EP0002018A1 - Process for producing mixtures of crystalline zeolite and sodium triphosphate - Google Patents
Process for producing mixtures of crystalline zeolite and sodium triphosphate Download PDFInfo
- Publication number
- EP0002018A1 EP0002018A1 EP78101313A EP78101313A EP0002018A1 EP 0002018 A1 EP0002018 A1 EP 0002018A1 EP 78101313 A EP78101313 A EP 78101313A EP 78101313 A EP78101313 A EP 78101313A EP 0002018 A1 EP0002018 A1 EP 0002018A1
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- EP
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- Prior art keywords
- zeolite
- zeolites
- sodium
- orthophosphate
- molar ratio
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- 239000010457 zeolite Substances 0.000 title claims abstract description 36
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910021536 Zeolite Inorganic materials 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 16
- 239000000203 mixture Substances 0.000 title claims abstract description 12
- HWGNBUXHKFFFIH-UHFFFAOYSA-I pentasodium;[oxido(phosphonatooxy)phosphoryl] phosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O HWGNBUXHKFFFIH-UHFFFAOYSA-I 0.000 title claims abstract description 10
- 235000019832 sodium triphosphate Nutrition 0.000 title claims abstract description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 14
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 12
- 239000011734 sodium Substances 0.000 claims abstract description 12
- 239000007921 spray Substances 0.000 claims abstract description 11
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims abstract description 11
- 239000010452 phosphate Substances 0.000 claims abstract description 10
- 239000000047 product Substances 0.000 claims abstract description 10
- 239000000725 suspension Substances 0.000 claims abstract description 9
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims abstract description 5
- 238000002360 preparation method Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 9
- 238000001694 spray drying Methods 0.000 claims description 5
- 239000007900 aqueous suspension Substances 0.000 claims description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- -1 aluminum silicates Chemical class 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 150000001768 cations Chemical class 0.000 claims description 2
- 238000005507 spraying Methods 0.000 abstract 1
- 235000021317 phosphate Nutrition 0.000 description 8
- 235000011178 triphosphate Nutrition 0.000 description 5
- 239000001226 triphosphate Substances 0.000 description 5
- UNXRWKVEANCORM-UHFFFAOYSA-N triphosphoric acid Chemical compound OP(O)(=O)OP(O)(=O)OP(O)(O)=O UNXRWKVEANCORM-UHFFFAOYSA-N 0.000 description 5
- 239000001177 diphosphate Substances 0.000 description 4
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 description 4
- 235000011180 diphosphates Nutrition 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000003599 detergent Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 239000007859 condensation product Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005216 hydrothermal crystallization Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D11/00—Special methods for preparing compositions containing mixtures of detergents
- C11D11/02—Preparation in the form of powder by spray drying
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/06—Phosphates, including polyphosphates
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/12—Water-insoluble compounds
- C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
- C11D3/1246—Silicates, e.g. diatomaceous earth
- C11D3/128—Aluminium silicates, e.g. zeolites
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S423/00—Chemistry of inorganic compounds
- Y10S423/24—LTA, e.g. A, alpha, ZK-4, ZK-21, ZK-22
Definitions
- the present invention relates to a process for the preparation of mixtures of crystalline zeolites and sodium triphosphate by spray drying aqueous solutions or suspensions of sodium orthophosphate in a room in which the zeolites are introduced at the same time.
- Mixtures of this type which in addition to the triphosphate generally contain between 10 and 50% by weight of zeolites, are used above all as so-called builders for low-phosphate detergents.
- the procedure is such that the components which are produced in separate ways are mixed together in powder form, the triphosphate using known processes from sodium orthophosphate solutions or suspensions which contain about 28 to 32% by weight of P 2 O 5 and a Na: P molar ratio of 1.667, preferably obtained by spray drying at 350 to 500 ° C.
- the zeolites are obtained by hydrothermal crystallization of a water glass-aluminate synthesis mixture, the crystallization product being dried at 100 to 350 ° C. after separation from the mother liquor in a rotary tube or in a hot air spray tower.
- this causes the condensation of the phosphates to form a high proportion of diphosphate, on the other hand, part of the zeolites is structurally changed.
