RU2006119185A - CARRIER MATERIAL FOR CATALYSTS CONTAINING ZIRCONIUM DIOXIDE - Google Patents

CARRIER MATERIAL FOR CATALYSTS CONTAINING ZIRCONIUM DIOXIDE Download PDF

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RU2006119185A
RU2006119185A RU2006119185/04A RU2006119185A RU2006119185A RU 2006119185 A RU2006119185 A RU 2006119185A RU 2006119185/04 A RU2006119185/04 A RU 2006119185/04A RU 2006119185 A RU2006119185 A RU 2006119185A RU 2006119185 A RU2006119185 A RU 2006119185A
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catalyst
palladium
procatalyst
gold
carrier material
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RU2006119185/04A
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Тао ВАН (US)
Тао ВАН
Лесли Э. УЭЙД (US)
Лесли Э. УЭЙД
Виктор ВОН (US)
Виктор ВОН
Дэвид М. ЛОУ (US)
Дэвид М. ЛОУ
Альфред ХЕЙДЖМЕЙЕР (US)
Альфред ХЕЙДЖМЕЙЕР
Цзюнь ХАНЬ (US)
Цзюнь ХАНЬ
Валерий СОКОЛОВСКИЙ (US)
Валерий СОКОЛОВСКИЙ
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Селаниз Интернэшнл Корпорейшн (Us)
Селаниз Интернэшнл Корпорейшн
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    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
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    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
    • B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
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    • B01J37/16—Reducing
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00—Preparation of carboxylic acid esters
    • C07C67/04—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides onto unsaturated carbon-to-carbon bonds
    • C07C67/05—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides onto unsaturated carbon-to-carbon bonds with oxidation
    • C07C67/055—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides onto unsaturated carbon-to-carbon bonds with oxidation in the presence of platinum group metals or their compounds
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    • B01J35/397—Egg shell like
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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Claims (46)

1. Способ получения катализатора или прокатализатора, подходящих для содействия получению алкенилалканоатов, включающий введение палладий- и золотосодержащих предшественников в контакт с материалом носителя, содержащим диоксид циркония и по существу состоящим из диоксида циркония, и восстановление, по меньшей мере, палладийсодержащего предшественника в результате введения восстанавливающей среды в контакт с материалом носителя, содержащим диоксид циркония.1. A method of producing a catalyst or procatalyst suitable for facilitating the production of alkenyl alkanoates, comprising contacting palladium and gold precursors with a carrier material containing zirconia and essentially consisting of zirconia, and recovering at least the palladium-containing precursor by a reducing medium in contact with a carrier material containing zirconia. 2. Способ по п.1, где материал носителя, содержащий диоксид циркония, характеризуется площадью удельной поверхности в диапазоне от приблизительно 5 м2/г до приблизительно 300 м2/г согласно измерениям по методу БЭТ.2. The method according to claim 1, where the carrier material containing zirconium dioxide, characterized by a specific surface area in the range from about 5 m 2 / g to about 300 m 2 / g according to measurements by the BET method. 3. Способ либо по п.1, либо по п.2, где материал носителя, содержащий диоксид циркония, характеризуется размером частиц в диапазоне от 5 мкм до приблизительно 10 мм.3. The method is either according to claim 1, or according to claim 2, wherein the carrier material containing zirconia is characterized by a particle size in the range from 5 μm to about 10 mm. 4. Способ по любому из пп.1 и 2, дополнительно включающий прокаливание введенного в контакт материала носителя, содержащего диоксид циркония, в невосстанавливающей атмосфере до стадии восстановления.4. The method according to any one of claims 1 and 2, further comprising calcining the contacted carrier material containing zirconia in a non-reducing atmosphere to the reduction stage. 5. Способ по п.1, где стадия введения в контакт включает импрегнирование палладий- и золотосодержащим предшественниками материала носителя, содержащего диоксид циркония.5. The method according to claim 1, where the stage of introduction into contact includes impregnation of palladium and gold-containing precursors of the carrier material containing zirconium dioxide. 6. Способ по п.5, где стадия импрегнирования включает последовательное импрегнирование палладий- и золотосодержащими предшественниками материала носителя, содержащего диоксид циркония.6. The method of claim 5, wherein the impregnation step comprises sequentially impregnating palladium and gold-containing precursors of a carrier material containing zirconia. 