WO1993022237A1 - Procede de production d'hydrotalcite synthetique - Google Patents

Procede de production d'hydrotalcite synthetique Download PDF

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Publication number
WO1993022237A1
WO1993022237A1 PCT/US1993/003903 US9303903W WO9322237A1 WO 1993022237 A1 WO1993022237 A1 WO 1993022237A1 US 9303903 W US9303903 W US 9303903W WO 9322237 A1 WO9322237 A1 WO 9322237A1
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WIPO (PCT)
Prior art keywords
source
magnesium
alkali metal
hydrotalcite
aluminum
Prior art date
Application number
PCT/US1993/003903
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English (en)
Inventor
Barry W. Preston
John A. Kosin
Claude R. Andrews
Original Assignee
J.M. Huber Corporation
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Publication date
Application filed by J.M. Huber Corporation filed Critical J.M. Huber Corporation
Publication of WO1993022237A1 publication Critical patent/WO1993022237A1/fr

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Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00—Medicinal preparations containing inorganic active ingredients
    • A61K33/06—Aluminium, calcium or magnesium; Compounds thereof, e.g. clay
    • A61K33/08—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/78—Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen
    • C01F7/784—Layered double hydroxide, e.g. comprising nitrate, sulfate or carbonate ions as intercalating anions
    • C01F7/785—Hydrotalcite
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/20—Two-dimensional structures
    • C01P2002/22—Two-dimensional structures layered hydroxide-type, e.g. of the hydrotalcite-type
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer

Definitions

  • the present invention relates to hydrotalcite and methods of producing synthetic hydrotalcite. More particularly, the present invention relates to methods of producing highly pure synthetic hydrotalcite which has a very small platelet morphology.
  • Hydrotalcite is a naturally occurring mineral which is found in relatively small amounts in limited areas. Hydrotalcite is known to be useful as an antacid which has a neutralizing effect on gastric juices. In addition to natural hydrotalcite, synthetic hydrotalcites have been produced.
  • U.S. Patent Nos. 3,539,306 and 3,650,704 to Kimura et al disclose synthetic hydrotalcites and methods for their manufacture. The synthetic hydrotalcite of these patents is described as having the following composition:
  • U.S. Patent No. 4,629,626 to Miyata et al discloses a hydrothermally treated product useful for treating an iron deficiency, which compound has a hydrotalcite like crystal structure and includes iron, magnesium, aluminum, and water within the structure.
  • U.S. Patent No. 4,904,457 to Misra discloses a method of producing a high purity hydrotalcite by reacting activated magnesia with a Bayer liquor at approximately 95°C.
  • U.S. Patent No. 4,883,533 to Kosin et al discloses a method of producing a modified synthetic hydrotalcite from a source of magnesium, a source of aluminum and a source of carbonate.
  • Another object of the present invention is to provide a method of producing a synthetic hydrotalcite which has a purity level of 99 percent or greater, a uniform platelet morphology, and an average particle size of below 2 microns.
  • a further object of the present invention is to provide a method of producing a synthetic hydrotalcite which has a purity level of 99 percent or greater, a uniform platelet morphology, and an average particle size of less than 0.5 microns with a particle size range of approximately 0.25 to 0.75 microns.
  • the present invention provides or a method of producing synthetic hydrotalcite which involves: reacting a mixture of a magnesium source, a carbonate source, alumina trihydrate, and an alkali metal aluminate under hydrothermal conditions at a temperature of about 160° - 200°C, wherein the molar ratio of the alumina trihydrate to the alkali metal aluminate is between about 10:1 to 5:1, the molar ratio of the magnesium source to the carbonate source is between about 0.9:1 to 1.1:1, and the atomic ratio of the magnesium to total aluminum ion is between about 2.2:1 to 2.3:1
  • the present invention further provides a method of producing synthetic hydrotalcite which involves: reacting an aqueous slurry of hydromagnesite with an aluminum source under hydrothermal conditions at a temperature of about 120° - 250°C for a period of about 0.1 - 1 hour, to produce a hydrotalcite, wherein the aluminum source is selected from the group consisting of alkali metal aluminate, Bayer liquor, and a mixture of alkali metal aluminate and aluminum trihydrate, and the molar ratio of magnesium to aluminum is between about 2.0 - 2.25
  • the present invention is directed to methods of producing synthetic hydrotalcite which utilize inexpensive reactants and which produce a synthetic hydrotalcite product 99 percent pure or greater.