- Aluminum silicates of the general formula (Kat 2 / n O) x are preferably used as zeolites. Al 2 O 3 . (Si0 2 ) y used, in which Kat is a calcium-exchangeable cation of valence n, x is a number from 0.7 to 1.5 and y is a number from 0.8 to 6.
- Type A zeolites are used in particular. Spray drying is best carried out at temperatures between 350 and 500 ° C.
- the process according to the invention enables the condensation of the sodium triphosphate without significant diphosphate formation, the drying of the zeolite and the intensive mixing of both components in a single step. In comparison to the previous procedure, this means saving a spray tower for zeolite drying and, if appropriate, a device for mixing the components.
- the method according to the invention allows the production of mixtures of any composition.
- the Na: P molar ratio of the orthophosphate used must be less than 1.66 and greater than 1.56 in the process according to the invention, depending on the zeolite content desired in the end product.
- a spray tower 140 kg per hour of a P 2 0 5 20 weight percent sodium orthophosphate solution with a theoretical Na: P molar ratio of 1.66 for the formation of sodium triphosphate and 175 kg of an aqueous mash with 40% by weight zeolite A are separated by two nozzles (Nozzle spacing: 1 m) sprayed at a temperature of 410 ° C so that the two spray cones only touch when the surface of the zeolite particles are dry and the phosphate particles are at least partially condensed.
- a product mixture is obtained which, according to analytical and X-ray findings, consists in each case of 50% by weight of crystalline zeolite A and condensed phosphates. According to the paper chromatogram, the phosphate condensation product contains only 55% triphosphate in addition to 45% diphosphate.
- the same sodium orthophosphate solution and the zeolite mash are sprayed through two separate channels instead of through two spatially separate nozzles via a multi-substance nozzle or so that the spray cones touch immediately out of the nozzle.
- a product will be made whose phosphate content consists of 80% sodium diphosphate and only 20% triphosphate.
- the product contains only 30% Zeolite A instead of the expected content of 50%. The remaining 20% of the silicate material is in a modified, not examined form.
- Example 2 350 kg / h of an aqueous mash with 40% by weight of zeolite A and 120 kg / h of a sodium orthophosphate solution with a Na: P molar ratio of 1.59 are separated by two nozzles at the top of a spray tower (nozzle spacing: 1 m) as in Example 2 sprayed.
- the exhaust gas temperature of the tower is 380 ° C.
- the product mixture obtained consists, according to analytical and X-ray findings, of a mixture of the crystalline components zeolite A and sodium triphosphate in a weight ratio of 70:30. 4% of the total P 2 0 5 in the product were present as diphosphate.
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
Die vorliegende Erfindung betrifft ein Verfahren zur Herstellung von Gemischen aus Zeolith und Natriumtriphosphat, indem man Lösungen oder Suspensionen von Natriumorthophosphat gleichzeitig mit Zeolithen sprühtrocknet, wobei man Natriumorthophosphat einsetzt, das, ausgehend von dem für Natriumtriphosphat im Falle eines zeolithfreien Produktes theoretischen Na: P-Molverhältnis von 1,66, pro Anteil von jeweils 10 Gew.% Zeolith im Endprodukt, ein um jeweils 0,01 niedrigeres Na: P-Molverhältnis aufweist, und daß man die Zeolithsuspension in einer solchen Entfernung vom Orthophosphat versprüht, daß sich die Sprühkegel beider Komponenten erst dann berühren, wenn die Zeolithteilchen an ihrer Oberfläche bereits getrocknet und die Phosphatteilchen zumindest teilweise kondensiert sind.The present invention relates to a process for the preparation of mixtures of zeolite and sodium triphosphate by spraying solutions or suspensions of sodium orthophosphate simultaneously with zeolites, using sodium orthophosphate which, based on the theoretical Na: P molar ratio for sodium triphosphate in the case of a zeolite-free product of 1.66, per portion of 10% by weight of zeolite in the end product, has a respectively lower Na: P molar ratio of 0.01, and that the zeolite suspension is sprayed at such a distance from the orthophosphate that the spray cones of both components Do not touch until the surface of the zeolite particles has already dried and the phosphate particles are at least partially condensed.
