Method for production of a sealed coating for surfaces of buildings comprising a cross-linked sealed silicone membrane, adhesive and ready-to-use kit for application of said method

CA 02452306 2003-12-23 WO 03/002677 PCT / FR02 / 02286 1 Method for producing a waterproof coating of surfaces for buildings comprising a crosslinked and waterproof silicone membrane, glue and ready-to-use kit for use of this process The field of the invention is that of silicone compositions curable by crosslinking and usable in particular as mastic or any other sealing material, or to form water-repellent elastomeric coatings, applicable by spreading or spraying (eg: paints, semi-thick, flexible coatings).

More specifically, the invention relates to the production of a waterproof coating to be placed on the surface of floors, walls or building ceilings.

These coatings will be called, in what follows, by the expression "surface coatings".

In particular, the coverings in question are intended to be laid in damp places or rooms.

Conventionally, these coatings comprise, by way of external covering, ceramic tiles, in mineral material included in a resin matrix or in a cement matrix or even concrete tiles.

In addition to this outer covering, for example in tiling, the coating in question in the present invention consists of a superposition of layers comprising, from the surface to be coated:

-> optionally at least one layer of adhesion primer, - ~ at least one waterproof polymer membrane, - ~ optionally at least one web of fibrous material, woven or not, for reinforcement, ~ at least one layer of glue, ~ and the outer cover, for example tiling.

In this type of surface coverings, a waterproofing membrane consisting of a flexible and deformable polymer film is interposed between the outer covering, namely for example the tiling, and the surface (screed) to be coated in a sealed manner.

These waterproof polymer membranes, for example under tiling, are intended to guarantee the waterproofing of the construction in rooms or damp places (showers, bathrooms, kitchens, water rooms, swimming pool edges, etc.).

It is important that this waterproof polymer membrane can adhere to all surfaces encountered in the building industry (concrete, metals, wood, among others), that it be resistant, that it fills in a durable and reliable way over time. its sealing function, and that it allows the adhesion, on its external surface, of the adhesive of the external coating, for example in tiling.

Floor coverings for damp rooms or places are already known, consisting of a superposition of layers comprising, from the surface to be coated:

- a film of adhesion primer covering the surface of the floor, wall or ceiling, CA 02452306 2003-12-23 WO 03/002677 PCT / FR02 / 02286 2 - a first membrane in acrylic (co) polymer or in copolymer vinyl / diene monomer such as for example the styrene / butadiene copolymer, most often made of acrylic (co) polymer, - a reinforcing sheet of non-woven fibrous material (for example polyester fiber mat), - a second membrane in acrylic (co) polymer or in vinyl monomer / diene copolymer such as for example styrene / butadiene copolymer, most often in acrylic (co) polymer, - a layer of adhesive, - and finally the outer cover, by example in ceramic tiles.

These known multilayer structures comprising membranes obtained from eg acrylic latex exhibit a certain number of drawbacks.

First of all, these waterproof acrylic polymer membranes are not water resistant shortly after their application.

Thus, the water present in the work environment disturbs the crosslinking / curing of acrylic polymer films.

As a result, their mechanical qualities and their water barrier qualities may be altered.

Sealed meinbrans made from organic polymers suffer from another major drawback which is their lack of elasticity.

Once installed, they therefore tend to crack so that they can no longer fulfill their primary sealing function.

To overcome this, it is necessary to insert in the superposition of the constituent layers of the coating, at least one sheet of reinforcing fibrous material.

It is clear that this operation does not go in the direction of simplifying the process for producing the covering, for example for tiled floors.

In addition, these membranes, for example under tiling made of organic polymer, have the defect of not being "breathable".

Indeed, they form a barrier to water as well as to air, so that all the conditions conducive to the development of mold are created.

Another drawback of these superpositions or layers constituting such surface coatings comprising waterproof organic polymer membranes, results from the very long waiting times for curing / crosslinking which it is necessary to observe between each coating layer of organic polymer. .

These waiting times increase the duration of the process for constructing the surface coating all the more if the latter comprises at least two organic polymeric sealing membranes.

CA 02452306 2003-12-23 WO 03/002677 PCT / FR02 / 02286 3 All of this also involves the task of the operator who carries out these surface coatings.

Furthermore, the known constructions of surface coatings comprising waterproofing membranes made of organic polymer, require the use of adhesion primers on all surfaces, in order to have a correct adhesion of the latex membranes and of the tiling on the surface. to be coated.