  • the methods of the invention produce a synthetic hydrotalcite product which has an average particle size which is less than 2 microns, and in some cases less than 0.5 microns.
  • the synthetic hydrotalcite produced by the methods of the present invention have a uniform platelet morphology.
  • the synthetic hydrotalcites which are produced by the methods of the present invention can be used in any known manner such as for fillers, reinforcing agents, or flame retardants, in a variety of polymer systems, including plastics and elastomers.
  • the present invention is particularly useful for producing synthetic hydrotalcites which are used in pharmaceutical applications such as antacids.
  • the methods of producing synthetic hydrotalcites according to the present invention involve reacting a magnesium source, a carbonate and an aluminum source.
  • two different reaction schemes are useful for producing the synthetic hydrotalcites of the present invention.
  • One reaction scheme which is hereafter referred to a the first embodiment of the present invention, involves a rapid reaction between the magnesium source, carbonate and aluminum source.
  • This embodiment produces a synthetic hydrotalcite which is 99 percent pure or greater and has an average particle size of less than 2 microns, and typically less than 1 micron.
  • the magnesium source and the carbonate are first reacted together to form an intermediate product which is then reacted with the aluminum source.
  • This embodiment produces a synthetic hydrotalcite which is 99 percent pure or greater and has an average particle size of less than 0.5 microns and a particle size range of approximately 0.25 to 0.75 microns.
  • each embodiment of the present invention provides particular advantages.
  • the first embodiment provides a simple, rapid method of producing highly pure synthetic hydrotalcite.
  • the second embodiment provides a method of producing a synthetic hydrotalcite which has an extremely small, and relatively uniform particle size.
  • synthetic crystalline hydrotalcite is produced by combining together and reacting a mixture comprising a magnesium source, a carbonate, and an aluminum source under aqueous hydrothermal conditions at a temperature of about 160° - 200° C.
  • synthetic crystalline hydrotalcite is produced by combining together and reacting a source of magnesium and a source of carbonate under atmospheric conditions. preferably at a temperature between 60° - 80°C, *o produce a hydromagnesite intermediate precipite. Thereafter, the hydromagnesite intermediate, made as above or otherwise, is reacted with a source of aluminum under hydrothermal conditions at a temperature of about 120° - 250°C for approximately 0.1 - 1.0 hour to produce synthetic hydrotalcite.
  • the magnesium source may be selected from the group consisting of magnesium oxide, magnesium hydroxide or mixtures thereof.
  • the preferred source of magnesium is magnesium hydroxide which can be provided as aqueous slurry with a solids percent of about 40 to 60%. Equivalent sources of magnesium may be used.
  • the carbonate source may be selected from alkali metal bicarbonates, alkali metal carbonates, carbon dioxide gas, carbonic acid, or mixtures thereof.
  • the aluminum source may be Bayer liquor, alkali metal aluminate or a mixture of alkali metal aluminate and solid alumina trihydrate. It is noted that while a mixture of alkali metal aluminate and solid alumina trihydrate can be used, it has been discovered that alumina trihydrate alone does not give a product having the desired fine particle size.
  • the magnesium source, carbonate, and aluminum source reactants are combined together in a closed reactor in an aqueous medium to react under hydrothermal conditions.
  • the reactant mixture is then heated at a temperature of about 160° - 200°C for about 1 to 3 hours.
  • the inventors discovered that at temperatures below about 160°C, the reaction proceeds very slowly, if at all, and that at temperatures above about 200°C, dawsonite contaminant is produced.
  • the more preferred temperature range has been determined to be 170° - 190°C, with a temperature of 175°C being the most preferred.
