GB2252305A - Zeolite manufacture by a continuous gel crystallization process - Google Patents

Zeolite manufacture by a continuous gel crystallization process Download PDF

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Publication number
GB2252305A
GB2252305A GB9102056A GB9102056A GB2252305A GB 2252305 A GB2252305 A GB 2252305A GB 9102056 A GB9102056 A GB 9102056A GB 9102056 A GB9102056 A GB 9102056A GB 2252305 A GB2252305 A GB 2252305A
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United Kingdom
Prior art keywords
gel
crystallizer
zeolite
process according
temperature
Prior art date
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GB9102056A
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GB9102056D0 (en
Inventor
Puerto Ramon Artigas
Benito Juan Forner
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Foret SA
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Foret SA
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Publication date
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Priority to GB9102056A priority Critical patent/GB2252305A/en
Publication of GB9102056D0 publication Critical patent/GB9102056D0/en
Publication of GB2252305A publication Critical patent/GB2252305A/en
Withdrawn legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/20—Silicates
    • C01B33/26—Aluminium-containing silicates, i.e. silico-aluminates
    • C01B33/28—Base exchange silicates, e.g. zeolites
    • C01B33/2807—Zeolitic silicoaluminates with a tridimensional crystalline structure possessing molecular sieve properties; Isomorphous compounds wherein a part of the aluminium ore of the silicon present may be replaced by other elements such as gallium, germanium, phosphorus; Preparation of zeolitic molecular sieves from molecular sieves of another type or from preformed reacting mixtures
    • C01B33/2815—Zeolitic silicoaluminates with a tridimensional crystalline structure possessing molecular sieve properties; Isomorphous compounds wherein a part of the aluminium ore of the silicon present may be replaced by other elements such as gallium, germanium, phosphorus; Preparation of zeolitic molecular sieves from molecular sieves of another type or from preformed reacting mixtures of type A (UNION CARBIDE trade name; corresponds to GRACE's types Z-12 or Z-12L)
    • C01B33/2823—Zeolitic silicoaluminates with a tridimensional crystalline structure possessing molecular sieve properties; Isomorphous compounds wherein a part of the aluminium ore of the silicon present may be replaced by other elements such as gallium, germanium, phosphorus; Preparation of zeolitic molecular sieves from molecular sieves of another type or from preformed reacting mixtures of type A (UNION CARBIDE trade name; corresponds to GRACE's types Z-12 or Z-12L) from aqueous solutions of an alkali metal aluminate and an alkali metal silicate excluding any other source of alumina or silica
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
    • C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

Zeolites are proposed by continuous crystallization of a gel through a cascade of crystallizers (preferably 10) 9 to 18, of increasing temperature throughout the series e.g. with an initial temperature of 80 DEG C and a final temperature of 100 DEG C, with controlled agitation and a maximum residence time from one crystallizer to the other of 5 minutes. The gel is conventionally produced starting from reactors 1 and 5. In reactor 1 natural silica coming from tank 2 reacts with sodium hydroxide coming from tank 4, while in reactor 5 the aluminium mineral coming from tank 6 reacts with sodium hydroxide. The mass is cooled and concentrated in step 19 being afterwards filtered in 20, dried in 23 and final product Zeolite, is ready to be used in 24. Zeolite 4A for use in detergents is the preferred product. <IMAGE>