Such systematic coating of primers affects the speed of the manufacturing process of the surface coating.

In this state of the art, one of the essential objectives of the present invention is to remedy the drawbacks of the surface coatings (having for example an external tile covering) of the prior art, in particular in terms of resistance to water. water, simplicity of implementation and reduction in exposure time.

Another essential objective of the invention is to provide a method for producing a waterproof surface covering for buildings (floor / wall / ceiling) in which the number of layers and therefore of labor operations is limited.

Another essential objective of the present invention is to provide a process for producing a waterproof surface covering for buildings (floor / wall / ceiling) in which the intermediate polymeric sealing membrane has mechanical qualities, and in particular elasticity. , allowing it to withstand mechanical stresses over time and thus avoid the use of a fibrous reinforcing mat in the superposition of layers constituting the surface coating.

Another essential objective of the invention is to provide a process for producing a waterproof surface covering for buildings (floor / wall / ceiling) in which the polymeric waterproofing membrane is obtained in a simple and practical manner. , from an aqueous dispersion of easily applicable polymer, for example with a brush or a roller.

Another essential objective of the invention is to provide a method for producing a waterproof surface covering for buildings (floor / wall / ceiling) in which it is possible to do without, for certain surfaces, the preliminary step. application of an adhesion primer.

Another essential objective of the invention is to provide a process for producing a waterproof surface covering for buildings (floor / wall / ceiling), in which the adhesion between the covering and the surface (concrete or wooden screed for example), as well as the adhesion between the adhesive introduced between the external covering (for example in tiles) and the waterproofing membrane, is as good as possible.

Another essential objective of the invention is to provide a process for producing a waterproof surface covering for buildings (floor / wall / ceiling) in which the waterproofing membrane (s) used, n 'is not subject to the problem of CA 02452306 2009-04-30 4 uptake of water and is not sensitive to water, in particular shortly (about 3 hours) after its coating to form a crosslinked polymer film / hardened.

Another essential objective of the invention is to provide a method of producing a waterproof surface covering for buildings (floor / wall / ceiling) in which the durations of the labor operations and the waiting times are reduced. .

Another essential objective of the invention is to provide a process for producing a waterproof surface coating for buildings (floor / wall / ceiling) making it possible to obtain good adhesion to damp surfaces and involving products which do not 'have no harmful effects on the environment and which are not likely to soil the tools and equipment used for their implementation, in such a way that cleaning is heavy and restrictive.

Another essential objective of the invention is to provide an adhesive for waterproof surface coatings of buildings (floor / wall / ceiling), capable of being used for the implementation of the process used (adhesive for example for tiling).

Another essential objective of the invention is to provide a ready-to-use kit for implementing the aforementioned method and comprising in particular:

- an aqueous silicone dispersion making it possible to quickly and easily obtain a crosslinked waterproof film - and optionally an adhesive for the outer covering (for example tiling), - or even the outer covering (for example tiling).

These objectives, among others, are achieved by the present invention which relates first of all to a process for producing a waterproof surface covering, for buildings (floor / wall / ceiling), of the type of those consisting in fixing to the wall. surface a superposition of layers or elements comprising, from the surface to be coated:

~ optionally at least one layer of adhesion primer, ~ at least one waterproof polymer membrane, ~ (optionally at least one web of fibrous material, woven or not,) ~ at least one layer of glue, ~ at least an outer cover;

characterized in that:

at. the waterproof membrane is selected from those capable of being obtained from an aqueous dispersion of silicone oil (s) comprising:

-A- 100 parts by weight of at least one oil CA 02452306 2009-04-30 4a organopolysiloxane (A) having a viscosity greater than or equal to 10 Pa.s. and capable of crosslinking by condensation, if necessary in the presence of a crosslinking agent (B), into an elastomer;

CA 02452306 2009-04-30 WO 03/002677 PCT / FR02 / 02236 -A'- optionally up to 30 parts by weight of at least one non-reactive organopolysiloxane oil;

-B- if necessary, from 0.1 to 100 parts by weight of at least one crosslinking agent (B);

5 -C- optionally, up to 50 parts by weight of at least one adhesion promoter (C);

-D- up to 200 parts by dry weight of at least one filler (D);

-E- a catalytically effective amount of a catalytic curing compound (E) of up to 3 parts by weight;

-F- at least one emulsifier (F);

-G- optionally at least one functional additive (G);

-H- and water;

b. the glue used is based on cement and on a binder and further comprises at least one adhesion promoter (C ′);

vs. the aqueous dispersion of silicone oil (s) is applied as a film on the surface;

d. crosslinking of the silicone film then takes place, preferably at room temperature;

e. at least one layer of adhesive containing the adhesion promoter C is then applied, preferably by coating on the crosslinked silicone film;

f. then finally the outer cover is placed.