  • the product can be isolated by filtration and dried at an elevated temperature, e.g., 105°C according to conventional processes. It has been found that the hydrotalcite produced by this embodiment of the present invention is easy to filter and the dried product is very friable.- As discussed above, the resulting synthetic hydrotalcite has an average particle size less than about 2 microns, and typically, the resulting synthetic hydrotalcite produced by this embodiment has an average particle size of less than 1 micron.
  • the synthetic hydrotalcite product has a platelet morphology and is produced at a purity level of 99 percent or greater, with a typical purity of 100 percent.
  • the aluminum be present as a mixture of alkali metal aluminate and solid alumina trihydrate.
  • the alkali metal aluminate comprises sodium aluminate.
  • there is a proper ratio of the alkali metal aluminate and solid alumina trihydrate which produces the unique synthetic hydrotalcite of the present invention and distinguishes the method of the present invention.
  • the present inventors have discovered that the molar ratio of the alumina trihydrate to the alkali metal aluminate must be between about 10:1 to 5:1, with a ratio of 9 to 7:1 being preferred.
  • a more preferred ratio of alumina trihydrate to alkali metal aluminate has been determined to be 8:1.
  • the molar ratio of the alkali metal aluminate which is preferably sodium aluminate (Na 2 O/Al 0 3 ) , be as low as possible, i.e. have a low alkali metal content on a molar basis.
  • the molar ratio of the alkali metal aluminate increases above 1.25, the possibility of producing dawsonite, as an impurity, along with the hydrotalcite increases.
  • the molar ratio of the alkali metal aluminate was as high as 1.5, a significant amount of dawsonite contaminant was produced with the hydrotalcite.
  • the preferred alkali metal aluminate is a sodium aluminate, which is commercially available at a molar ratio of 1.25 Na 2 O/Al 2 0 3 .
  • a sodium aluminate having a molar ratio of less than 1.25 would be more preferred.
  • the carbonate reactant used in the first embodiment of the present invention is preferably present as an alkali metal bicarbonate.
  • the use of carbon dioxide and mixtures of an alkali metal bicarbonate is less preferred in this embodiment of the invention, but could be used.
  • the preferred alkali metal bicarbonate is sodium bicarbonate.
  • this ratio must be kept in the range of substantially 0.9:1 to 1.1:1. If the ratio of magnesium to bicarbonate is less than 0.9, dawsonite contaminant is produced. If this ratio is greater than 1.1, the purity of the synthetic hydrotalcite decreases.
  • the atomic ratio of magnesium to total aluminum ion from all sources is substantially 2.25:1, i.e. about 2.2:1 to about 2.3:1.
  • the hydrotalcite produced according to the first embodiment of the present invention has a high purity and a small particle size.
  • the hydrotalcite product has been determined to be suitable for use as a stabilizer and acid acceptor in polymer systems such as polypropylene, polyvinyl chloride, chlorosulfonated polyethylene, etc.
  • polymer systems such as polypropylene, polyvinyl chloride, chlorosulfonated polyethylene, etc.
  • Comparative Example No. 1 in this example a total of 1,594 grams of water, 250 grams of a Mg0H 2 in slurry (55% solids), 240 grams of sodium aluminate solution (molar ratio of 2.0Na 2 0/Al 2 0 3 ) and 204 grams of NaHC0 3 were placed in a stirred one- gallon Parr reactor. The reactor was heated to 175°C and stirred for 2 hours. The product was isolated by filtration and dried at 105°C. The resulting hydrotalcite was found to be 98% pure by x-ray diffraction analysis (XRD) . The molar ratios of the reactants were as follows:
  • the purity of the hydrotalcite produced according to the method of this example was approximately 98 percent. As this method is scaled up to commercial capacity the purity may drop as low as 95 percent due to physical mixing limitations.
  • the resulting hydrotalcite had a platelet morphology and an average particle size of 2 to 3 microns with a purity determined by x-ray diffraction of about 95 percent.
  • the product purity level approaches 100 percent.
  • the particle size of the product was always greater than 2 microns and often ranged up to 4 or 5 microns. If this process were scaled up for production purposes, the size of the particles would also increased due to mixing limitations.