Description
Die vorliegende Erfindung betrifft ein Verfahren zur Herstellung von Gemischen aus kristallinen Zeolithen und Natriumtriphosphat, durch Sprühtrocknen wäßriger Lösungen oder Suspensionen von Natriumorthophosphat in einem Raum, in welchen gleichzeitig die Zeolithe eingebracht werden.The present invention relates to a process for the preparation of mixtures of crystalline zeolites and sodium triphosphate by spray drying aqueous solutions or suspensions of sodium orthophosphate in a room in which the zeolites are introduced at the same time.
Derartige Gemische, die neben dem Triphosphat im allgemeinen zwischen 10 und 50 Gewichts% Zeolithe enthalten, werden vor allem als sogenannte Builder für phosphatarme Waschmittel verwendet.Mixtures of this type, which in addition to the triphosphate generally contain between 10 and 50% by weight of zeolites, are used above all as so-called builders for low-phosphate detergents.
Im allgemeinen verfährt man dabei so, daß man die jeweils auf getrennten Wegen hergestellten Komponenten in pulverförmigem Zustand miteinander vermischt, wobei das Triphosphat nach bekannten Verfahren aus Natriumorthophosphatlösungen oder -suspensionen, die etwa 28 bis 32 Gewichts% P2O5 enthalten und ein Na : P-Molverhältnis von 1,667 aufweisen, vorzugsweise durch Sprühtrocknung bei 350 bis 500°C erhalten wird.In general, the procedure is such that the components which are produced in separate ways are mixed together in powder form, the triphosphate using known processes from sodium orthophosphate solutions or suspensions which contain about 28 to 32% by weight of P 2 O 5 and a Na: P molar ratio of 1.667, preferably obtained by spray drying at 350 to 500 ° C.
Die Zeolithe werden dagegen durch hydrothermale Kristallisation einer Wasserglas-Aluminatsynthesemischung erhalten, wobei das Kristallisationsprodukt nach Abtrennung von der Mutterlauge im Drehrohr oder in einem Heißluftsprühturm bei 100 bis 3500C getrocknet wird.The zeolites, on the other hand, are obtained by hydrothermal crystallization of a water glass-aluminate synthesis mixture, the crystallization product being dried at 100 to 350 ° C. after separation from the mother liquor in a rotary tube or in a hot air spray tower.
Bei den bekannten Verfahren ist in jedem Fall eine getrennte Herstellung und Lagerung beider Builderkomponenten erforderlich.In the known methods, separate production and storage of both builder components is required in each case.
Diese bisherige Praxis könnte deutlich wirtschaftlicher gestaltet werden, wenn es gelänge, insbesondere den apparativ aufwendigen Verfahrensschritt der Trocknung der Zeolithe mit der Herstellung des Triphosphates zu kombinieren. Es ist auch schon versucht worden, bei der Herstellung phosphatarmer Wasch- und Reinigungsmittel zumindest einen Teil der Zeolithe während der Zerstäubungstrocknung des phosphathaltigen wäßrigen Waschmittelansatzes in pulveriger Form in den Raum einzubringen, in welchem die zerstäubten Partikel getrocknet werden (DE-OS 2 529 685).This previous practice could be made significantly more economical if it were possible to combine, in particular, the complex process step of drying the zeolites with the production of the triphosphate. In the manufacture of low-phosphate detergents and cleaning agents, attempts have also already been made to introduce at least some of the zeolites in powder form into the space in which the atomized particles are dried during the atomization drying of the phosphate-containing aqueous detergent batch (DE-OS 2 529 685). .
Vom apparativen Aufwand her, wie auch aus Gründen der Energieeinsparung schien es zweckmäßig, die Zeolithmaische gemeinsam mit der Orthophosphatlösung bzw. -suspension unter Verwendung einer Zweistoffdüse gemeinsam zu versprühen; doch führten entsprechende Versuche nicht zu den gewünschten Produkten, da offenbar beim Austritt der Komponenten aus der Sprühdüse eine Wechselwirkung der Komponenten aufeinander über die noch vorhandene wäßrige Phase erfolgt.In terms of equipment, as well as for reasons of energy saving, it seemed expedient to spray the zeolite mash together with the orthophosphate solution or suspension using a two-component nozzle; However, corresponding tests did not lead to the desired products, since the components apparently interact with one another via the aqueous phase which is still present when the components emerge from the spray nozzle.