According to this process, an aqueous silicone dispersion is used making it possible to obtain a sealing membrane which gives the surface coatings water resistance, only three hours after its application.

In addition, the waterproof silicone membrane which is produced in this process according to the invention has mechanical properties which are clearly superior to the organic waterproofing membranes (eg acrylic) encountered in known systems and requiring the use of reinforcing layers. , the installation of which consumes time.

The method according to the invention also has the great advantage of significantly reducing the duration of the production of waterproof surface coatings and of reducing the number of operating phases.

Another advantage linked to the use, in the process according to the invention, of silicone elastomer membranes for sealing, lies in the fact that these silicone elastomer membranes form a waterproof barrier but are permeable to air, which makes it possible to limit the proliferation of molds.

CA 02452306 2003-12-23 WO 03/002677 PCT / FR02 / 02286 6 It is particularly advantageous to have in addition drying times and therefore particularly short process times, since the surface coatings concerned are at the same time. 'exterior (terrace).

In addition, the method according to the invention makes it possible to have good adhesion on wet surfaces.

In this process, silicone products are also used which respect the environment and allow easy removal, by washing with water, of the soiling made on the tools used for the application.

Finally, taking into account the elasticity provided by the silicone sealing membrane, it is possible to implement the method according to the invention on surfaces liable to undergo small movements.

The fact of using at least one adhesion promoter C 'in the adhesive is an important provision of the invention, which makes it possible to make this adhesive compatible with the waterproof silicone membrane, which is produced by coating and crosslinking. hardening of the aqueous silicone dispersion.

According to a remarkable characteristic of the invention, the amount of adhesion promoter C 'in the adhesive is less than 20% relative to the total weight of the composition constituting the adhesive, preferably between 0.1 and 15% by weight. , and more preferably still between 0.5 and 10% by weight.

This adhesive for exterior roofing of the tiling type, for example, is advantageously prepared by mixing a powder part and a dispersing liquid, preferably water.

The adhesion promoter It is preferably incorporated into the dispersant liquid, before mixing.

In practice, the adhesive used in the process according to the invention is an adhesive based on cement and a specific binder.

It has great mechanical resistance and flexibility which make it particularly suitable for bonding, for example, ceramic, stone or concrete tiles.

According to a preferred method of the process according to the invention, the glue used has the following composition (in parts by weight in the composition):

= hydraulic cement 100 = mineral binder with organic or inorganic additive (s) 100-300 preferably 170-200 = adhesion promoter (C ') (dry) 1-50 preferably 20-40 = water 20-100 preferably 40-80 CA 02452306 2003-12-23 WO 03/002677 PCT / FR02 / 02286 7 In this composition, the hydraulic cement is advantageously a conventional cement mainly containing calcium silicates Ca2SiO4 and Ca3SiO5 (metastable ).

It may be, for example, Portland cement.

As regards the mineral binder, it comprises at least one compound selected from the group including: siliceous sands, cellulose derivatives, limestone fillers, acrylic resins in dispersion, specific adjuvants and mixtures thereof.

According to a preferred characteristic of the invention, the adhesion promoter CII identical to C.

On a practical level, it can be specified that the glue can be prepared by mixing a powder based on hydraulic cement and mineral binder (with additive (s) organic (s) or inorganic (s)), d 'water and adhesion promoter (C'). Mention will be made, as powder which is suitable, for example, of the mixture marketed by the company BAL under the name BAL-SINGLE PART FLEXIBLE.

On the practical level also, it can be specified that very advantageously, the preparation of the glue is carried out by mixing 70 to 90% by weight of powder, 5 to 20% by weight of water and 2 10% by weight of adhesion promoter (% by weight relative to the total mass of the composition comprising the powder, water and the dry promoter).

