DE3346943A1 - Preparation of hydrotalcite with improved properties - Google Patents
Preparation of hydrotalcite with improved propertiesInfo
- Publication number
- DE3346943A1 DE3346943A1 DE19833346943 DE3346943A DE3346943A1 DE 3346943 A1 DE3346943 A1 DE 3346943A1 DE 19833346943 DE19833346943 DE 19833346943 DE 3346943 A DE3346943 A DE 3346943A DE 3346943 A1 DE3346943 A1 DE 3346943A1
- Authority
- DE
- Germany
- Prior art keywords
- hydrotalcite
- sodium carbonate
- magnesium oxide
- aluminum
- magnesium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 title claims abstract description 18
- 229910001701 hydrotalcite Inorganic materials 0.000 title claims abstract description 17
- 229960001545 hydrotalcite Drugs 0.000 title claims abstract description 17
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 19
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 15
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 15
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 13
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 8
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 4
- 239000000376 reactant Substances 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000000347 magnesium hydroxide Substances 0.000 claims description 5
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 4
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 2
- 230000000694 effects Effects 0.000 abstract description 8
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical class [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 abstract description 4
- 229940069428 antacid Drugs 0.000 abstract description 4
- 239000003159 antacid agent Substances 0.000 abstract description 4
- 230000001458 anti-acid effect Effects 0.000 abstract description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 2
- 239000011707 mineral Substances 0.000 abstract description 2
- 230000002035 prolonged effect Effects 0.000 abstract description 2
- 239000000725 suspension Substances 0.000 abstract description 2
- 159000000013 aluminium salts Chemical class 0.000 abstract 1
- 229910000329 aluminium sulfate Inorganic materials 0.000 abstract 1
- 239000001164 aluminium sulphate Substances 0.000 abstract 1
- 235000011128 aluminium sulphate Nutrition 0.000 abstract 1
- BUACSMWVFUNQET-UHFFFAOYSA-H dialuminum;trisulfate;hydrate Chemical compound O.[Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O BUACSMWVFUNQET-UHFFFAOYSA-H 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 11
- 229960000869 magnesium oxide Drugs 0.000 description 9
- 235000012245 magnesium oxide Nutrition 0.000 description 9
- 239000000047 product Substances 0.000 description 7
- 239000002253 acid Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000002002 slurry Substances 0.000 description 6
- MPRVXUYAJZZBHG-UHFFFAOYSA-K dicarbonoperoxoyloxyalumanyl hydroxy carbonate Chemical compound [Al+3].OOC([O-])=O.OOC([O-])=O.OOC([O-])=O MPRVXUYAJZZBHG-UHFFFAOYSA-K 0.000 description 4
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 2
- JGDITNMASUZKPW-UHFFFAOYSA-K aluminium trichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Al](Cl)Cl JGDITNMASUZKPW-UHFFFAOYSA-K 0.000 description 2
- 229940063656 aluminum chloride Drugs 0.000 description 2
- 229940009861 aluminum chloride hexahydrate Drugs 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 229940091250 magnesium supplement Drugs 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 235000012501 ammonium carbonate Nutrition 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 229940082150 encore Drugs 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/16—Preparation of alkaline-earth metal aluminates or magnesium aluminates; Aluminium oxide or hydroxide therefrom
-
- 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
- A61K33/10—Carbonates; Bicarbonates
-
- 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, with or without oxygen or hydrogen, and containing two or more other elements
- C01F7/784—Layered double hydroxide, e.g. comprising nitrate, sulfate or carbonate ions as intercalating anions
- C01F7/785—Hydrotalcite
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Geology (AREA)
- Medicinal Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
Description
Herstellung von Hydrotalcit mit verbesserten Eigenschaf-Production of hydrotalcite with improved properties
ten Die Erfindung betrifft ein neues Verfahren zur Synthese von Hydrotalcit als leichtfiltrierbarer, kristalliner Substanz.The invention relates to a new process for the synthesis of hydrotalcite as an easily filterable, crystalline substance.
Hydrotalcit ist ein bekanntes Mineral, das z.B. in Norwegen, in der UdSSR und in Österreich gefunden wird.Hydrotalcite is a well-known mineral found e.g. in Norway, in the USSR and is found in Austria.
