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Methods of making alkenyl alkanoates

a technology of alkenyl alkanoate and catalyst, which is applied in the field of catalysts, methods of making catalysts, and methods of making alkenyl alkanoates, can solve the problems of little investigation of differences between support materials, and achieve the effect of improving va production and lowering costs

Inactive Publication Date: 2005-08-18
CELANESE INT CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

[0021] The present invention addresses at least four different aspects relating to catalyst structure, methods of making those catalysts and methods of using those catalysts for making alkenyl alkanoates. Separately or together in combination, the various aspects of the invention are directed at improving the production of alkenyl alkanoates and VA in particular, including reduction of by-products and improved production efficiency. A first aspect of the present invention pertains to a unique palladium / gold catalyst or pre-catalyst (optionally calcined) that includes rhodium or another metal. A second aspect pertains to a palladium / gold catalyst or pre-catalyst that is based on a layered support material where one layer of the support material is substantially free of catalytic components. A third aspect pertains to a palladium / gold catalyst or pre-catalyst on a zirconia containing support material. A fourth aspect pertains to a palladium / gold catalyst or pre-catalyst that is produced from substantially chloride free catalytic components.

Problems solved by technology

But very little investigation of the differences between the support materials has been done.

Method used

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  • Methods of making alkenyl alkanoates

Examples

Experimental program
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Effect test

example 1

[0107] A support material containing palladium and rhodium metal was prepared as follows: The support material in an amount of 250 ml consisting of Sud Chemie KA-160 silica spheres having a nominal diameter of 7 mm., a density of about 0.569 g / ml, in absorptivity of about 0.568 g H2O / g support, a surface area of about 160 to 175 m2 / g, and a pore volume of about 0.68 ml / g., was first impregnated by incipient wetness with 82.5 ml of an aqueous solution of sodium tetrachloropalladium (II) (Na2PdCl4) and rhodium chloride trihydrite (RhCl3.3H2O) sufficient to provide about 7 grams of elemental palladium and about 0.29 grams of elemental rhodium per liter of catalyst. The support was shaken in the solution for 5 minutes to ensure complete absorption of the solution. The palladium and rhodium were then fixed to the support as palladium (II) and rhodium (III) hydroxides by contacting the treated support by roto-immersion for 2.5 hours at approximately 5 rpm with 283 ml of an aqueous sodium ...

example 2

[0108] A support material utilizing palladium and rhodium hydroxides was prepared as described in Example 1. The palladium and rhodium containing support was then calcined at 400° C. for 2 hours under air and then allowed to naturally cool to room temperature. The calcined support material containing palladium and rhodium hydroxides was then impregnated with an aqueous solution (81 ml) containing 1.24 g Au from NaAuCl4 and 2.71 g 50% NaOH solution (1.8 equivalents with respect to Au) using the incipient wetness method. The NaOH treated pills were allowed to stand overnight to ensure precipitation of the Au salt to the insoluble hydroxide. The pills were thoroughly washed with deionized water (˜5 hours) to remove chloride ions and subsequently dried at 100° C. in a fluid bed drier for 1.2 hours. The palladium, rhodium, and gold were then reduced by contacting the support with C2H4 (1% in nitrogen) in the vapor phase at 150° C. for 5 hours. Finally the catalyst was impregnated by inci...

example 3

[0109] A support material containing palladium and rhodium hydroxides was prepared as described in Example 1. The palladium and rhodium containing support was then calcined at 400° C. for 2 hours under air and then allowed to naturally cool to room temperature. The calcined support material containing palladium and rhodium hydroxides was then reduced by contacting the support with C2H4 (1% in nitrogen) in the vapor phase at 150° C. for 5 hours. The support containing palladium and rhodium metal was subsequently impregnated with an aqueous solution (81 ml) containing 1.24 g Au from NaAuCl4 and 2.71 g 50% NaOH solution (1.8 equivalents with respect to Au) using the incipient wetness method. The NaOH treated pills were allowed to stand overnight to ensure precipitation of the Au salt to the insoluble hydroxide. The pills were thoroughly washed with deionized water (˜5 hours) to remove chloride ions and subsequently dried at 100° C. in a fluid bed drier for 1.2 hours. The palladium, rho...

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Abstract

The present invention addresses at least four different aspects relating to catalyst structure, methods of making those catalysts and methods of using those catalysts for making alkenyl alkanoates. Separately or together in combination, the various aspects of the invention are directed at improving the production of alkenyl alkanoates and VA in particular, including reduction of by-products and improved production efficiency. A first aspect of the present invention pertains to a unique palladium / gold catalyst or pre-catalyst (optionally calcined) that includes rhodium or another metal. A second aspect pertains to a palladium / gold catalyst or pre-catalyst that is based on a layered support material where one layer of the support material is substantially free of catalytic components. A third aspect pertains to a palladium / gold catalyst or pre-catalyst on a zirconia containing support material. A fourth aspect pertains to a palladium / gold catalyst or pre-catalyst that is produced from substantially chloride free catalytic components.

Description

CLAIM OF PRIORITY [0001] The present application claims the benefit of U.S. provisional application 60 / 531,415; 60 / 530,936; 60 / 531,486; and 60 / 530,937, all filed on Dec. 19, 2003 and claims the benefit of international applications PCT / U.S.2004 / ______ (Atty. No 1197.001WO); PCT / U.S. 2004 / ______ (Atty. No 1197.002WO); PCT / U.S.2004 / ______ (Atty. No 1197.003WO); and PCT / U.S.2004 / ______ (Atty. No 11197.004WO), all filed on Nov. 19, 2004, all of which are hereby incorporated by reference.FIELD OF THE INVENTION [0002] The present invention relates to catalysts, methods of making the catalysts, and methods of making alkenyl alkanoates. More particularly, the invention relates to methods of making vinyl acetate. BACKGROUND OF THE INVENTION [0003] Certain alkenyl alkanoates, such as vinyl acetate (VA), are commodity chemicals in high demand in their monomer form. For example, VA is used to make polyvinyl acetate (PVAc), which is used commonly for adhesives, and accounts for a large portion o...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): B01J23/66
CPCB01J23/464B01J23/52B01J23/58B01J33/00B01J35/002B01J35/008B01J35/0086C07C67/055B01J35/026B01J37/0201B01J37/0244B01J37/16C07C69/15B01J35/31B01J35/397B01J35/398B01J35/50B01J35/30B01J35/613B01J35/635B01J35/615
Inventor WANG, TAOWADE, LESNICOLAU, IOANKIMMICH, BARBARAWONG, VICTORLIU, YUMINHAN, JUNSOKOLOVSKII, VALERYHAGEMEYER, ALFREDLOWE, DAVID M.
Owner CELANESE INT CORP
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