FR2744115A1 - Hydrophobising especially glass or silica surfaces - Google Patents

Hydrophobising especially glass or silica surfaces Download PDF

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Publication number
FR2744115A1
FR2744115A1 FR9601319A FR9601319A FR2744115A1 FR 2744115 A1 FR2744115 A1 FR 2744115A1 FR 9601319 A FR9601319 A FR 9601319A FR 9601319 A FR9601319 A FR 9601319A FR 2744115 A1 FR2744115 A1 FR 2744115A1
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Prior art keywords
minerals
silica particles
glass surfaces
hydrophobic
hydrophobising
Prior art date
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FR9601319A
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French (fr)
Inventor
Francis Millasseau
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DUCHENE SABINE
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DUCHENE SABINE
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Publication date
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Priority to FR9601319A priority Critical patent/FR2744115A1/en
Publication of FR2744115A1 publication Critical patent/FR2744115A1/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/126Preparation of silica of undetermined type
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B13/00Oxygen; Ozone; Oxides or hydroxides in general
    • C01B13/02Preparation of oxygen
    • C01B13/0203Preparation of oxygen from inorganic compounds
    • C01B13/0211Peroxy compounds
    • C01B13/0214Hydrogen peroxide
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C15/00Surface treatment of glass, not in the form of fibres or filaments, by etching
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/28Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material
    • C03C17/30Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material with silicon-containing compounds
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C23/00Other surface treatment of glass not in the form of fibres or filaments
    • C03C23/0075Cleaning of glass
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/53After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone involving the removal of at least part of the materials of the treated article, e.g. etching, drying of hardened concrete
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28Compounds of silicon
    • C09C1/30Silicic acid
    • C09C1/3081Treatment with organo-silicon compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/12Treatment with organosilicon compounds

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Structural Engineering (AREA)

Abstract

Process for hydrophobising glass surfaces, silica particles and other minerals, by silanisation following decontamination, employs a catalyst such as iron perchloride for producing oxygen radicals from hydrogen peroxide during the decontamination step. Preferably, silanisation is carried out by immersion in a solution of not more than 10<-2> mol/l. alkyl trichlorosilane in a conventional solvent such as a light alkane.

Description

La présente invention consiste à traiter des surfaces minérales (ex: silice) dans le but de les rendre hydrophobes selon un procédé simplifié.The present invention consists in treating mineral surfaces (eg silica) with the aim of making them hydrophobic according to a simplified process.

Actuellement les surfaces en silice peuvent être rendues hydrophobes par silanisation. Ce procédé consiste à greffer sur ces surfaces des molécules d'alkyltrichlorosilanes, une fois qu'elles sont parfaitement nettoyées. A ce jour la décontamination de telles surfaces peut être obtenue grâce à l'action de l'acide sulfurique et de l'eau oxygénée suivi d'un traitement à l'ozone en présence d'un rayonnement ultra-violet. Ce dernier traitement produit de l'oxygéne radicalaire super oxydant selon la réaction:

Figure img00010001
Currently, silica surfaces can be made hydrophobic by silanization. This process consists in grafting onto these surfaces alkyltrichlorosilane molecules, once they are perfectly cleaned. To date, the decontamination of such surfaces can be obtained by virtue of the action of sulfuric acid and hydrogen peroxide followed by treatment with ozone in the presence of ultraviolet radiation. This last treatment produces super oxidizing radical oxygen according to the reaction:
Figure img00010001

Nous proprosons un procédé beaucoup plus simple et moins polluant pour produire l'oxyoéne radicalaire selon la réaction:

Figure img00010002
We are proposing a much simpler and less polluting process to produce radical oxyene according to the reaction:
Figure img00010002

<tb> H202---catalyseur--- > H20 <SEP> + <SEP> 0
<tb>
La cinétique de cette réaction peut être modulée grâce à l'utilisation d'un catalyseur peu coûteux le perchlorure de fer (en autres). Un tel procédé évite non seulement l'utilisation de l'acide sulfurique ( produit particulièrement polluant), mais aussi la rejet de l'ozone dans la biomasse.
<tb> H202 --- catalyst ---> H20 <SEP> + <SEP> 0
<tb>
The kinetics of this reaction can be modulated through the use of an inexpensive catalyst, iron perchloride (among others). Such a process avoids not only the use of sulfuric acid (a particularly polluting product), but also the rejection of ozone in the biomass.

La deuxième étape, actuellement utilisée consiste à silaniser la surface ainsi décontaminée par trempage dans un mélange d'hexadécane et d'un solvant chloré en présence d'un alkyltrichlorosilane. Ce procédé est non seulement coûteux mais aussi polluant ( ex: le tétrachlorure de carbone est connu pour ses propriétés tératogénes ).The second step, currently used, consists in silanizing the surface thus decontaminated by soaking in a mixture of hexadecane and a chlorinated solvent in the presence of an alkyltrichlorosilane. This process is not only expensive but also polluting (eg carbon tetrachloride is known for its teratogenic properties).

Le procédé que nous préconisons fait appel à des solvants classiques couramment utilisés tels que le gas-oil ou des alcanes légers (ex: o.ctane). Le trempage dans de tels solvants en présence d'alkyltrichlorosilanes ( au maximum 10-2 molellitre) conduit, au bout de 30 minutes au plus, à une surface hydrophobe dont la tension critique est del 'ordre de22 mNm L selon le. critère deZisman.The process we recommend uses conventional solvents commonly used such as gas oil or light alkanes (eg o.ctane). Soaking in such solvents in the presence of alkyltrichlorosilanes (maximum 10-2 molelliter) leads, after 30 minutes at most, to a hydrophobic surface whose critical tension is of the order of 22 mNm L according to. Zisman criterion.