Dadurch verläuft einerseits die Kondensation der Phosphate unter Bildung eines hohen Anteils an Diphosphat, andererseits wird ein Teil der Zeolithe strukturell verändert.On the one hand, this causes the condensation of the phosphates to form a high proportion of diphosphate, on the other hand, part of the zeolites is structurally changed.
Überraschenderweise wurde nun gefunden, daß sich die Nachteile der bekannten Arbeitsweisen vermeiden lassen, wenn man Natriumorthophosphatlösungen oder -suspensionen in einem Raum sprühtrocknet, die, ausgehend von dem für Natriumtriphosphat im Falle eines zeolithfreien Produktes theoretischen Na : P-Molverhältnis von 1,66, pro Anteil von jeweils 10 Gewichts% Zeolith im Endprodukt, ein um jeweils 0,01 niedrigeres Na : P-Molverhältnis aufweisen, und wenn man gleichzeitig die Zeolithe in Form einer wäßrigen Suspension in den genannten Raum einbringt, wobei die Zeolithsuspension in einer solchen Entfernung vom Orthophosphat versprüht wird, daß sich die Sprühkegel beider Komponenten erst dann berühren, wenn die Zeolithteilchen an ihrer Oberfläche bereits getrocknet und die Phosphatteilchen zumindest teilweise kondensiert sind. Als Zeolithe werden dabei vorzugsweise Aluminiumsilikate der allgemeinen Formel (Kat2/nO)x. Al2O3. (Si02)y eingesetzt, worin Kat ein mit Calcium austauschbares Kation der Wertigkeit n, x eine Zahl von 0,7 bis 1,5 und y eine Zahl von 0,8 bis 6 ist.Surprisingly, it has now been found that the disadvantages of the known procedures can be avoided by spray-drying sodium orthophosphate solutions or suspensions in a room which, based on the theoretical Na: P molar ratio of 1.66 for a zeolite-free product, is 1.66 per Proportion of 10% by weight of zeolite in the end product, each having a Na: P molar ratio which is lower by 0.01, and if the zeolites are simultaneously introduced into the space in the form of an aqueous suspension, the zeolite suspension being at such a distance from the orthophosphate is sprayed that the spray cones of both components only touch when the zeolite particles have already dried on their surface and the phosphate particles are at least partially condensed. Aluminum silicates of the general formula (Kat 2 / n O) x are preferably used as zeolites. Al 2 O 3 . (Si0 2 ) y used, in which Kat is a calcium-exchangeable cation of valence n, x is a number from 0.7 to 1.5 and y is a number from 0.8 to 6.
Insbesondere verwendet man Zeolithe des Typs A. Das Sprühtrocknen führt man am besten bei Temperaturen zwischen 350 und 500°C durch.Type A zeolites are used in particular. Spray drying is best carried out at temperatures between 350 and 500 ° C.
Die erhaltenen Gemische zeichnen sich dadurch aus, daß sie sehr feinteilig, rieselfähig und lagerbeständig sind.The mixtures obtained are distinguished by the fact that they are very finely divided, free-flowing and stable in storage.
Das erfindungsgemäße Verfahren ermöglicht die Kondensation des Natriumtriphosphates ohne nennenswerte Diphosphatbildung, die Trocknung des Zeolithen und die intensive Vermischung beider Komponenten in einem einzigen Arbeitsschritt. Im Vergleich zur bisherigen Verfahrensweise bedeutet dies eine Einsparung eines Sprühturmes für die Zeolithtrocknung und gegebenenfalls einer Vorrichtung zur Mischung der Komponenten.The process according to the invention enables the condensation of the sodium triphosphate without significant diphosphate formation, the drying of the zeolite and the intensive mixing of both components in a single step. In comparison to the previous procedure, this means saving a spray tower for zeolite drying and, if appropriate, a device for mixing the components.
Das erfindungsgemäße Verfahren erlaubt die Herstellung von Gemischen beliebiger Zusammensetzung.The method according to the invention allows the production of mixtures of any composition.