Hydrotalcit kann auch folgendermaßen synthetisiert werden: In einem Verfahren wird Ammoniumcarbonat oder Trockeneis einer Mischung von Magnesiumoxid und g -Aluminiumoxid (oder dem thermischen Zersetzungsprodukt aus Magnesium-und Aluminiumnitrat) zugesetzt und auf 325"C bei erhöhtem Drücken von 2.000-20.000 Pfund je Quadratzoll (p.s.i) erhitzt (Roy et al, Am. J. Sciene 251, 350 (1953)).Hydrotalcite can also be synthesized in the following ways: In one Method uses ammonium carbonate or dry ice a mixture of magnesium oxide and g -aluminium oxide (or the thermal decomposition product of magnesium and Aluminum nitrate) was added and raised to 325 "C at elevated pressures of 2,000-20,000 pounds heated per square inch (p.s.i) (Roy et al, Am. J. Sciene 251, 350 (1953)).
Hydrotalcit kann auch synthetisch durch Umsetzung eines wasserlöslichen Aluminiumsalzes und eines wasserlöslichen Magnesiumsalzes mit Natriumcarbonat und Natriumhydroxid hergestellt werden (DE 1 592 126).Hydrotalcite can also be produced synthetically by converting a water-soluble one Aluminum salt and a water-soluble magnesium salt with sodium carbonate and Sodium hydroxide are produced (DE 1 592 126).
Hydrotalcit bildet sich auch bei der Alterung von Aluminiumhydroxycarbonatgel und Magnesiumhydroxidgelmischungen während eines Zeitraumes von bis zu 500 Tagen bei 250C (Vanderlaan et al., G.- Pharm. Science 71, 780 (1982)).Hydrotalcite also forms when aluminum hydroxycarbonate gel ages and magnesium hydroxide gel mixtures for a period of up to 500 days at 250C (Vanderlaan et al., G. Pharm. Science 71, 780 (1982)).
Die genannten Verfahren haben jedoch Nachteile: Das erstzitierte Verfahren muß bei hoher Temperatur und hohem Druck durchgeführt werden und stellt sicherlich ein für die großtechnische Herstellung undurchführbares Verfahren dar.However, the procedures mentioned have disadvantages: The procedure cited first must be done at high temperature and high pressure and certainly poses is an impracticable process for large-scale production.
Das zweitgenannte Verfahren weist auch Nachteile auf: Das Produkt wird als Gel erhalten, das sehr leicht Basen absorbiert und sich sehr schwer filtrieren läßt. Das Waschen dieses Produktes ist sehr mühsam. Deshalb sind spezielle Isolier- und Trocknungsverfahren unentbehrlich.The latter method also has disadvantages: The product is obtained as a gel that absorbs bases very easily and is very difficult to filter leaves. Washing this product is very troublesome. Therefore, special insulating and drying process indispensable.
Das dritte Verfahren hat den deutlichen Nachteil, daß es sehr zeitraubend und damit auch für die technische Herstellung undurchführbar ist.The third method has the distinct disadvantage that it is very time consuming and is therefore impracticable for technical production.
Gegenstand der vorliegenden Erfindung ist daher ein Verfahren zur Herstellung von Hydrotalcit der Formel Al203.The present invention is therefore a method for Production of hydrotalcite of the formula Al203.
6MgO.COz.12H20, bei dem man Magnesiumoxid oder Magnesiumhydroxid mit einer AluminiuKchlorid- oder Aluminiumsulfatlösung in Gegenwart von Natriumcarbonat in wäßriger Lösung umsetzt.6MgO.COz.12H20, in which one uses magnesium oxide or magnesium hydroxide with an aluminum chloride or aluminum sulfate solution in the presence of sodium carbonate converts in aqueous solution.
Vorzugsweise erfolgt das Verfahren bei erhöhter Temperatur, besonders bevorzugt bei Temperaturen zwischen ca.The process is preferably carried out at an elevated temperature, especially preferably at temperatures between approx.
70 und ca. 100 DC, ganz besonders bevorzugt zwischen 80"C und 900C.70 and approx. 100 DC, very particularly preferably between 80 ° C and 900 ° C.
Erfindungsgemäß kann die Alterungszeit von bis zu 50 Tagen bei der Umsetzung von Aluminiumhydroxycarbonatgel mit Magnesiumoxid oder Magnesiumhydroxidmischungen auf einige Stunden verringert werden, indem diese Umsetzung bei erhöhten Temperaturen, vorzugsweise bei Temperaturen um ca.According to the invention, the aging time of up to 50 days at the Conversion of aluminum hydroxycarbonate gel with magnesium oxide or magnesium hydroxide mixtures be reduced to a few hours by this reaction at elevated temperatures, preferably at temperatures around approx.
