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WO1991015429A1 - Procede pour fabriquer des silicates stratifies susceptibles de gonfler - Google Patents

Procede pour fabriquer des silicates stratifies susceptibles de gonfler Download PDF

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Publication number
WO1991015429A1
WO1991015429A1 PCT/EP1991/000586 EP9100586W WO9115429A1 WO 1991015429 A1 WO1991015429 A1 WO 1991015429A1 EP 9100586 W EP9100586 W EP 9100586W WO 9115429 A1 WO9115429 A1 WO 9115429A1
Authority
WO
WIPO (PCT)
Prior art keywords
reaction
hydrothermal
reaction mixture
ammonia
water
Prior art date
Application number
PCT/EP1991/000586
Other languages
German (de)
English (en)
Inventor
Britta Liesenfeld
Hans Dolhaine
Heinz Müller
Claus-Peter Herold
Stephan Von Tapavicza
Willi WÜST
Josef Wollmann
Original Assignee
Henkel Kommanditgesellschaft Auf Aktien
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 Henkel Kommanditgesellschaft Auf Aktien filed Critical Henkel Kommanditgesellschaft Auf Aktien
Publication of WO1991015429A1 publication Critical patent/WO1991015429A1/fr

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Classifications

    • 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
    • C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
    • C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
    • C01B33/40—Clays
    • 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
    • C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
    • C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
    • C01B33/40—Clays
    • C01B33/405—Clays not containing aluminium