Der Zusammenhang zwischen dem Zeolithanteil im Endprodukt und dem erforderlichen Na : P-Molverhältnis in der eingesetzten Orthophosphatlösung bzw.-suspension ist in dem nachfolgenden Diagramm dargestellt.The relationship between the zeolite content in the end product and the required Na: P molar ratio in the orthophosphate solution or suspension used is shown in the diagram below.
Wie aus dem Diagramm hervorgeht, muß nach dem erfindungsgemäßen Verfahren, je nach dem im Endprodukt gewünschten Zeolithanteil, das Na : P-Molverhältnis des eingesetzten Orthophosphates kleiner als 1,66 und größer als 1,56 sein.As can be seen from the diagram, the Na: P molar ratio of the orthophosphate used must be less than 1.66 and greater than 1.56 in the process according to the invention, depending on the zeolite content desired in the end product.
Anhand der folgenden Beispiele soll die vorliegende Erfindung näher erläutert werden.The present invention is to be explained in more detail with the aid of the following examples.
Am Kopf eines Sprühturmes werden stündlich 140 kg einer an P205 20 gewichtsprozentigen Natriumorthophosphatlösung mit einem für die Bildung von Natriumtriphosphat theoretischen Na : P-Molverhältnis von 1,66 und 175 kg einer wäßrigen Maische mit 40 Gewichts% Zeolith A getrennt durch zwei Düsen (Düsenabstand: 1 m) bei einer Temperatur von 410°C so eingesprüht, daß sich die beiden Sprühkegel erst berühren, wenn die Zeolithteilchen an der Oberfläche trocken und die Phosphatteilchen zumindest teilweise kondensiert sind. Erhalten wird ein Produktgemisch, das nach analytischem und röntgenographischem Befund zu je 50 Gewichts% aus kristallinem Zeolith A und kondensierten Phosphaten besteht. Das Phosphatkondensationsprodukt enthält laut Papierchromatogramm nur 55 % Triphosphat neben 45 % Diphosphat.At the top of a spray tower, 140 kg per hour of a P 2 0 5 20 weight percent sodium orthophosphate solution with a theoretical Na: P molar ratio of 1.66 for the formation of sodium triphosphate and 175 kg of an aqueous mash with 40% by weight zeolite A are separated by two nozzles (Nozzle spacing: 1 m) sprayed at a temperature of 410 ° C so that the two spray cones only touch when the surface of the zeolite particles are dry and the phosphate particles are at least partially condensed. A product mixture is obtained which, according to analytical and X-ray findings, consists in each case of 50% by weight of crystalline zeolite A and condensed phosphates. According to the paper chromatogram, the phosphate condensation product contains only 55% triphosphate in addition to 45% diphosphate.
In Abänderung von Beispiel 1 wird eine Natriumorthophosphatlösung mit einem Na : P-Molverhältnis von 1,61 bei sonst unveränderten Bedingungen eingesetzt. In diesem Fall enthält das kristalline Reaktionsprodukt neben 50 Gewichtsteilen Zeolith A zu gleichen Teilen ein Phosphatkondensationsprodukt,das zu 95 % aus Natriumtriphosphat besteht.In a modification of Example 1, a sodium orthophosphate solution with a Na: P molar ratio of 1.61 is used under otherwise unchanged conditions. In this case, the crystalline reaction product contains 50 parts by weight of zeolite A in equal parts and a phosphate condensation product which consists of 95% sodium triphosphate.
In Abänderung zum Beispiel 2 werden die gleiche Natriumorthophosphatlösung und die Zeolithmaische statt über zwei räumlich getrennte Düsen über eine Mehrstoff-Düse durch zwei separate Kanäle eingesprüht o daß sich die Sprühkegel unmittelbar nach aus der Düse berühren. In diesem Fall wird ein Produkt eine fen, dessen Phosphatanteil zu 80 % aus Natriumdiphosphat und nur 20 % aus Triphosphat besteht. Daneben enthält das Produkt nur 30 % Zeolith A statt des zu erwartenden Gehaltes von 5o %. Die restlichen 20 % des silikatischen Materials liegen in veränderter, nicht näher untersuchter Form vor.In modification for example 2, the same sodium orthophosphate solution and the zeolite mash are sprayed through two separate channels instead of through two spatially separate nozzles via a multi-substance nozzle or so that the spray cones touch immediately out of the nozzle. In this case, a product will be made whose phosphate content consists of 80% sodium diphosphate and only 20% triphosphate. In addition, the product contains only 30% Zeolite A instead of the expected content of 50%. The remaining 20% of the silicate material is in a modified, not examined form.