850C durchgeführt wird. Mittels Röntgendifraktionsanalyse kann man verfolgen, wie das Magnesium oder Magnesiumhydroxid bzw. -oxid verschwindt und der Hydrotalcit sich bildet. Nach einer Reaktionszeit von zwei Stunden bei 850C enthält der Hydrotalcit noch etwas Magnesiumoxid, aber nach einem Zeitraum von 4 Stunden ist das Magnesiumoxid vollkommen verschwunden und das Reaktionsprodukt ist reiner Hydrotalcit. Der erhaltene Hydrotalcit ist leicht filtrierbar und läßt sich auch leicht mit Wasser waschen. Gelartige Produkt, die sich nur mühsam isolieren, waschen und trocknen lassen werden nicht erhalten.850C is carried out. By means of X-ray diffraction analysis one can track how the magnesium or magnesium hydroxide or oxide disappears and the Hydrotalcite forms. Contains after a reaction time of two hours at 850C the hydrotalcite still some magnesium oxide, but after a period of 4 hours the magnesium oxide has completely disappeared and the reaction product is purer Hydrotalcite. The hydrotalcite obtained is easily filterable and can also be wash easily with water. Wash gel-like products that are difficult to isolate and let dry are not preserved.
Das Aluminiumhydroxycarbonatgel kann, wie beschrieben, dadurch hergestellt werden, daß eine Aluminiumchlorid-oder -sulfatlösung einer Natriumcarbonat/Natriumhydrogencarbonatlösung zugesetzt wird. Es ist jedoch einfacher, dieses Gel dadurch herzustellen, daß eine Aluminiumsulfat oder -chloridlösung einer Natriumcarbonat-Magnesiumoxidaufschlämmung zugesetzt wird. Das Molverhältnis zwischen dem Aluminium und dem Magnesium sollte bevorzugt ca. 1:3 betragen. Die Temperatur sollte bei ca. 850C gehalten werden. Eine Reaktionszeit von vier Stunden genügt für eine vollständige Reaktion.The aluminum hydroxycarbonate gel can be prepared as described thereby be that an aluminum chloride or sulfate solution of a sodium carbonate / sodium hydrogen carbonate solution is added. However, it is easier to make this gel by having a Aluminum sulfate or chloride solution of a sodium carbonate-magnesia slurry is added. The molar ratio between the aluminum and the magnesium should be preferably about 1: 3. The temperature should be kept at around 850C. A reaction time of four hours is sufficient for a complete reaction.
Die Eigenschaften des erhaltenen Hydrotalcits hängen von der Konzentration der eingesetzten Reaktionspartner ab Ein Hydrotalcit mit einer optimalen säurebindenden und antaziden Wirkung wird dann erhalten, wenn folgende Konzentrationen eingesetzt werden: Aluminiumsalz 0,2 Mol/ 1000 ml, Magnesiumoxid 0,6 Mol/1000 ml und Natriumcarbonat 0,85 Mol/1000 ml.The properties of the hydrotalcite obtained depend on the concentration the reactants used from A hydrotalcite with an optimal acid-binding and antacid effect is obtained when the following concentrations are used aluminum salt 0.2 mol / 1000 ml, magnesium oxide 0.6 mol / 1000 ml and sodium carbonate 0.85 moles / 1000 ml.
Die säurebindende Wirkung des hergestellten Hydrotalcits wurde durch eine Bestimmung der zur Neutralisierung von 1 g Produkt erforderlichen Menge (in ml) an 0,1-n-Chlorwasserstoffsäure geprüft.The acid-binding effect of the hydrotalcite produced was through a determination of the amount required to neutralize 1 g of product (in ml) on 0.1 N hydrochloric acid.
Die antazide Wirkung dient als Hinweis auf eine verlängerte Wirksamkeit. Sie wird dadurch bestimmt, indem 150 ml 0,1 n-Chlorwasserstoffsäure mit 1 g der zubereiteten Substanz bei 37° versetzt wird und die Suspension 80 Minuten lang gerührt wird. Der pH-Wert wurde in 10-minütigen Abständen gemessen und 20.0 ml 0,1 n-Chlorwasserstoffsäure worden zugegeben.The antacid effect serves as an indication of a prolonged effectiveness. It is determined by mixing 150 ml of 0.1 N hydrochloric acid with 1 g of the prepared substance is added at 37 ° and the suspension is stirred for 80 minutes will. The pH was measured every 10 minutes and 20.0 ml of 0.1 N hydrochloric acid been admitted.