Definitions

  • the invention relates to a simplified synthesis process for the production of water-swellable smectite clays and describes in particular a possibility in a simple manner to master the difficulties which arise in the production of highly swellable hectorites, saponites and / or saponite-hectorite hybrids.
  • a large-scale application area of high swellable synthetic layered silicates of the type concerned here is. the use thereof as a viscosity-building agent in aqueous drilling mud and borehole treatment agents in the exploration and development of deposits of, for example, petroleum and natural gas, but also in Ceothermal drilling, water drilling, in the execution of geoscientific drilling and in drilling in the mining sector.
  • EP-A 260 538 should be mentioned here in particular.
  • the use of selected synthetic swellable sheet silicates of the hectorite and / or saponite type for such water-based drilling fluid systems is described here.
  • Example 1 The last-mentioned literature reference describes in Example 1 a typical process for the production of the synthetic layer silicates of the hectorite type to be used there.
  • An aqueous suspension is prepared from magnesium sulfate, sodium hydroxide solution, sodium silicate solution and lithium carbonate and is then reacted for about 4 hours at 180 ° C. in a stirred autoclave.
  • the resulting product must then be filtered off from the mother liquor and the filter cake thus obtained must be washed with deionized water before the material is dried.
  • These decisive steps of filtering a primarily formed hectorite slurry with subsequent washing of the separated solid phase are also integral components of the flow diagrams 3 and 4 from the cited literature reference Karl-Heinz Bergk et al.
  • the invention has set itself the task of designing the known process for the production of synthetic and, in particular, highly swellable smectite clays in such a way that cleaning the crude reaction product by filtration and subsequent washing no longer poses the previously known difficulties.
  • the invention aims to make it possible to obtain high-purity smectite clays of a given structure and swellability by simply drying up the reaction crude product which is primarily obtained in the hydrothermal reaction, without intensive washing of the reaction raw product being necessary.
  • the invention provides two main elements: the formation of the basic environment for the hydrothermal conversion is ensured by the use of a selected volatile base.
  • the reactant mixture for the hydrothermal layered silicate-forming reaction should also be free or practical be free from those constituents that form non-volatile reaction by-products, in particular corresponding salts, during the implementation.
  • the invention accordingly relates to a process for the production of swellable layered silicates of the smectite type by hydrothermal pressure treatment of mixtures and / or coprecipitates of the layered silicate-forming components in the presence of an excess of water and free bases.
  • the new process is characterized in that a reaction mixture is introduced into the hydrothermal reaction stage, the base excess of which is formed by means of ammonia.
  • the aqueous-basic reaction medium is at least partially separated from the layered silicate formed.
  • reaction mixtures containing at least predominantly oxidic and / or hydroxide reactants are used as the starting material for the hydrothermal reaction.
  • feed mixtures are essentially free of non-volatile foreign constituents and contain, as volatile mixture components, the water required for hydrothermal synthesis and ammonia for setting the basic reaction medium.
  • the reactants containing magnesium, aluminum and silicon are introduced as oxidic and / or hydroxide reaction components.
  • Mixed compounds, such as sodium silicate and / or sodium aluminate, can be added to the reaction mixture in a manner known per se. It is essential for the invention that the use of disruptive amounts of foreign constituents, such as are entered into the reaction mixture, for example when magnesium salts are used - for example of the type of magnesium sulfate or magnesium chloride - and thus the need for subsequent separation and Request cleaning of the raw reaction product.
  • the swellable layered silicates formed can be freed from water and ammonia simply by drying. This drying can be carried out at normal pressure and / or at reduced pressure and can be accelerated by using elevated temperatures.
  • the portions of the reaction mixture which are driven off via the vapor phase can, if desired, be condensed and used in whole or in part in circulation for further reaction mixtures.
  • the drying of the product and / or that The free volatile base can be stripped off, for example, at temperatures up to 300 ° C., preferably in the range between 50 and approximately 250 ° C., the temperature range from approximately 80 to 180 ° C. being particularly important.
  • this drying stage not only the water but in particular also the volatile basic compound used for the reaction control can be driven off in the process according to the invention.
  • This process step can be carried out in one or more stages in the sense of a joint removal of water and volatile base or a gradual separation of these volatile reaction aids.
  • the time period for such a final drying and / or temperature treatment results primarily from the time period required for the volatile components to be driven off. In general, this period will not exceed 1 to 2 hours.
  • the temperature treatment can range from a few minutes to about 45 minutes.
  • the solid reaction product obtained is expediently ground into a fine powder.
  • All suitable grinding devices for example toothed disk mills, are suitable for this.
  • magnesium hydroxide or magnesium oxide can be used as the magnesium-containing compound; in particular, amorphous silicic acid, for example precipitated silica, diatomaceous earth, but also water glass can be used as the silicon-containing compound, with the proviso that the sodium hydroxide content which is registered at the same time is the stoichiometric desired proportion not or not significantly exceeds.
  • Aluminum hydroxide, so-called aluminum moist hydrate or aluminate lye can be used as the aluminum-containing compound, taking into account the restriction given previously for water glass.
  • a suitable lithium-containing compound is, for example, lithium hydroxide. If fluoride ions are to be introduced into the reaction product, appropriate proportions of sodium and / or lithium fluoride are particularly suitable.
  • the amount of volatile base to be used in each case can be in a relatively wide range and - based on the magnesium oxide present in the reaction mixture - can be, for example, in the range from 0.1 to 5 mol of the volatile base per mol of magnesium oxide. It will generally be preferred to limit the amount of this basic component as much as possible so that preferred addition amounts of the base to the reaction mixture for the hydrothermal reaction are in the range of about 0.2 to 2 moles of ammonia per mole of magnesium oxide in the reaction mixture.
  • the reaction is carried out in particular under the pressure of the reaction mixture at process temperature.
  • the process temperatures in particular range from about 150 to 300 ° C., expediently from about 200 to 270 ° C.
  • the reaction time is in the range of 1 to 100 hours, preferably between about 1 and 20 hours. After about 2 to 8 hours, the reaction has usually progressed so far that the workup can be carried out in the sense of the drying treatment according to the invention.
  • the solids contents during the hydrothermal reaction phase are in the usual range.
  • the solids content can be up to about 40% (by mass) in aqueous / basic Reaction mixture can be raised.
  • preference is given to working at lower solids contents which are in the range up to approximately 15% (mass fraction) and in particular below approximately 10% (mass fraction).
  • the invention relates to the swellable smectite clays produced by the process according to the invention and to their use in particular in the context of water-based drilling fluid systems, as described in detail in EP-A 260 538.
  • the mixture of reactants in this batch corresponds to the following molar ratios:
  • Magnesium oxide was slurried in about 700 g of water on a Pendraulik stirrer, lithium hydroxide was dissolved in it, and the mixture of water glass, about 150 g of water and precipitated silica was added. After stirring for 5 minutes, the suspension was added to the autoclave, to which the ammonia solution was added after sealing. Crystallization: 4 hours at 250 ° C