350 kg/h einer wäßrigen Maische mit 40 Gewichts% Zeolith A und 120 kg/h einer Natriumorthophosphatlösung mit einem Na : P-Molverhältnis von 1,59 werden getrennt durch zwei Düsen am Kopf eines Sprühturmes (DUsenabstand: 1 m) wie im Beispiel 2 eingesprüht. Die Abgastemperatur des Turmes beträgt 380°C. Das erhaltene Produktgemisch besteht nach analytischem und röntgenographischem Befund aus einem Gemisch der kristallinen Komponenten Zeolith A und Natriumtriphosphat im Gewichtsverhältnis 70 : 30. 4 % des Gesamt-P205 im Produkt lagen als Diphosphat vor.350 kg / h of an aqueous mash with 40% by weight of zeolite A and 120 kg / h of a sodium orthophosphate solution with a Na: P molar ratio of 1.59 are separated by two nozzles at the top of a spray tower (nozzle spacing: 1 m) as in Example 2 sprayed. The exhaust gas temperature of the tower is 380 ° C. The product mixture obtained consists, according to analytical and X-ray findings, of a mixture of the crystalline components zeolite A and sodium triphosphate in a weight ratio of 70:30. 4% of the total P 2 0 5 in the product were present as diphosphate.
Claims (4)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19772751354 DE2751354A1 (en) | 1977-11-17 | 1977-11-17 | PROCESS FOR THE PREPARATION OF MIXTURES FROM CRYSTALLINE ZEOLITE AND SODIUM TRIPHOSPHATE |
| DE2751354 | 1977-11-17 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0002018A1 true EP0002018A1 (en) | 1979-05-30 |
| EP0002018B1 EP0002018B1 (en) | 1981-06-10 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP78101313A Expired EP0002018B1 (en) | 1977-11-17 | 1978-11-04 | Process for producing mixtures of crystalline zeolite and sodium triphosphate |
Country Status (4)
| Country | Link |
|---|---|
| US (1) | US4180471A (en) |
| EP (1) | EP0002018B1 (en) |
| DE (2) | DE2751354A1 (en) |
| IT (1) | IT1109288B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1446104B2 (en) † | 2001-11-01 | 2011-08-03 | Novartis AG | Spray drying methods |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2820554A1 (en) * | 1978-05-11 | 1979-11-22 | Hoechst Ag | DETERGENTS AND DETERGENTS |
| EP0061296B1 (en) * | 1981-03-20 | 1984-10-24 | Unilever Plc | Process for the manufacture of detergent compositions containing sodium aluminosilicate |
| DE3111236A1 (en) * | 1981-03-21 | 1982-09-30 | Hoechst Ag, 6000 Frankfurt | GRANULATE FROM ALKALIALUMINUM SILICATE AND PENTANATRIUM TRIPHOSPHATE AND METHOD FOR THE PRODUCTION THEREOF |
| US5110776A (en) * | 1991-03-12 | 1992-05-05 | Mobil Oil Corp. | Cracking catalysts containing phosphate treated zeolites, and method of preparing the same |
| AU652222B2 (en) * | 1991-03-12 | 1994-08-18 | Mobil Oil Corporation | Preparation of cracking catalysts, and cracking process using them |
| US20030203036A1 (en) | 2000-03-17 | 2003-10-30 | Gordon Marc S. | Systems and processes for spray drying hydrophobic drugs with hydrophilic excipients |
| US7575761B2 (en) | 2000-06-30 | 2009-08-18 | Novartis Pharma Ag | Spray drying process control of drying kinetics |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2529685A1 (en) * | 1974-07-04 | 1976-01-15 | Henkel & Cie Gmbh | METHOD FOR PRODUCING LOW PHOSPHATE OR PHOSPHATE-FREE DETERGENT OR CLEANING AGENTS |
| DE2510675A1 (en) * | 1975-03-12 | 1976-09-23 | Degussa | Ion-exchanging aluminium silicate - having a hydrophilised surface obtained by treatment with phosphate ions |