  • the hydrotalcite product produced by this method had an impurity level of 100 percent (determined by x-ray diffraction) and ' platelet morphology witn // percent of the platelets falling between 0.5 and 1.5 microns by
  • the product had an average particle size of about 1 micron.
  • the molar ratio of A1(0H) 3 to sodium aluminate was 8 to 1.
  • the molar ratio of the magnesium source to the bicarbonate source was
  • hydrotalcite is very important in determining its functionality in acid acceptor/stabilizing applications.
  • hydrotalcite can be added to polyvinyl chloride formulations to function as an acid acceptor and thus enhance thermal stability.
  • Hydrotalcite is known to react with HC1 generated as the polyvinyl chloride begins to degrade to form the insoluble chloride form of hydrotalcite.
  • a trace amount (2 to 5 percent) of magnesium hydroxide contaminant reacts to form the soluble magnesium chloride. Soluble chloride can cause yellowing of the PVC and aid in early degradation.
  • a hydrotalcite containing 2 percent Mg0H 2 was added (0.5 phr) to a PVC formulation and compared with the hydrotalcite of 100 percent purity of the present invention.
  • the samples containing the hydrotalcites were oven aged at 190°C and the samples were removed and examined every 5 minutes. It was found that after approximately 40 minutes the PVC containing 98 percent purity hydrotalcite changed from a light yellow color to black signifying degradation. The PVC sample containing 100 percent purity hydrotalcite did not degrade until after approximately 60 minutes. Accordingly, it can be seen that the performance characteristics of a 98 percent pure hydrotalcite vs. a hydrotalcite which is 100 percent pure is significant.
  • crystalline hydrotalcite is produced by first combining together and reacting a source of magnesium and a source of carbonate under atmospheric conditions, preferably at a temperature between 60° - 80°C, to produce a hydromagnesite intermediate precipitant.
  • hydromagnesite intermediate is reacted with a source of aluminum under hydrothermal conditions at a temperature of about 120° - 250°C for approximately 0.1 - 1.0 hour to produce hydrotalcite.
  • the reaction of the magnesium source and the carbonate source produces a pure hydromagnesite precipitant having no extraneous salts when C0 2 is used as the carbonate source. Although the C0 2 will react with the magnesium source at any temperature between 0° -
  • a water temperature of about 25° - 95°C is preferred for most efficient use of the carbon dioxide, with a temperature of 40° - 80°C being most preferred.
  • any extraneous salts should be washed from the hydromagnesite if desired before its introduction into the next step.
  • an aluminum source is added to the reaction slurry so that the molar ratio of magnesium to aluminum is approximately between 2 to 2.25. This molar ratio is necessary in order to obtain the high purity of the final product.
  • the aluminum source may be Bayer liquor, alkali metal aluminate or a mixture of alkali metal aluminate and solid alumina trihydrate. It is noted that while a mixture of alkali metal aluminate and solid alumina trihydrate can be used, it has been discovered that alumina trihydrate alone does not give a product having the desired fine particle size.
  • the preferred aluminum source is sodium aluminate which is commercially available at a molar ratio of 1.25 Na 2 0/Al 2 O 3 .
  • This aluminum source is preferred in order to reduce the amount of excess sodium produced in the reaction. Excess sodium should be avoided if possible because it can result in unfavorable economics and can make the product more difficult to wash.
  • the hydromagnesite intermediate is placed together in a closed reactor in an aqueous medium with the aluminum component to react under hydrothermal conditions. This mixture is heated to a temperature of about 120° - 250°C under agitation for about 0.1 - 1.0 hour.
  • the reaction temperature is not critical to the formation of the final product. However, if the reaction temperature is below about 120°C, the reaction proceeds more slowly.
  • the more preferred temperature range for the reaction is about 140° - 180°C, with a temperature of 175°C being most preferred for fast reaction and high reactor throughput. A temperature of 140°C is more preferred for reduced energy demand.
  • the product is isolated by filtration and dried at an elevated temperature, e.g., 105°C.
  • the resulting hydrotalcite is easy to filter and the dried product is very friable.
  • the resulting hydrotalcite product has an average particle size less than about 1 micron, and typically has an average particle size of 0.4 microns.