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

Est décrit un procédé simplifié pour fabriquer des silicates stratifiés susceptibles de gonfler, du type smectite, par traitement hydrothermal sous pression de mélanges et/ou de coprécipités des constituants formant les silicates stratifiés, en présence d'un excès d'eau et de bases libres. Ce nouveau procédé est caractérisé en ce qu'un mélange de réaction contenant un excédent de bases sous forme d'ammoniaque est introduit dans l'étape de réaction hydrothermale, et en ce que pendant le traitement du produit brut de réaction, le milieu de réaction aqueux-basique est au moins partiellement séparé du silicate stratifié formé, si on le désire.
PCT/EP1991/000586 1990-04-04 1991-03-26 Procede pour fabriquer des silicates stratifies susceptibles de gonfler WO1991015429A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19904010878 DE4010878A1 (de) 1990-04-04 1990-04-04 Vereinfachtes verfahren zur herstellung von quellfaehigen schichtsilikaten (i)
DEP4010878.3 1990-04-04

Publications (1)

Publication Number Publication Date
WO1991015429A1 true WO1991015429A1 (fr) 1991-10-17

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ID=6403753

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP1991/000586 WO1991015429A1 (fr) 1990-04-04 1991-03-26 Procede pour fabriquer des silicates stratifies susceptibles de gonfler

Country Status (2)

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DE (1) DE4010878A1 (fr)
WO (1) WO1991015429A1 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102024121958A1 (de) 2023-08-11 2025-02-13 Devinochem GmbH & Co.KG Schichtsilikat, Verfahren zu dessen Herstellung und dessen Verwendung

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2189491A1 (fr) * 1972-05-26 1974-01-25 Nl Industries Inc
US3892655A (en) * 1972-12-01 1975-07-01 Chevron Res Layered clay minerals, catalysts, and processes for using
US3959118A (en) * 1972-05-26 1976-05-25 N L Industries, Inc. Hydrocarbon cracking with synthetic smectite compositions
FR2349541A1 (fr) * 1976-04-26 1977-11-25 Nl Industries Inc Argiles synthetiques gonflantes et leur preparation
JPS58181718A (ja) * 1982-04-16 1983-10-24 Kunimine Kogyo Kk 新規合成珪酸塩ならびにその製造方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2189491A1 (fr) * 1972-05-26 1974-01-25 Nl Industries Inc
US3959118A (en) * 1972-05-26 1976-05-25 N L Industries, Inc. Hydrocarbon cracking with synthetic smectite compositions
US3892655A (en) * 1972-12-01 1975-07-01 Chevron Res Layered clay minerals, catalysts, and processes for using
FR2349541A1 (fr) * 1976-04-26 1977-11-25 Nl Industries Inc Argiles synthetiques gonflantes et leur preparation
JPS58181718A (ja) * 1982-04-16 1983-10-24 Kunimine Kogyo Kk 新規合成珪酸塩ならびにその製造方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
World Patents Indexe Latest Accession, Nr. 83-830471, Woche 48, Derwent Publications Ltd., (London, GB), & JP-A-58181718 (KUNIMINE KOGYO), 24. Oktober 1983 *

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Publication number Publication date
DE4010878A1 (de) 1991-10-10

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