| US4019998A (en) * | 1974-09-27 | 1977-04-26 | The Procter & Gamble Company | Process for preparing a pyrophosphate-silicate detergent product |
| DE2742484A1 (en) * | 1976-09-24 | 1978-03-30 | Lion Fat Oil Co Ltd | PROCESS FOR THE MANUFACTURING OF A GRILLY DETERGENT OR CLEANING AGENT |
Family Cites Families (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2080557A1 (en) * | 1970-02-17 | 1971-11-19 | Albert Ag Chem Werke | |
| US3684724A (en) * | 1970-04-20 | 1972-08-15 | Stauffer Chemical Co | Process for making mixtures of sodium polyphosphates and sodium sulfate |
| US3629955A (en) * | 1970-07-31 | 1971-12-28 | Procter & Gamble | Multilevel spray-drying apparatus |
| US3996149A (en) * | 1971-09-27 | 1976-12-07 | Burke Oliver W Jun | Detergent compositions and detergent adjuvant combinations thereof, and processes for forming the same |
| US4083793A (en) * | 1973-05-23 | 1978-04-11 | Henkel Kommanditgesellschaft Auf Aktien | Washing compositions containing aluminosilicates and nonionics and method of washing textiles |
| US3985669A (en) * | 1974-06-17 | 1976-10-12 | The Procter & Gamble Company | Detergent compositions |
| AT338948B (en) * | 1974-10-10 | 1977-09-26 | Henkel & Cie Gmbh | POWDERED DETERGENTS AND CLEANING AGENTS AND METHOD FOR THEIR PRODUCTION |
| US4088593A (en) * | 1975-03-12 | 1978-05-09 | Henkel Kommanditgesellschaft Auf Aktien (Henkel Kgaa) | Ion-exchanging aluminum silicate with hydrophilic surfaces |
| US4019999A (en) * | 1975-07-23 | 1977-04-26 | The Procter & Gamble Co. | Spray-dried granular detergent containing aluminosilicate, silicate, and pyrophosphate |
| US4102977A (en) * | 1975-11-18 | 1978-07-25 | Mizusawa Kagaku Kogyo Kabushiki Kaisha | Process for the preparation of alkali aluminosilicate detergent builder |
-
1977
- 1977-11-17 DE DE19772751354 patent/DE2751354A1/en not_active Withdrawn
-
1978
- 1978-11-04 EP EP78101313A patent/EP0002018B1/en not_active Expired
- 1978-11-04 DE DE7878101313T patent/DE2860759D1/en not_active Expired
- 1978-11-13 US US05/960,240 patent/US4180471A/en not_active Expired - Lifetime
- 1978-11-15 IT IT51905/78A patent/IT1109288B/en active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2529685A1 (en) * | 1974-07-04 | 1976-01-15 | Henkel & Cie Gmbh | METHOD FOR PRODUCING LOW PHOSPHATE OR PHOSPHATE-FREE DETERGENT OR CLEANING AGENTS |
| US4019998A (en) * | 1974-09-27 | 1977-04-26 | The Procter & Gamble Company | Process for preparing a pyrophosphate-silicate detergent product |
| DE2510675A1 (en) * | 1975-03-12 | 1976-09-23 | Degussa | Ion-exchanging aluminium silicate - having a hydrophilised surface obtained by treatment with phosphate ions |
| DE2742484A1 (en) * | 1976-09-24 | 1978-03-30 | Lion Fat Oil Co Ltd | PROCESS FOR THE MANUFACTURING OF A GRILLY DETERGENT OR CLEANING AGENT |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1446104B2 (en) † | 2001-11-01 | 2011-08-03 | Novartis AG | Spray drying methods |
| US8936813B2 (en) | 2001-11-01 | 2015-01-20 | Novartis Ag | Spray drying methods and related compositions |
Also Published As
| Publication number | Publication date |
|---|---|
| DE2751354A1 (en) | 1979-05-23 |
| EP0002018B1 (en) | 1981-06-10 |
| IT1109288B (en) | 1985-12-16 |
| DE2860759D1 (en) | 1981-09-17 |
| US4180471A (en) | 1979-12-25 |
| IT7851905A0 (en) | 1978-11-15 |
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