydroxide is between 278-370 K; the concentration of peptizing agents is in the range of 0.01-2 mol/l; and the peptizing in step 2) is conducted at a temperature between 278-373 K.

9. The preparation method according to claim 6, wherein the heat treating in step 3) is selected from the group consisting of a solvothermal method, a heating and refluxing method, and a microwave irradiation method.

10. The preparation method according to claim 6, wherein the drying process is selected from the group of drying processes consisting of drying the precipitates at 313-523 K in vacuum to obtain transition metal-Fe3O4 nanocomposite materials, drying and oxidizing the precipitates in oxygen-containing atmosphere to produce transition metal-γ-Fe2O3 nanocomposite materials and drying and partly oxidizing the precipitates in oxygen-containing atmosphere to produce transition metal-magnetic iron oxides nanocomposite materials, the magnetic iron oxide being produced by partly oxidating the Fe3O4.

11. The preparation method according to claim 10, wherein the transition metal-γ-Fe2O3 nanocomposite is reduced at a temperature between 278-473 K using a reductant selected from the group consisting of hydrogen, glycolic acid, alcohol and aldehyde.

12. A method for producing the nanocomposite materials of claim 1 comprising the steps of: 1) preparing a transition metal colloids by dissolving at least one soluble salt or acid containing a transition metal into an alcohol solution or alcohol/water mixture to form a transition metal compound solution with a concentration of 0.01-100 g/l; adding mixing an alcohol solution, or aqueous solution, or alcohol/water mixture containing an alkali metal hydroxide or alkaline-earth metal hydroxide into the transition metal compound solution; wherein the molar ratio of alkali metal hydroxide or alkaline-earth metal hydroxide to the salt or acid containing the transition metal in the range of 3 to 30, the alcohols selected from the group consisting of alcohols containing 1-8 carbon atoms and one, two, or three hydroxyl groups, and their derivatives containing one methoxyl or ethoxyl group and the volume content of water in the alcohol/water mixtures is between 0-50%; heating the mixture between 373-473 K; adding an acidic aqueous solution to form a precipitate of transition metal nanoclusters dispersing the precipitate of transition metal nanoclusters into an ethylene glycol solutions containing an alkali metal hydroxide or alkaline-earth metal hydroxide, or into another organic solvent, in order to produce a colloidal solution of transition metal nanoclusters; wherein the organic solvents are selected from the group consisting of alcohols containing two or three hydroxyl groups and 1-8 carbon atoms, ketone, 1,4-dioxane, DMSO, THF and DMF; 2) preparing a ferric hydroxide colloid by forming a precipitate of ferric hydroxide by adding an alkaline solution into a solution containing Fe3+ salts to adjust the pH value to 4-12; peptizing the precipitate of ferric hydroxide in peptizing agents to produce a colloidal solution of ferric hydroxide with a concentration of 1-300 g/l the peptizing agents selected from the group consisting of ferric chloride solution, ferric nitrate solution and hydrochloric acid; and 3) preparing a nanocomposite material having transition nanoclusters and magnetic iron oxide nanoparticles; mixing the transition metal colloidal solution prepared in step 1) with the ferric hydroxide colloidal solution prepared in step 2) at a mass ratio of metal colloidal solution to ferric hydroxide colloidal solution of between 1:3-1:13400; adding an organic reductant to the mixture; heat treating the mixture with the organic reductant at a temperature between 313-523 K for 1-200 h; and drying the mixture with the organic reductant at a temperature between 313-523 K, in order to provide the nanocomposite material composed of transition metal nanoclusters and magnetic iron oxide nanoparticles; wherein the organic reductant is selected from the group consisting of formaldehyde, glycolic acid, sodium glycolate, isopropyl alcohol, glyoxal, oxalic acid and hydrogen.

13. The preparation method according to claim 12, wherein the soluble salt or acid containing the transition metal in step 1) are selected from a salt or acid containing an element selected from the group consisting of Pt, Pd, Ru, Rh, Ir and Os.

14. The preparation method according to claim 12, wherein the concentration of the Fe3+ salts in the solutions is 0.01-4 mol/l; the alkali metal hydroxide or alkaline-earth metal hydroxide is selected from the group consisting of ammonia, potassium hydroxide, sodium hydroxide, lithium hydroxide, and tetramethylammonium hydroxide; the ferric hydroxide is precipitated at a temperature between 278-370 K; the concentration of peptizing agents is in the range of 0.01-2 mol/l; and the precipitate of ferric hydroxide is peptized at a temperature between 278-373 K.

15. The preparation method according to claim 12, wherein the molar ratio of the organic reductant to ferric hydroxide in step 3) is between 0.1-10.

16. The preparation method according to claim 12, wherein the heat treating in step 3) is selected from the group consisting of a solvothermal method, a heating and refluxing method, and a microwave irradiation method.

17. The preparation method according to claim 12, wherein the drying process in step 3) conducted by a drying process selected from the group consisting of drying the precipitates at 313-523 K in vacuum to obtain a transition metal-Fe3O4 nanocomposite material, drying and oxidizing the precipitates in an oxygen-containing atmosphere to produce a transition metal-γ-Fe2O3 nanocomposite material, and drying and partly oxidizing the precipitates in an oxygen-containing atmosphere to produce a transition metal-magnetic iron oxide nanocomposite material, the magnetic iron oxide being produced by partly oxidizing Fe3O4.

18. The preparation method according to claim 17, wherein the transition metal-γ-Fe2O3 nanocomposite is reduced at a temperature between 278-473 K using a reductant selected from the group consisting of hydrogen, glycolic acid, alcohol and aldehyde.


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