Nach den angegebenen Maßnahmen hergestellte Proben hatten eine säurebindende Wirkung von wenigsten 270 ml 0,1 n-Chlorwasserstoffsäure und zeigten bei der Prüfung der antaziden Wirkung nach 70 Min., einen pH-Wert von >3,0 Folgende Beispiele erläutern die Erfindung: Beispiel 1 Zu 250 ml destilliertem Wasser wurden 45,1 g wasserfreies Natriumcarbonat und 13,6 g 90 %iges Magnesiumoxid (leicht) zugegeben. Nach 10-minütigem Rühren wurde die Aufschlämmung auf 85"C erhitzt. 33,3 g Aluminiumsulfatoctadecahydrat, gelöst in 250 ml dest. Wasser, wurden innerhalb einer Stunde eingetropft. Die Mischung wurde noch vier Stunden erhitzt. Die Aufschlämmung wurde dann auf Raumtemperatur abgekühlt. Der weiße Niederschlag wurde abfiltriert (Büchnertrichter) und mit 100 ml dest.Samples produced according to the specified measures were acid-binding Effect of at least 270 ml of 0.1 N hydrochloric acid and showed when tested the antacid effect after 70 minutes, a pH value of> 3.0 The following examples explain the invention: Example 1 To 250 ml of distilled water 45.1 g of anhydrous sodium carbonate and 13.6 g of 90% magnesium oxide (light) admitted. After stirring for 10 minutes, the slurry was heated to 85 "C. 33.3 g aluminum sulfatoctadecahydrate, dissolved in 250 ml dist. Water, were inside dropped in for an hour. The mixture was heated for a further four hours. The slurry was then cooled to room temperature. The white precipitate was filtered off (Büchner funnel) and with 100 ml dist.
Wasser gewaschen. Das Produkt wurde aus dem Büchnertrichter entfernt und zu 200 ml dest. Wasser zugegeben.Water washed. The product was removed from the Buchner funnel and to 200 ml dist. Water added.
Nach 30-minütigem Rühren wurde es nochmals durch Filtration isoliert, mit weiteren 100 ml Wasser gewaschen, vollständig trocken gesaugt und 15 Stunden bei 700C getrocknet.After stirring for 30 minutes, it was isolated again by filtration, washed with another 100 ml of water, sucked completely dry and 15 hours dried at 700C.
Säurebindende Wirkung: 290 ml n/10 HCl Beispiel 2 Zu der 45,1 g wasserfreies Natriumcarbonat enthaltenden Lösung wurde 13,6 g leichtes Magnesiumoxid (90 %ig) zugegeben. Die Aufschlämmung wurde 30 Minuten gerührt und dann auf 85"C erhitzt. 24,1 g Aluminiumchloridhexahydrat in 250 ml dest. Wasser wurden innerhalb einer Stunde eingetropft. Nach 4 weiteren Stunden bei 850C wurde die Mischung auf Raumtemperatur abgekühlt und dann durch Filtration auf einem Büchnertrichter isoliert.Acid-binding effect: 290 ml of n / 10 HCl. Example 2 To the 45.1 g of anhydrous Sodium carbonate containing solution was 13.6 g of light magnesium oxide (90%) admitted. The slurry was stirred for 30 minutes and then heated to 85 "C. 24.1 g aluminum chloride hexahydrate in 250 ml dist. Water were inside a Dripped in for an hour. After a further 4 hours at 85 ° C., the mixture came to room temperature cooled and then isolated by filtration on a Buchner funnel.
Das Produkt wurde analog Beispiel 1 gewaschen und getrocknet. Säurebindende Wirkung: 298 ml n/10 HCl.The product was washed and dried analogously to Example 1. Acid binding agents Effect: 298 ml n / 10 HCl.
