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Novel hydrotalcites, syntheses, and uses

a hydrotalcite and synthetic technology, applied in the field of catalysts, can solve the problems of limited success of butyric acid, water-insoluble acid, and acid that is a csub>4 /sub>acid

Inactive Publication Date: 2005-01-27
FUJII MASAKI +6
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the method of the Schutz '329 patent works rather well for most water-soluble carboxylic acids such as C1 to C4 carboxylic acids, it does not work well for those acids, which are water-insoluble.
In fact, butyric acid, which is a C4 acid, has only limited success in the method of the Schutz '329 patent.

Method used

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  • Novel hydrotalcites, syntheses, and uses
  • Novel hydrotalcites, syntheses, and uses
  • Novel hydrotalcites, syntheses, and uses

Examples

Experimental program
Comparison scheme
Effect test

example 1

Step I Carried Out in Water Medium

CATAPAL® alumina (0.26 moles) was suspended in 500 ml deionized water in a 4-liter beaker and stearic acid (0.23 moles) was added to the stirred suspension. The beaker was fitted with a crystallizing dish filled with ice water to condense volatiles in the beaker as it was heated to 75°-85° C. and the temperature was maintained for 4 to 8 hours. At the end of this period, magnesium oxide (0.44 moles) was added, followed by 1.5 liters of deionized water. The mixture was heated to 90°-95° C. and the temperature was maintained for 4 to 8 hours. The mixture was cooled to room temperature overnight with stirring. The resulting material can preferably be dried in one of two ways:

a) in an air oven at 130° C. until a semi-dry solid is obtained, which is further dried in a vacuum oven at 80° C. overnight; or

b) by spray-drying at approximately 200° C. inlet temperature and about 100° C. outlet temperature.

The powder obtained after drying the material i...

example 2

Step I Carried Out in Organic Solvent(s)

The reaction of the trivalent cation source and carboxylic acids that are water immiscible, such as stearic acid, can preferably be carried out in an organic solvent, such as refluxing hexane. CATAPAL® alumina (0.26 moles) was suspended in 200 ml hexane in a 4-liter beaker and the acid (0.23 moles) was added to the stirred suspension. The beaker was fitted with a crystallizing dish filled with ice water to condense volatiles in the beaker as it was heated to about 65° C. and the temperature was maintained for 4 to 8 hours. The solvent may preferably be removed by evaporation or filtration. Water was added to the resulting residue. Magnesium oxide (0.44 moles) was then added with vigorous stirring. The mixture was heated to about 90°-95° C. and the temperature was maintained for 4 to 8 hours. Product isolation, i.e., drying, was carried out as described in Example 1 above. Using this approach, a homogenous synthetic hydrotalcite was obtained ...

example 3

Step I Carried Out in an Acid Melt

A beaker containing the required amount of solid stearic acid was heated on an oil bath until the acid melted. The desired stoichiometric amount of alumina was added in small portions to the melt with stirring. The temperature was maintained for about two or more hours. Water was added to the product, and the mixture was stirred to an even consistency. Magnesium oxide was added, followed by 1.5 liters of deionized water. The mixture was heated to 90°-95° C. and the temperature was maintained for 4 to 8 hours. The mixture was allowed to cool to room temperature overnight with stirring. Product isolation was carried out as in Example 1 above.

A difficulty encountered with this approach was similar to that observed in Example 1, i.e., the product was greasy. However, an advantage of using the acid melt approach is that the reaction rate in an acid melt is much faster than that observed in water. With adequate mixing in the acid melt, a more complete...

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Abstract

Synthetic hydrotalcites of the general formula: [M2+1-xM3+x(OH)2]x+[An−x / n·mH2O]x−where M2+ is a divalent cation, M3+ is a trivalent cation and An− is an organic anion selected from straight chain carboxylates of C16-C18 acids, carboxylates of aromatic acids, carboxylates of acrylic acid, unsaturated carboxylates of methacrylic acid and unsaturated carboxylates of vinylacetic acid are disclosed, along with methods of synthesis and uses.

Description

FIELD OF THE INVENTION This invention relates in general to catalysts and, more specifically, to novel synthetic hydrotalcites, their syntheses and uses. The synthetic hydrotalcites of the present invention are made from organic anions longer than C4, and also from organic anions with functional groups including saturated carboxylates of C6, C8, C10, and C18, straight chain acids; aromatics such as benzoates, chlorobenzoates, naphthoates, and p-hydroxybenzoates; carboxylates of acrylic, methacrylic and vinylacetic acids; and mixtures of these organic anions. BACKGROUND OF THE INVENTION Hydrotalcites are derivatives of brucite, a naturally-occurring, layered, magnesium hydroxide mineral. Synthetic hydrotalcites can be made by substituting a trivalent metal cation, such as aluminum, for some of the magnesium cations normally present in a layer. The magnesium cations can also be substituted by other divalent cations. This substitution will result in a net positive charge residing on ...

Claims

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Application Information

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IPC IPC(8): C01F7/785C08J3/20C07F5/06C08K3/10C08K5/00C08K5/04C08K5/098C08K9/04C08L101/00C09C1/02C09C1/22C09C1/34C12S11/00
CPCC01F7/005C01P2002/22C01P2002/72C01P2002/78C01P2004/03C01P2004/04C08K5/0091C01P2004/30C01P2004/61C07F5/069C08L23/02C01F7/785
Inventor FUJII, MASAKIGALLAHER, GEORGE R. JR.KIM, SEHYUNMONACO, STEVEN J.TOWNSEND, EDWIN B. IVBRIMA, THOMAS S.HAWK, GWENDOLYN
Owner FUJII MASAKI
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