  • the hydrotalcite product has a particle size which ranges from 0.25 to 0.75 micron.
  • the particles produced have a uniform platelet morphology and a purity level of 99 percent or greater, with a typical purity level of 100 percent.
  • the hydrotalcite produced by this embodiment of the present invention has a high purity level and a small particle size which makes is particularly suitable for use as a stabilizer and acid acceptor in polymer systems such as polyethylene, polyvinyl chloride, chlorosulfonated polyethylene, etc.
  • the hydrotalcite of either embodiment of the present invention may be surface treated with a conventional anionic surface active agent, such as a higher fatty acid or its alkali metal salt, to aid its dispersibility in polymer applications.
  • a conventional anionic surface active agent such as a higher fatty acid or its alkali metal salt
  • This surface treatment may be added at the beginning of the hydrothermal step, to the reacted slurry or to the final dried product.
  • a more thorough discussion of the surface treatment of hydrotalcite may be found in U.S. Patent 4,558,102 to Miyata.
  • the amount of surface treatment may vary as desired but it is preferred that the amount be sufficient to substantially coat the hydrotalcite product with at least a monolayer of treatment chemical.
  • Magnesium hydroxide slurry was added for exactly 90 minutes and a total of 468 grams was reacted in this time period. After ninety minutes, the magnesium hydroxide and C0 2 were stopped and the batch was allowed to digest 15 minutes with agitation. After digestion, the Ph had increased to approximately 8.0 and accordingly C0 2 was again injected to bring the reaction slurry back down to pH 7.0 ⁇ 0.3. The C0 2 was then stopped and 427 grams of sodium aluminate (18.9 percent Na 2 0, 24.9 percent A1 2 0 3 , Na 2 0/Al 2 0 3 molar ratio equal 1.30) was added. The reactants were mixed for ten minutes.
  • a scanning electron photomicrograph showed a hydrotalcite with a platelet morphology with platelets ranging between 0.25 - 0.75 microns in diameter. Sedigraph analysis showed the hydrotalcite to have an average particle size of 0.4 microns. A chemical analysis showed the following empirical formula 4.5MgO•A1 2 0 3 " »C0 2 •10H 2 0 .

Abstract

Procédés permettant de produire de l'hydrotalcite synthétique possédant un niveau de pureté de 99 % ou supérieur et une dimension moyenne de particules inférieure à deux microns. Selon un mode de réalisation de l'invention, on combine et on fait réagir ensemble, dans des conditions hydrothermiques, une source de magnésium, une source de carbonate et une source d'aluminium. Selon un autre mode de réalisation avec lequel le produit obtenu possède une dimension moyenne de particules inférieure à un micron, on fait réagir ensemble une source de magnésium et une source de carbonate, de façon à constituer une hydromagnésite qu'on fait ensuite réagir avec une source d'aluminium dans des conditions hydrothermiques.
PCT/US1993/003903 1992-04-30 1993-04-27 Procede de production d'hydrotalcite synthetique WO1993022237A1 (fr)

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US876,316 1992-04-30

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Cited By (29)

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WO1996023727A1 (fr) * 1995-02-03 1996-08-08 RWE-DEA Aktiengesellschaft für Mineraloel und Chemie Procede de preparation d'hydrotalcites et leurs oxydes de metal
WO1996030440A1 (fr) * 1995-03-25 1996-10-03 Henkel Kommanditgesellschaft Auf Aktien Composes cationiques a structure en couche, leur production et leur application
EP0761227A1 (fr) * 1994-06-06 1997-03-12 Yamanouchi Pharmaceutical Co. Ltd. Antiacide solide et procede de production de ce compose