Description

ZEOLITE MANITACIIJE BY A CONTINUOUS GEL CRYSTALLIZATION PROCESS PURPOSE OF THE INVENTION The invention is referred to a continuous gel crystallization process in order to manufacture zeolites to be used in detergents. This process has the characteristic of crystallization throughout a phase without any operative interruption, obtaining a product with a particle size between 1 and 7 microns, and an optimum calcium absortion capacity with less energy and saving in manpower compared with a repetitive cicle operative process.
This process requires less quality control compared with the traditional operation.
BACKGROUND OF THE INVENTION Zeolite 4A is used in detergent manufacturing due to its capacity to retain the calcium present in the water.
However, it has been verified that the efficiency of Zeolite 4A in cloth washing does not only depends on Ca2+ absorption (washing water softening) but, basically, on the washing water Ca2+ depletion rate. The particle size of the product, completed in the crystalliztion phase, is decisive in relation to the kinetic reponse against of the Ca2+ in the washing process. Continuous crystallization, according to the present invention, allows a fine particle size adjutment and guarantees a regularity in the physical and chemical characteristics of the product.
STATE OF THE ART It is not the first attempt of continuous crystallization. The document DE 2941636 proposed a multi-phase crystallization in a tubular reactor. This attempt has not achieved the desired results since the proposed crystallization is not flexible in times, requires a continuous control and does not allow any particle size adjustment.
Against the prior art, the invention allows a stage by stage control in order to manufacture a final optimization.
High productivity and easy control are a need for any Zeolite crystallization process, and this is the purpose of this invention.
As an informative matter, we refer to patent documents with a non-continuous crystallization cicle, such as US 3310373 and BE 840315.
DESCRIPTION OF THE INVENTION The process of this invention lies on passing the gel formed in a gellyfier by cascaded crystallizers (preferibly ten), each one provided with time and temperature controllers, with adjustable agitation, being the first crystallizier at 80 C of temperature, while the last one is at 100 C, with a temperature increasing in each crystallizer with a continuous renewal sothe reacting mass does not stay more than 5 minutes in each crytallizer.
DESCRIPTION OF TIIE DRAWINGS In order to illustrate grafically what has been said, attached there is a drawing sheet representing a complete diagram of the Zeolite manufacture process including the crystallization process of this invention.
DESCRIPTION OF AN EXAMPLE OF REALIZATION In reactor 1, natural silica from tank 1 reacts with sodium hydroxide from tank 4; in reactor 5 aluminum mineral from tank 6 reacts with sodium hydroxide from tank 4; the reaction product of reactor 1 passes to the gel preparation step 7, while the reaction product of reactor 5 passes across the heat exchanger 8, and then, at 75"C of temperature, passes to the gel preparation step 7.
The gel from step 7 passes to the crytallizer 9 at 80 C of temperature, mantaining a controlled agitation and residence time. From crytallizer 9 it passes to crytallizer 10 continuing this way until it arrives to crytallizer 18, controlling time and temperature in each crytallizer, with a progressive temperature increasing until the achievement of 100 C and with a maximum temporary cicle of 5 minutes from one to the other.
The slurry obtained in the crystallization process is cooled and concentrated in 19, afterwards it is filtrated and washed in step 20, where the mother liquor is recicled after their passing by exchanger 8 to reactor 5. Washing waters pass to purifier 21 to be treated with an alkaline solution of SiO2. The resulting suspension is filtered in filter 22, being the liquid recirculated to reactor 1 and the solid to reactor 5. After drying in stage 23 at a temperature not above llO"C, Zeolite 4A is manufactured.
SUMMARY OF THE INVENTION In brief, the invention lies on passing a gel coming from the jellyfying step 7 throughout several (preferably 10) cascaded crytallizers 9 to 18, with an initial temperature of 80"C in progression until a final temperature of 100"C, with controlled agitation and a maximum residence time from one crytallizer to the other of 5 minutes.
The gel is conventionally produced starting from reactors 1 and 5. In reactor 1 natural silica coming from tank 2 reacts with sodium hydroxide coming from tank 4, while in reactor 5 the aluminum mineral coming from tank 6 reacts with sodium hydroxide. The mass is cooled and concentrated in step 19, being afterwards filtered in 20, dried in 23 and the final product, Zeolite, is ready to be used in 24.

Claims (10)