7. Способ по п.4, где стадию прокаливания проводят до импрегнирования золотосодержащим предшественником.7. The method according to claim 4, where the stage of calcination is carried out before impregnation with a gold-containing precursor. 8. Способ по п.1, дополнительно включающий, по меньшей мере, одну стадию фиксации при помощи фиксирующего вещества.8. The method according to claim 1, further comprising at least one stage of fixation using a fixing substance. 9. Способ по п.1, где стадию восстановления проводят до импрегнирования золотосодержащим предшественником.9. The method according to claim 1, where the stage of recovery is carried out before impregnation with a gold-containing precursor. 10. Способ по п.5, где стадия импрегнирования включает совместное импрегнирование палладий- и золотосодержащими предшественниками.10. The method according to claim 5, where the stage of impregnation involves the joint impregnation of palladium and gold-containing precursors. 11. Способ по п.5, где стадия импрегнирования включает импрегнирование материала носителя, содержащего диоксид циркония, растворимыми в воде по существу не содержащими хлоридов растворами предшественников.11. The method according to claim 5, where the impregnation step comprises impregnating zirconia containing carrier material with water-soluble substantially chloride-free precursor solutions. 12. Способ по п.1, где по существу не содержащие хлоридов палладийсодержащие предшественники включают Pd(NH3)2(NO2)2, Pd(NH3)4(OH)2, Pd(NH3)4(NO3)2, Pd(NO3)2, Pd(NH3)4(OAc)2, Pd(NH3)2(OAc)2, Pd(OAc)2 в КОН, или NMe4OH, или NaOH, Pd(NH3)4(HCO3)2, оксалат палладия или их комбинации.12. The method according to claim 1, where the substantially chloride-free palladium-containing precursors include Pd (NH 3 ) 2 (NO 2 ) 2 , Pd (NH 3 ) 4 (OH) 2 , Pd (NH 3 ) 4 (NO 3 ) 2 , Pd (NO 3 ) 2 , Pd (NH 3 ) 4 (OAc) 2 , Pd (NH 3 ) 2 (OAc) 2 , Pd (OAc) 2 in KOH, or NMe 4 OH, or NaOH, Pd (NH 3 ) 4 (HCO 3 ) 2 , palladium oxalate or combinations thereof. 13. Способ по п.1, где по существу не содержащие хлоридов золотосодержащие предшественники включают KAuO2, NaAuO2, NMe4AuO2, Au(OAc)3 в КОН или NMe4OH, HAu(NO3)4 в азотной кислоте или их комбинации.13. The method according to claim 1, where essentially chloride-free gold-containing precursors include KAuO 2 , NaAuO 2 , NMe 4 AuO 2 , Au (OAc) 3 in KOH or NMe 4 OH, HAu (NO 3 ) 4 in nitric acid or their combinations. 14. Способ по п.5, где стадия импрегнирования включает импрегнирование материала носителя, содержащего диоксид циркония, содержащими хлориды растворами предшественников с последующей стадией фиксации, включающей фиксацию при помощи фиксирующего вещества.14. The method according to claim 5, where the impregnation step comprises impregnating zirconia-containing carrier material with chloride precursor solutions, followed by a fixing step comprising fixing with a fixing substance. 15. Способ по п.1, где стадия введения в контакт дополнительно включает введение в контакт с предшественником третьего компонента.15. The method of claim 1, wherein the step of contacting further comprises contacting a third component of the precursor. 16. Способ по п.15, где предшественник третьего компонента содержит W, Ni, Nb, Ta, Ti, Zr, Y, Re, Os, Fe, Cu, Co, Zn, In, Sn, Ce, Ge, Rh, Ga и их комбинации.16. The method according to clause 15, where the precursor of the third component contains W, Ni, Nb, Ta, Ti, Zr, Y, Re, Os, Fe, Cu, Co, Zn, In, Sn, Ce, Ge, Rh, Ga and their combinations. 17. Способ по п.15, где стадия введения в контакт включает введение в контакт третьего компонента и палладия при атомном отношении между третьим компонентом и палладием в диапазоне от приблизительно 0,01 до приблизительно 0,5.17. The method according to clause 15, where the stage of introduction into contact includes the introduction into contact of the third component and palladium at an atomic ratio between the third component and palladium in the range from about 0.01 to about 0.5. 18. Способ по п.4, где стадия прокаливания включает нагревание введенного в контакт материала носителя, содержащего диоксид циркония, при температуре в диапазоне от приблизительно 200 до приблизительно 700°С.18. The method according to claim 4, where the calcination step comprises heating the contacted carrier material containing zirconia at a temperature in the range of from about 200 to about 700 ° C. 19. Способ по п.1, дополнительно включающий введение ацетата щелочного металла в контакт с материалом носителя, содержащим диоксид циркония.19. The method according to claim 1, further comprising introducing alkali metal acetate into contact with a carrier material containing zirconia. 20. Способ по п.19, где ацетатом щелочного металла является ацетат калия.20. The method according to claim 19, where the alkali metal acetate is potassium acetate. 