Beispiel 3 Ein Aluminiumhydroxycarbonatgel wurde hergestellt, indem eine Lösung von 0,05 Mol (24,1 g) Aluminiumchloridhexahydrat in 100 ml dest. Wasser zu einer Lösung von 0,425 g (45,1 g) wasserfreies Natriumcarbonat in 150 ml dest. Wasser zugegeben wurde. Nach 30-minütigem Rühren bei Raumtemperatur wurde diese Aufschlämmung innerhalb 1 Stunde zu einer vorerhitzten (850C) Aufschlämmung von 0,3 Mol (12,2 g) Magnesiumoxid in 250 ml dest. Wasser zugegeben. Während der Zugabe wurde die Temperatur bei 850C gehalten. Die Mischung wurde noch 4 Stunden bei 850 erhitzt, dann auf Raumtemperatur abgekühlt und analog Beispiel 1 aufgearbeitet.Example 3 An aluminum hydroxycarbonate gel was prepared by a solution of 0.05 mol (24.1 g) of aluminum chloride hexahydrate in 100 ml of distilled water. water to a solution of 0.425 g (45.1 g) of anhydrous sodium carbonate in 150 ml of distilled water. Water was added. After stirring at room temperature for 30 minutes, this became Slurry to a preheated (850C) slurry of within 1 hour 0.3 mol (12.2 g) magnesium oxide in 250 ml dist. Water added. During the encore the temperature was kept at 850C. The mixture was still 4 hours at 850 heated, then cooled to room temperature and worked up analogously to Example 1.
Säurebindendes Vermögen: 286 ml n/10 HClAcid-binding capacity: 286 ml n / 10 HCl
Claims (6)
Priority Applications (6)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19833346943 DE3346943A1 (en) | 1983-12-24 | 1983-12-24 | Preparation of hydrotalcite with improved properties |
| KR1019840005765A KR870000365B1 (en) | 1983-12-24 | 1984-09-20 | Process for producing hydrotalcite |
| ES538755A ES8601069A1 (en) | 1983-12-24 | 1984-12-18 | Manufacture of hydrotalcite with improved properties |
| JP59267578A JPS60231416A (en) | 1983-12-24 | 1984-12-20 | Manufacture of hydrotalcite with improved properties |
| IT24162/84A IT1177488B (en) | 1983-12-24 | 1984-12-21 | HYDROTALCITE PRODUCTION EQUIPPED WITH IMPROVED PROPERTIES |
| PT79749A PT79749A (en) | 1983-12-24 | 1984-12-21 | Process for preparing hydrotalcite with improved properties |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19833346943 DE3346943A1 (en) | 1983-12-24 | 1983-12-24 | Preparation of hydrotalcite with improved properties |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE3346943A1 true DE3346943A1 (en) | 1985-07-04 |
Family
ID=6218037
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DE19833346943 Withdrawn DE3346943A1 (en) | 1983-12-24 | 1983-12-24 | Preparation of hydrotalcite with improved properties |
Country Status (6)
| Country | Link |
|---|---|
| JP (1) | JPS60231416A (en) |
| KR (1) | KR870000365B1 (en) |
| DE (1) | DE3346943A1 (en) |
| ES (1) | ES8601069A1 (en) |
| IT (1) | IT1177488B (en) |
| PT (1) | PT79749A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5292910A (en) * | 1990-04-02 | 1994-03-08 | Henkel Kommanditgesellschaft Auf Aktien | Use of hydrophobized hydrotalcites as catalysts for ethoxylation or propoxylation |
| WO1996005140A1 (en) * | 1994-08-15 | 1996-02-22 | Aluminum Company Of America | Two powder synthesis of hydrotalcite and hydrotalcite-like compounds |
| US5539135A (en) * | 1991-04-04 | 1996-07-23 | Henkel Kommanditgesellschaft Auf Aktien | Process for producing hydrophobicized double-layer hydroxide compounds |
| US8568792B2 (en) | 1997-09-19 | 2013-10-29 | Cytochroma Development Inc. | Metal compounds, mixed or sulphated, as phosphate binders |
| US9066917B2 (en) | 2009-08-03 | 2015-06-30 | Cytochroma Development Inc. | Mixed metal compound |
| US9566302B2 (en) | 2010-02-04 | 2017-02-14 | Opko Ireland Global Holdings, Ltd. | Composition comprising mixed metal compounds and xanthan gum |
| EP3210600A1 (en) | 2007-07-27 | 2017-08-30 | Opko Ireland Global Holdings, Ltd. | Mixed metal compounds used as antacids |
