EP0002018B1 - Procédé pour la fabrication de mélanges de zéolithe cristallin et de triphosphate de sodium - Google Patents

Procédé pour la fabrication de mélanges de zéolithe cristallin et de triphosphate de sodium Download PDF

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Publication number
EP0002018B1
EP0002018B1 EP78101313A EP78101313A EP0002018B1 EP 0002018 B1 EP0002018 B1 EP 0002018B1 EP 78101313 A EP78101313 A EP 78101313A EP 78101313 A EP78101313 A EP 78101313A EP 0002018 B1 EP0002018 B1 EP 0002018B1
Authority
EP
European Patent Office
Prior art keywords
zeolite
zeolites
sodium
molar ratio
sodium triphosphate
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.)
Expired
Application number
EP78101313A
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German (de)
English (en)
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EP0002018A1 (fr
Inventor
Klaus Dr. Schrödter
Joachim Dr. Kandler
Hasso Spott
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hoechst AG
Original Assignee
Hoechst AG
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Hoechst AG filed Critical Hoechst AG
Publication of EP0002018A1 publication Critical patent/EP0002018A1/fr
Application granted granted Critical
Publication of EP0002018B1 publication Critical patent/EP0002018B1/fr
Expired legal-status Critical Current

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Classifications

    • 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 a powdery state, the triphosphate using known processes from sodium orthophosphate solutions or suspensions which contain about 28 to 32% by weight of P205 and a Na: P- Have 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. In the known methods, separate production and storage of both builder components is required in each case.
  • the zeolite powder If the zeolite powder is dusted in at a point where the particles of the atomized mixture are still moist, they bind the aluminum silicate powder to agglomerates. This is done e.g. B. in the vicinity of the atomizer nozzles.
  • 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.
  • Type A zeolites are used in particular. Spray drying is best carried out at temperatures between 350 and 500 ° C.
  • the mixtures obtained are distinguished by the fact that they are very finely divided, free-flowing and stable in storage.
  • the process according to the invention enables the condensation of the sodium orthophosphate 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.
  • Example 2 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.
  • 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.
  • the same sodium orthophosphate solution and the zeolite mash are sprayed through a separate nozzle through two separate channels instead of through two spatially separate nozzles, so that the spray cones touch immediately after the nozzle emerges.
  • a product is obtained whose phosphate content consists of 80% sodium diphosphate and only 20% triphosphate.
  • the product contains only 30% Zeolite A instead of the expected 50% content. The remaining 20% of the silicate material is in a modified, not examined form.
  • Example 2 350Xg / 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)

Claims (4)

1. Procédé de préparation de mélanges d'une zéolite cristalline et de triphosphate de sodium par atomisation de suspensions aqueuses contenant du phosphate de sodium dans une chambre dans laquelle on introduit simultanément les zéolites, caractérisé en ce que l'on met en oeuvre des solutions ou suspensions d'orthophosphate de sodium qui, partant du rapport molaire Na/P théorique de 1,66 pour le triphosphate de sodium dans le cas d'un produit exempt de zéolite, présentent un rapport molaire Na/P abaissé de 0,01 pour chaque fraction de 10% en poids de zéolite dans le produit final, et en ce qu'on introduit les zéolites à l'état de suspension aqueuse dans la même chambre par pulvérisation à une distance de l'orthophosphate telle que les billes d'atomisation des deux composants n'entrent en contact que lorsque les particules de zéolite sont déjà sèches en surface et les particules de phosphate condensées en partie au moins.
2. Procédé selon la revendication 1, caractérisé en ce que l'on utilise en tant que zéolites des aluminosilicates de formule générale (Cat2/nO)x, Ah03. (Si02)y dans laquelle Cat représente un cation de valence n échangeable contre le calcium, x est un nombre allant de 0,7 à 1,5 et y un nombre allant de 0,8 à 6.
3. Procédé selon la revendication 1 ou 2, caractérisé en ce que l'on utilise en tant que zéolites des zéolites de type A
4. Procédé selon les revendications 1 à 3, caractérisé en ce que l'atomisation est effectuée à des températures de 350 à 5000 C.
EP78101313A 1977-11-17 1978-11-04 Procédé pour la fabrication de mélanges de zéolithe cristallin et de triphosphate de sodium Expired EP0002018B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19772751354 DE2751354A1 (de) 1977-11-17 1977-11-17 Verfahren zur herstellung von gemischen aus kristallinem zeolith und natriumtriphosphat
DE2751354 1977-11-17