Qualitatively, the adhesion promoter C and / or C ′ is a water-soluble compound capable of dissolving in water at a temperature of 25 C to a level of at least 5% by weight and chosen from silanes and / or the hydroxylated and carrier POSs, per molecule of at least one hydroxyl and of at least one hydrophilic anchoring function on the support (Fas), as well as among the mixtures of these products, said Fas functions which are identical or different from one another being, preferably, selected from the group comprising the functions: amino, epoxy, acrylo, methacrylo, ureido, mercapto, thiol, chloroalkyl.

More precisely, the adhesion promoter C or It is advantageously:

= a linear hydroxylated polydiorganosiloxane with D and / or MD siloxyl units and / or a hydroxylated POS resin comprising T and optionally M and / or D and / or Q siloxyl units or even Q and M and / or D siloxyl units and / or T, preferably a resin selected from those of the T (OH), DT (OH), DQ (OH), DT (OH), MQ (OH), MDT (OH), MDQ (OH) type or mixtures of these;

= and / or a functionalized silane having the formula:

(RS) 'Sl (R) 4-, ~ formula in which:

- cest0; 1 or 2 - the R5 radicals, identical or different, correspond to the R3 and R4 radicals of the oil (A) of formula (I) as defined below, CA 02452306 2009-04-30 8 - the R radical corresponds to the OH group polyorganosiloxane oil (A) of formula (I) as defined below.

Preferably, the adhesion promoter C or C ′ is aminopropyltriethoxysilane, aminopropyl-methyldiethoxysilane or glycidoxypropyl-trimethoxysilane.

The siloxyl units M, D, T, Q used in the above description of the adhesion promoter are defined as follows:

- unit M = R 3SiO1 / 2 - unit D = R 2 Si02 / 2 - unit T = R Si03 / 2 - unit Q = SiO4 / 2 The R radicals are identical or different and correspond to a hydrocarbon radical, such as for example a alkyl radical (eg methyl, ethyl, isopropyl, tert-butyl and n-hexyl), hydroxyl, alkenyl (eg vinyl, allyl) or even a Fas function.

The adhesion promoter (C) or (C ') are therefore POSs, silicone resins and / or silanes each carrying at least one hydroxyl group and at least one Fas linked to at least one Si atom. .

Preferably, the Fas are non-salified aminoalkyl groups containing 1 to 6 carbon atoms of general formula:

Roo-N RoiRoa or R00-NH- Roo-NRoiRo2 + Roo = divalent hydrocarbon residue, for example - {CH2) n = R l, R02: corresponding independently to H, CnH2õ + 1 = Free valence: linked to Si As illustration of 'an adhesion promoter (C) in (C') which is suitable, there may be mentioned the POS resin obtained from S-aminopropryltriethoxylsilane hydrolyzed and subjected to "stripping" of the ethanol formed by hydrolysis.

The polyhomocondensed resin obtained is a mixture of oligomers containing from 4 to 10 silicon and comprising units:

T (OH) = R Si (OH) 02i2 T = R Si03 / 2 T (OH) 2 = R Si (OH) 201iZ T (OH) 3 = R Si (OH) 3 CA 02452306 2009-04-30 8a Ces units being respectively present in decreasing quantity and R = NHZ (CH2) 3-.

It is for example an amino T (OH) resin.

In practice, the adhesion promoters C or C ′ are silicone compounds making it possible to modulate the physicochemical properties of the silicone elastomer compositions, obtained after crosslinking of the dispersions used in the process according to the invention.

CA 02452306 2003-12-23 WO 03/002677 PCT / FR02 / 02286 9 Concerning the silicone phase of the dispersion according to step a) of the process of the invention, and in particular the constituent or essential constituents of this silicone phase , namely the oil (A), it is advantageously selected from α, co-hydroxylated oils or functional oils comprising per molecule at least 2 functional groups which can be condensed optionally after hydrolysis.