21. Способ по п.20, где ацетат калия присутствует в количестве в диапазоне приблизительно от 10 до 70 г на один литр катализатора.21. The method according to claim 20, where the potassium acetate is present in an amount in the range of from about 10 to 70 g per liter of catalyst. 22. Способ по п.1, где стадия введения в контакт включает введение в контакт от приблизительно 1 до приблизительно 10 г палладия и от приблизительно 0,5 до приблизительно 10 г золота на один литр катализатора, при этом количество золота находится в диапазоне от приблизительно 10 до приблизительно 125 мас.% при расчете на массу палладия.22. The method according to claim 1, where the stage of contacting comprises contacting from about 1 to about 10 g of palladium and from about 0.5 to about 10 g of gold per liter of catalyst, wherein the amount of gold is in the range of from about 10 to about 125 wt.% Based on the weight of palladium. 23. Способ по п.22, где атомное отношение между золотом и палладием находится в диапазоне от приблизительно 0,50 до приблизительно 1,00.23. The method according to item 22, where the atomic ratio between gold and palladium is in the range from about 0.50 to about 1.00. 24. Способ по п.1, где стадии способа в результате приводят к получению катализатора или прокатализатора с активной зоной на поверхности, катализатора или прокатализатора со структурой активной зоны типа "желток в яйце", катализатора или прокатализатора со структурой активной зоны типа "белок в яйце" или катализатора или прокатализатора с активной зоной по всему материалу.24. The method according to claim 1, where the stages of the method result in a catalyst or procatalyst with a core on the surface, a catalyst or procatalyst with a core structure of the yolk in egg type, a catalyst or procatalyst with a core structure of the protein in type egg "or catalyst or procatalyst with an active zone throughout the material. 25. Способ по п.24, где поверхностная оболочка характеризуется толщиной в диапазоне от приблизительно 5 до приблизительно 300 мкм.25. The method according to paragraph 24, where the surface shell is characterized by a thickness in the range from about 5 to about 300 microns. 26. Каталитическая композиция для получения алкенилалканоатов, содержащая26. A catalytic composition for producing alkenylalkanoates containing материал носителя, содержащий диоксид циркония, по существу состоящий из диоксида циркония и содержащий введенные с ним в контакт, по меньшей мере, палладий и золото с получением катализатора или прокатализатора.a carrier material comprising zirconia essentially consisting of zirconia and containing at least palladium and gold contacted with it to form a catalyst or procatalyst. 27. Композиция по п.26, где палладий и золото подвергают прокаливанию.27. The composition of claim 26, wherein the palladium and gold are calcined. 28. Композиция по любому из пп.26 и 27, где палладий и золото подвергают восстановлению.28. The composition according to any one of paragraphs.26 and 27, where palladium and gold are subjected to reduction. 29. Композиция по п.28, где перед восстановлением золото не прокаливают.29. The composition of claim 28, wherein the gold is not calcined before reduction. 30. Композиция по п.26, где золото не восстанавливают.30. The composition according to p, where the gold is not restored. 31. Композиция по п.26, где катализатор или прокатализатор содержат третий компонент.31. The composition according to p, where the catalyst or procatalyst contains a third component. 32. Композиция по п.31, где третий компонент выбирают из W, Ni, Nb, Ta, Ti, Zr, Y, Re, Os, Fe, Cu, Co, Zn, In, Sn, Ce, Ge, Rh, Ga и их комбинаций.32. The composition according to p, where the third component is selected from W, Ni, Nb, Ta, Ti, Zr, Y, Re, Os, Fe, Cu, Co, Zn, In, Sn, Ce, Ge, Rh, Ga and their combinations. 33. Композиция по п.26, где атомное отношение между третьим компонентом и палладием находится в диапазоне от приблизительно 0,01 до приблизительно 0,5.33. The composition according to p, where the atomic ratio between the third component and palladium is in the range from about 0.01 to about 0.5. 34. Композиция по п.33, где катализатор или прокатализатор содержат от приблизительно 1 до приблизительно 10 г палладия и от приблизительно 0,5 до приблизительно 10 г золота на один литр катализатора, при этом количество золота находится в диапазоне от приблизительно 10 до приблизительно 125 мас.% при расчете на массу палладия.34. The composition according to p, where the catalyst or procatalyst contains from about 1 to about 10 g of palladium and from about 0.5 to about 10 g of gold per liter of catalyst, the amount of gold is in the range from about 10 to about 125 wt.% when calculating the weight of palladium. 