Publications (2)

Publication Number Publication Date
EP0002018A1 EP0002018A1 (fr) 1979-05-30
EP0002018B1 true EP0002018B1 (fr) 1981-06-10

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP78101313A Expired EP0002018B1 (fr) 1977-11-17 1978-11-04 Procédé pour la fabrication de mélanges de zéolithe cristallin et de triphosphate de sodium

Country Status (4)

Country Link
US (1) US4180471A (fr)
EP (1) EP0002018B1 (fr)
DE (2) DE2751354A1 (fr)
IT (1) IT1109288B (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8337895B2 (en) 2000-06-30 2012-12-25 Novartis Ag Spray drying process control of drying kinetics
US8802149B2 (en) 1996-12-31 2014-08-12 Novartis Pharma Ag Systems and processes for spray drying hydrophobic and hydrophilic components

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2820554A1 (de) * 1978-05-11 1979-11-22 Hoechst Ag Wasch- und reinigungsmittel
EP0061296B1 (fr) * 1981-03-20 1984-10-24 Unilever Plc Procédé pour la préparation de compositions détergentes contenant de l'aluminosilicate de sodium
DE3111236A1 (de) * 1981-03-21 1982-09-30 Hoechst Ag, 6000 Frankfurt Granulat aus alkalialuminiumsilikat und pentanatrium-triphosphat sowie verfahren zu dessen herstellung
AU652222B2 (en) * 1991-03-12 1994-08-18 Mobil Oil Corporation Preparation of cracking catalysts, and cracking process using them
US5110776A (en) * 1991-03-12 1992-05-05 Mobil Oil Corp. Cracking catalysts containing phosphate treated zeolites, and method of preparing the same
US8524279B2 (en) 2001-11-01 2013-09-03 Novartis Ag Spray drying methods and related compositions

Family Cites Families (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2080557A1 (fr) * 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
AT334489B (de) * 1974-07-04 1976-01-25 Henkel & Cie Gmbh Verfahren zur herstellung phosphatarmer bzw. phosphatfreier wasch- und reinigungsmittel
US4019998A (en) * 1974-09-27 1977-04-26 The Procter & Gamble Company Process for preparing a pyrophosphate-silicate detergent product
AT338948B (de) * 1974-10-10 1977-09-26 Henkel & Cie Gmbh Pulverformige wasch- und reinigungsmittel und verfahren zu ihrer herstellung
DE2510675C3 (de) * 1975-03-12 1983-12-15 Degussa Ag, 6000 Frankfurt Verfahren zur Herstellung eines kristallinen, ionenaustauschenden Alkalialuminiumsilikates mit hydrophiler Oberfläche und dessen Verwendung
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
US4129511A (en) * 1976-09-24 1978-12-12 The Lion Fat & Oil Co., Ltd. Method of spray drying detergents containing aluminosilicates

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8802149B2 (en) 1996-12-31 2014-08-12 Novartis Pharma Ag Systems and processes for spray drying hydrophobic and hydrophilic components
US8337895B2 (en) 2000-06-30 2012-12-25 Novartis Ag Spray drying process control of drying kinetics

Also Published As

Publication number Publication date
EP0002018A1 (fr) 1979-05-30
DE2860759D1 (en) 1981-09-17
DE2751354A1 (de) 1979-05-23
IT7851905A0 (it) 1978-11-15
IT1109288B (it) 1985-12-16
US4180471A (en) 1979-12-25

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