| US9907816B2 (en) | 2006-01-31 | 2018-03-06 | Opko Ireland Global Holdings, Ltd. | Water-insoluble, iron-containing mixed metal, granular material |
| US10155040B2 (en) | 2007-10-16 | 2018-12-18 | Opko Ireland Global Holdings, Ltd. | Mixed metal compounds for treatment of hyperphosphataemia |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100454273B1 (en) * | 2001-09-25 | 2004-10-26 | 주식회사 두본 | A method of hydrotalcite by polyhydric alcohol and polyhydric alcohol ester or metallic substituent and the hydrotalcite made of thereof |
| JP4585163B2 (en) * | 2002-05-10 | 2010-11-24 | 神島化学工業株式会社 | Hydrotalcite-based hydrated metal compound and method for producing the same, alkylene oxide addition reaction catalyst obtained by firing the compound, and method for evaluating the catalyst |
| KR101067900B1 (en) * | 2009-02-16 | 2011-09-27 | 경북대학교 산학협력단 | Method for preparing layered double hydroxide using metal hydroxide |
| JP5943176B2 (en) * | 2010-10-29 | 2016-06-29 | 三菱マテリアル株式会社 | Method and apparatus for treating harmful substance-containing water. |
| JP5915834B2 (en) * | 2010-10-29 | 2016-05-11 | 三菱マテリアル株式会社 | Method for producing purification treatment material |
| JP5794423B2 (en) * | 2011-09-30 | 2015-10-14 | 三菱マテリアル株式会社 | Processing method and processing apparatus for removing harmful substances |
-
1983
- 1983-12-24 DE DE19833346943 patent/DE3346943A1/en not_active Withdrawn
-
1984
- 1984-09-20 KR KR1019840005765A patent/KR870000365B1/en not_active Expired
- 1984-12-18 ES ES538755A patent/ES8601069A1/en not_active Expired
- 1984-12-20 JP JP59267578A patent/JPS60231416A/en active Pending
- 1984-12-21 IT IT24162/84A patent/IT1177488B/en active
- 1984-12-21 PT PT79749A patent/PT79749A/en unknown
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5292910A (en) * | 1990-04-02 | 1994-03-08 | Henkel Kommanditgesellschaft Auf Aktien | Use of hydrophobized hydrotalcites as catalysts for ethoxylation or propoxylation |
| US5539135A (en) * | 1991-04-04 | 1996-07-23 | Henkel Kommanditgesellschaft Auf Aktien | Process for producing hydrophobicized double-layer hydroxide compounds |
| WO1996005140A1 (en) * | 1994-08-15 | 1996-02-22 | Aluminum Company Of America | Two powder synthesis of hydrotalcite and hydrotalcite-like compounds |
| US8568792B2 (en) | 1997-09-19 | 2013-10-29 | Cytochroma Development Inc. | Metal compounds, mixed or sulphated, as phosphate binders |
| US9242869B2 (en) | 1997-09-19 | 2016-01-26 | Opko Ireland Global Holdings, Ltd. | Metal compounds mixed or sulphated, as phosphate binders |
| US9907816B2 (en) | 2006-01-31 | 2018-03-06 | Opko Ireland Global Holdings, Ltd. | Water-insoluble, iron-containing mixed metal, granular material |
| EP3210600A1 (en) | 2007-07-27 | 2017-08-30 | Opko Ireland Global Holdings, Ltd. | Mixed metal compounds used as antacids |
| US10201501B2 (en) | 2007-07-27 | 2019-02-12 | Opko Ireland Global Holdings, Ltd. | Mixed metal compounds used as antacids |
| US10155040B2 (en) | 2007-10-16 | 2018-12-18 | Opko Ireland Global Holdings, Ltd. | Mixed metal compounds for treatment of hyperphosphataemia |
| US9066917B2 (en) | 2009-08-03 | 2015-06-30 | Cytochroma Development Inc. | Mixed metal compound |
| US9314481B2 (en) | 2009-08-03 | 2016-04-19 | Opko Ireland Global Holdings, Ltd. | Method |
| US9566302B2 (en) | 2010-02-04 | 2017-02-14 | Opko Ireland Global Holdings, Ltd. | Composition comprising mixed metal compounds and xanthan gum |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS60231416A (en) | 1985-11-18 |
| PT79749A (en) | 1985-01-01 |
| ES538755A0 (en) | 1985-11-01 |
| IT1177488B (en) | 1987-08-26 |
| KR850004954A (en) | 1985-08-19 |
| ES8601069A1 (en) | 1985-11-01 |
| KR870000365B1 (en) | 1987-03-06 |
| IT8424162A0 (en) | 1984-12-21 |
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| 8130 | Withdrawal |