35. Композиция по п.26, где катализатор или прокатализатор содержат ацетат щелочного металла.35. The composition according to p, where the catalyst or procatalyst contains alkali metal acetate. 36. Композиция по п.35, где ацетатом щелочного металла является ацетат калия.36. The composition according to clause 35, where the alkali metal acetate is potassium acetate. 37. Композиция по п.36, где ацетат калия присутствует в количестве в диапазоне приблизительно от 10 до 70 г на один литр катализатора.37. The composition according to clause 36, where the potassium acetate is present in an amount in the range of from about 10 to 70 g per liter of catalyst. 38. Композиция по п.26, где катализатор или прокатализатор включает катализатор или прокатализатор с активной зоной на поверхности, катализатор или прокатализатор со структурой активной зоны типа "желток в яйце", катализатор или прокатализатор со структурой активной зоны типа "белок в яйце" или катализатор или прокатализатор с активной зоной по всему материалу.38. The composition according to p, where the catalyst or procatalyst comprises a catalyst or procatalyst with a core on the surface, a catalyst or procatalyst with a core structure of the yolk in egg type, a catalyst or procatalyst with a core structure of the protein in egg type or a catalyst or procatalyst with an active zone throughout the material. 39. Композиция по п.26, где материал носителя, содержащий диоксид циркония, включает частицы материала носителя или измельченный материал носителя.39. The composition of claim 26, wherein the carrier material comprising zirconia comprises particles of a carrier material or ground carrier material. 40. Способ получения алкенилалканоатов, включающий введение исходного сырья, содержащего алкен, алкановую кислоту и окислитель, в контакт с катализатором или прокатализатором, содержащими палладий и золото на материале носителя, содержащем диоксид циркония и по существу состоящем из диоксида циркония.40. A method for producing alkenyl alkanoates, comprising introducing a feedstock containing alkene, alkanoic acid and an oxidizing agent into contact with a catalyst or procatalyst containing palladium and gold on a carrier material containing zirconia and essentially consisting of zirconia. 41. Способ по п.40, где алкеном является этилен, алкановой кислотой является уксусная кислота, а окислителем является кислородсодержащий газ.41. The method of claim 40, wherein the alkene is ethylene, the alkanoic acid is acetic acid, and the oxidizing agent is an oxygen-containing gas. 42. Способ либо по п.40, либо по п.41, где катализатор или прокатализатор содержат третий компонент.42. The method according to claim 40, or according to paragraph 41, wherein the catalyst or procatalyst contains a third component. 43. Способ по п.40, где третий компонент выбирают из W, Ni, Nb, Ta, Ti, Zr, Y, Re, Os, Fe, Cu, Co, Zn, In, Sn, Ce, Ge, Rh, Ga и их комбинаций.43. The method of claim 40, wherein the third component is selected from W, Ni, Nb, Ta, Ti, Zr, Y, Re, Os, Fe, Cu, Co, Zn, In, Sn, Ce, Ge, Rh, Ga and their combinations. 44. Способ по п.40, где катализатор или прокатализатор содержат третий компонент и палладий при атомном отношении между третьим компонентом и палладием в диапазоне от приблизительно 0,01 до приблизительно 0,5.44. The method of claim 40, wherein the catalyst or procatalyst comprises a third component and palladium at an atomic ratio between the third component and palladium in the range of from about 0.01 to about 0.5. 45. Способ по п.40, где катализатор или прокатализатор содержат от приблизительно 1 до приблизительно 10 г палладия и от приблизительно 0,5 до приблизительно 10 г золота на один литр катализатора, при этом количество золота находится в диапазоне от приблизительно 10 до приблизительно 125 мас.% при расчете на массу палладия.45. The method according to clause 40, where the catalyst or procatalyst contains from about 1 to about 10 g of palladium and from about 0.5 to about 10 g of gold per liter of catalyst, the amount of gold is in the range from about 10 to about 125 wt.% when calculating the weight of palladium. 46. Способ по п.40, где катализатор или прокатализатор включают катализатор или прокатализатор с активной зоной на поверхности, катализатор или прокатализатор со структурой активной зоны типа "желток в яйце", катализатор или прокатализатор со структурой активной зоны типа "белок в яйце" или катализатор или прокатализатор с активной зоной по всему материалу.46. The method according to clause 40, where the catalyst or procatalyst includes a catalyst or procatalyst with a core on the surface, a catalyst or procatalyst with a core structure of the yolk in an egg, a catalyst or procatalyst with a core structure of a protein in an egg or a catalyst or procatalyst with an active zone throughout the material.
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