Le procédé décrit selon la présente innovation est particulièrement destiné à rendre hydrophobes toutes surfaces et particules, telles que:
Lames de verre ordinaire (ex: lames de microscope)
Tubes de verre (ex: niveaux à bulle)
Produits en verre plat ( ex: vitres, mirroirs, plateaux, etc..)
Produitsemverresoufflé-(ex-: bouteilles et flacons divers)
Produits en verre travaillé ( ex: rétroviseurs, vaisselle)
Sables utilisés dans le ravalement de façades
Sables à forte teneur en silice (ex: sable à béton, chantier B.T.P)
Sables utilisés dans les jardins publics (ex: bacs à sable)
Le procédé décrit selon la présente invention, utilisé seulement dans son étape de décontamination, est applicable à tout les minéraux et polymères organiques (acide humiques et fulviques) insolubles dans l'eau, et en particulier au décapage des sols.
The process described according to the present innovation is particularly intended to make all surfaces and particles hydrophobic, such as:
Plain glass slides (e.g. microscope slides)
Glass tubes (ex: spirit levels)
Flat glass products (ex: panes, mirrors, trays, etc.)
Blown glass products - (ex-: various bottles and flasks)
Products in worked glass (ex: mirrors, dishes)
Sands used in facades
Sands with a high silica content (e.g. concrete sand, construction site)
Sands used in public gardens (ex: sandboxes)
The method described according to the present invention, used only in its decontamination step, is applicable to all minerals and organic polymers (humic and fulvic acids) insoluble in water, and in particular to soil stripping.

Claims (3)

- Revendications -- Claims - 1) Procédé pour rendre hydrophobes les surfaces de verre, les particules en silice. et autres minéraux. par silanisation après procédé de décontamination caractérisé par l'emploi d'un catalyseur tel que le perc.hlorure de fer pour la production d'oxygéne radicalaire à partir d'eau oxygénée lors de l'étape de décontamination1) Process for making glass surfaces hydrophobic, silica particles. and other minerals. by silanization after a decontamination process characterized by the use of a catalyst such as iron chloride for the production of radical oxygen from hydrogen peroxide during the decontamination step 2) Procédé pour rendre hydrophobes surfaces de verre, les particules en silice, et autres minéraux selon la revendication 1, caractérisé par l'utilisation de solvants classiques tels que les alcanes légers comme milieu de silanisation.2) A method for making glass surfaces, silica particles, and other minerals hydrophobic according to claim 1, characterized by the use of conventional solvents such as light alkanes as silanization medium. 3) Procédé pour rendre hydrophobes surfaces de verre, les particules en silice, et autres minéraux selon les revendications 1 et 2, caractérisé par le trempage de 30 minutes au plus des surfaces de verre, des particules en silice, et autres minéraux dans une solution contenant des molécules d'âlkyltrichlorosilanes avec une quantité maximale de 10-2 mole/litre. 3) Process for making hydrophobic glass surfaces, silica particles, and other minerals according to claims 1 and 2, characterized by soaking for 30 minutes at most glass surfaces, silica particles, and other minerals in a solution containing alkyltrichlorosilane molecules with a maximum amount of 10-2 mol / liter.
FR9601319A 1996-01-30 1996-01-30 Hydrophobising especially glass or silica surfaces Withdrawn FR2744115A1 (en)

Priority Applications (1)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014186316A1 (en) * 2013-05-17 2014-11-20 3M Innovative Properties Company Pressure sensitive adhesive assembly comprising filler material

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4520073A (en) * 1983-12-23 1985-05-28 Usg Corporation Pressure coating of mineral fillers
EP0352180A1 (en) * 1988-07-20 1990-01-24 Saint-Gobain Vitrage International Glass pane provided with an anti-ice coating
JPH02184539A (en) * 1989-01-11 1990-07-19 Furukawa Electric Co Ltd:The Surface treatment of preform for optical fiber
SU1625838A1 (en) * 1989-03-21 1991-02-07 Кубанский государственный университет Protective coat for glass

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4520073A (en) * 1983-12-23 1985-05-28 Usg Corporation Pressure coating of mineral fillers
EP0352180A1 (en) * 1988-07-20 1990-01-24 Saint-Gobain Vitrage International Glass pane provided with an anti-ice coating
JPH02184539A (en) * 1989-01-11 1990-07-19 Furukawa Electric Co Ltd:The Surface treatment of preform for optical fiber
SU1625838A1 (en) * 1989-03-21 1991-02-07 Кубанский государственный университет Protective coat for glass

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
CHEMICAL ABSTRACTS, vol. 92, no. 14, 7 April 1980, Columbus, Ohio, US; abstract no. 116474m, page 358; XP002017313 *
DATABASE WPI Week 03, Derwent World Patents Index; AN 92-022119, XP002017315 *
DATABASE WPI Week 35, Derwent World Patents Index; AN 90-264382, XP002017314 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014186316A1 (en) * 2013-05-17 2014-11-20 3M Innovative Properties Company Pressure sensitive adhesive assembly comprising filler material
US11518914B2 (en) 2013-05-17 2022-12-06 3M Innovative Properties Company Pressure sensitive adhesive assembly comprising filler material

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