EP0790872A1 (fr) * 1995-01-30 1997-08-27 Aristech Chemical Corporation Liants basiques mineraux
EP0799276A1 (fr) * 1994-12-22 1997-10-08 Reheis, Inc. Capteur d'halogene pour polymeres et copolymeres
WO1999041198A1 (fr) * 1998-02-11 1999-08-19 Akzo Nobel N.V. Procede de production d'argile anionique utilisant deux types de composes d'alumine
EP0952189A1 (fr) * 1997-07-22 1999-10-27 Kyowa Chemical Industry Co., Ltd. Agent ignifuge, resistant a la deterioration thermique, composition de resine et article moule
EP0933401A4 (fr) * 1997-07-04 2000-12-20 Kyowa Chem Ind Co Ltd Composition de resine synthetique resistant a la deterioration thermique et pieces moulees
WO2001004053A1 (fr) * 1999-07-08 2001-01-18 Mizusawa Industrial Chemicals, Ltd. Sel polybasique composite, procede de production de ce sel, et utilisation
WO2002085787A1 (fr) * 2001-04-19 2002-10-31 Süd-Chemie AG Procede de production d'hydrotalcites
US6514473B2 (en) 1995-02-03 2003-02-04 Sasol Germany Gmbh Process for producing hydrotalcites and the metal oxides thereof
JP2003524568A (ja) * 1998-02-11 2003-08-19 アクゾ ノーベル ナムローゼ フェンノートシャップ アニオン性クレー含有組成物の製造方法
WO2004050551A1 (fr) * 2002-12-02 2004-06-17 Council Of Scientific And Industrial Research Procede de preparation et d'assemblage automatique d'oxy/hydroxydes ternaires et binaires a taille nanometrique
WO2004056705A1 (fr) * 2002-12-23 2004-07-08 Council Of Scientific And Industrial Research Procede de preparation de couches chargees positivement de type hydrotalcite et brucite
US6803401B2 (en) 1997-10-24 2004-10-12 Reheis, Inc. Halogen scavenger for olefin formulations
US6815389B2 (en) 1998-02-11 2004-11-09 Akzo Nobel Nv Process for producing anionic clay using two types of alumina compounds
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US8227046B2 (en) 2002-11-29 2012-07-24 Council Of Scientific And Industrial Research Process for preparing self-assembling nanobinary and ternary oxy/hydroxides
US9133041B2 (en) 2006-04-06 2015-09-15 Commonwealth Scientific And Industrial Research Organisation Remediation of groundwater
US9242869B2 (en) 1997-09-19 2016-01-26 Opko Ireland Global Holdings, Ltd. Metal compounds mixed or sulphated, as phosphate binders
US9566302B2 (en) 2010-02-04 2017-02-14 Opko Ireland Global Holdings, Ltd. Composition comprising mixed metal compounds and xanthan gum
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CN113461037A (zh) * 2021-07-12 2021-10-01 安徽大学绿色产业创新研究院 一种镁铝水滑石制备方法
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Cited By (55)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0761227A1 (fr) * 1994-06-06 1997-03-12 Yamanouchi Pharmaceutical Co. Ltd. Antiacide solide et procede de production de ce compose
EP0761227A4 (fr) * 1994-06-06 1998-06-10 Yamanouchi Pharma Co Ltd Antiacide solide et procede de production de ce compose
EP0799276A1 (fr) * 1994-12-22 1997-10-08 Reheis, Inc. Capteur d'halogene pour polymeres et copolymeres
EP0799276A4 (fr) * 1994-12-22 1998-03-25 Reheis Inc Capteur d'halogene pour polymeres et copolymeres
EP0790872A1 (fr) * 1995-01-30 1997-08-27 Aristech Chemical Corporation Liants basiques mineraux
EP0790872A4 (fr) * 1995-01-30 1998-11-18 Aristech Chemical Corp Liants basiques mineraux
US6180764B1 (en) 1995-02-03 2001-01-30 Rwe-Dea Aktiengesellschaft Fur Mineraloel Und Chemie Process for producing hydrotalcites by hydrolyzing metal alcoholates
US6517795B1 (en) 1995-02-03 2003-02-11 Sasol Germany Gmbh Process for producing hydrotalcites and the metal oxides thereof
US6514473B2 (en) 1995-02-03 2003-02-04 Sasol Germany Gmbh Process for producing hydrotalcites and the metal oxides thereof
WO1996023727A1 (fr) * 1995-02-03 1996-08-08 RWE-DEA Aktiengesellschaft für Mineraloel und Chemie Procede de preparation d'hydrotalcites et leurs oxydes de metal
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