CLAIMS:
1. A process of preparing zeolite by continuous crystallization comprising preparing a gel by reacting together silicon dioxide (Si02) and aluminium oxide (A1203) in alkaline solution and passing the gel through a cascade of crystallizers, the temperature in each crystallizer being controlled such that in each crystallizer (except the first) the temperature is greater than the temperature in the immediately preceding crystallizer.
2. A process according to claim 1, wherein there are ten crystallizers in the cascade.
3. A process according to either preceding claim. wherein the level of the gel in each crystallizer is controlled.
4. A process according to any preceding claim, wherein the gel is subjected to controlled shaking in each crystallizer.
5. A process according to any preceding claim, wherein the temperatures in the crystallizer vary fram 80"C to 1000C.
6. A process according to any preceding claim, wherein residence time of the gel does not exceed five minutes.
7. A process according to any preceding claim, wherein the zeolite produced is washed with water and the washing water recycled for use in preparing the gel.
8. A process according to any preceding claim wherein the zeolite produced is subjected to one or more operations selected from cooling, concentrating, filtering and drying.
9. Gel continuous crystallization process in order to manufacture Zeolite characterized because it lies on passing a gel conventionally formed in a gel reactor starting from the reaction of two alkaline solution of SiO2 and A1203, by a plurality (preferably ten) cascaded crystallizers, each one provided with level control and adjustable agitation, being the first crystallizer at a temperature of 800C while the last one is at 100 0C, producing a temperature increasing between consecutive crystallizers, passing from one crystallizer to other assuring a total drainage in a maximum of 5 minutes, and being afterwards cooled, concentrated, filtrated and dried according to any conventional operation.
10. A process of preparing zeolite, substantially as described herein with reference to the accompanying drawings.
GB9102056A 1991-01-31 1991-01-31 Zeolite manufacture by a continuous gel crystallization process Withdrawn GB2252305A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
GB9102056A GB2252305A (en) 1991-01-31 1991-01-31 Zeolite manufacture by a continuous gel crystallization process

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GB9102056A GB2252305A (en) 1991-01-31 1991-01-31 Zeolite manufacture by a continuous gel crystallization process

Publications (2)

Publication Number Publication Date
GB9102056D0 GB9102056D0 (en) 1991-03-13
GB2252305A true GB2252305A (en) 1992-08-05

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Family Applications (1)

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GB9102056A Withdrawn GB2252305A (en) 1991-01-31 1991-01-31 Zeolite manufacture by a continuous gel crystallization process

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GB (1) GB2252305A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5989518A (en) * 1998-12-29 1999-11-23 Uop Llc Process for synthesizing and controlling the particle size and particle size distribution of a molecular sieve
WO2001034520A1 (en) * 1999-11-09 2001-05-17 Kao Corporation Process for preparing fine zeolite particles
US6656447B1 (en) 1998-12-29 2003-12-02 Uop Llc Process for synthesizing and controlling the particle size and particle size distribution of a molecular sieve

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4339419A (en) * 1980-02-25 1982-07-13 Degussa Ag Process for the production of crystalline zeolite powder of type A
US4591491A (en) * 1982-02-04 1986-05-27 Henkel Kommanditgesellschaft Auf Aktien Process for the continuous conversion of meta-kaolin into very finely-divided zeolitic sodium alumino-silicate
US4818509A (en) * 1984-03-23 1989-04-04 Mobil Oil Corporation Continuous process for manufacturing crystalline zeolites in continuously stirred backmixed crystallizers

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4339419A (en) * 1980-02-25 1982-07-13 Degussa Ag Process for the production of crystalline zeolite powder of type A
US4591491A (en) * 1982-02-04 1986-05-27 Henkel Kommanditgesellschaft Auf Aktien Process for the continuous conversion of meta-kaolin into very finely-divided zeolitic sodium alumino-silicate
US4818509A (en) * 1984-03-23 1989-04-04 Mobil Oil Corporation Continuous process for manufacturing crystalline zeolites in continuously stirred backmixed crystallizers

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5989518A (en) * 1998-12-29 1999-11-23 Uop Llc Process for synthesizing and controlling the particle size and particle size distribution of a molecular sieve
EP1016627A1 (en) * 1998-12-29 2000-07-05 Uop Llc Controlling the particle size and particle size distribution in a process for continuous synthesis of molecular sieves
US6656447B1 (en) 1998-12-29 2003-12-02 Uop Llc Process for synthesizing and controlling the particle size and particle size distribution of a molecular sieve
WO2001034520A1 (en) * 1999-11-09 2001-05-17 Kao Corporation Process for preparing fine zeolite particles
EP1435337A2 (en) * 1999-11-09 2004-07-07 Kao Corporation Process for preparing fine zeolite particles
US6831056B1 (en) 1999-11-09 2004-12-14 Kao Corporation Process for preparing fine alkaline earth metal zeolite particles
EP1435337A3 (en) * 1999-11-09 2006-10-04 Kao Corporation Process for preparing fine zeolite particles
US7211555B2 (en) 1999-11-09 2007-05-01 Kao Corporation Process for preparing fine zeolite particles

Also Published As

Publication number Publication date
GB9102056D0 (en) 1991-03-13

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