More precisely still, these oils (A) can be represented by the following generic formula (I):

(R3) a R ~ ~ R3) a (I) III R3- (a + b) S I- O - ~ - S I- O-- ~ n- SI R3- (a + b) ~) b ~) b R4 I 2 R4 formula in which:

- a is 0 or 1 - b is 0 or l - with a + b = 0; 1 or 2 - n a value sufficient to give the polymer of forinule (a) the desired viscosity - the radicals R are the same or different and represent = an OH group with a + b = 2;

= an alkoxy or alkenyloxy group containing from 1 to 10 carbon atoms;

= an aryloxy group containing 6 to 13 carbon atoms;

= an acyloxy group containing 1 to 13 carbon atoms;

= a ketiminoxy group containing 1 to 8 carbon atoms;

= an amino- or amido-functional group containing from 1 to 6 carbon atoms, bonded to silicon by an Si-N bond;

- the radicals R ′ and R2 are identical or different and represent organic aliphatic alkyl or alkenyl groups having from 1 to 10 carbon atoms, aromatic phenyl, said groups being optionally substituted with halogen atoms or cyano groups;

- the radicals R3 and R4 are identical or different and represent aliphatic organic groups alkyl, aminoalkyl, polyaminoalkyl, epoxyalkyl, alkenyl, containing from 1 to 13 carbon atoms, aromatic aryl containing from 6 to 13 carbon atoms;

CA 02452306 2009-04-30 at least 2 condensable functional groups optionally after hydrolysis being present per molecule and preferably at least 80% of the radicals R1 to R4 represent a methyl group.

By way of example of R radicals, there may be mentioned the groups:

= alkoxy such as, for example, methoxy, ethoxy, octyloxy;

= alkenyloxy such as for example vinyloxy, hexenyloxy, isopropenyloxy;

= aryloxy such as for example phenyloxy;

= acyloxy such as for example acetoxy;

= ketiminoxy such as, for example, ON = C (CH3) C2H5;

= aminofunctionals such as, for example, ethylamino, phenylamino;

.

10 amidofunctionals such as, for example, methylacetamido;

Among the aliphatic or aromatic organic radicals mentioned above, there may be mentioned as regards:

= R1, R2: for example methyl, ethyl, octyl, trifluoropropyl, vinyl, phenyl;

= R3, R4: for example methyl, ethyl, octyl, vinyl, allyl, phenyl groups;

- (CH2) 3-NH2; - (CH2) 3-NH- (CH2) 2-NH2;

As concrete examples of units D: R1R2SiO2i2, present in the oil (A), mention may be made of:

(CH3) 2SiO2r2; CH3 (CH2 = CH) SiO2r2; CH3 (C6H5) SiO2r2; (C6H5) 2SiO2 / 2.

As concrete examples of M: RR3R4SiO1i2 units, mention may be made of:

(CH3) 2 (OH) SiOli2 (OCH3) 3SiOli2; [OC (CH3) = CH2] 3SiOli2 [ON = C (CH3)] 3SiOli2; (NH-CH3) 3SiOli2; (NH-CO-CH3) 3SiOli2 It is important to note that a selection of silicone oil A of specific viscosity and nature was used.

Indeed, the dynamic viscosity of the oil (A) (and therefore overall of the silicone phase) is greater than or equal to 10 Pa.s, preferably to 50 Pa.s and more preferably to 70 Pa.s.

This viscosity is an important parameter of the invention.

CA 02452306 2009-04-30 10a All the viscosities referred to in this presentation correspond to a dynamic viscosity quantity at 25 C (called Newtonian), that is to say the dynamic viscosity which is measured in a known manner at a shear rate gradient low enough for the measured viscosity to be independent of the speed gradient (Brookfield viscometer * AFNOR NFT 76106 STANDARD of May 1982).

* (trademark) CA 02452306 2003-12-23 WO 03/002677 PCT / FR02 / 02286 11 Any non-reactive oils (A ') may meet the same definition as that given above for reactive oils (A ), with the difference that they do not include reactive functions.

The oils (A ') therefore cannot chemically crosslink.

They are neutral in this respect and can, for example, act as a diluent and / or as a means for adjusting the rheology.

As examples of oils (A '), mention will be made of polydimethylsiloxane oils having a viscosity at 25 ° C. ranging from 50 to 10,000 mPa.s.

A crosslinking agent (B) is preferably used when the oil (A) is an α, co- (dihydroxy) polydiorganosiloxane polymer.

Many crosslinking agents can be used in amounts depending on their nature; these are well known to those skilled in the art.

By way of example, a list of crosslinking agents will be found below with the corresponding amounts recommended, expressed in parts by weight per 100 parts of oil (A):

= 0.5 to 10 parts of sodium silicate = 0.1 to 15 parts of an alkali metal organosiliconate (European patent EP A-266,729) = 1 to 100 parts of a silsesquioxane resin microemulsion (US patents - A-3,355,406; 3 433 780) = 5 to 100 parts of a low molecular weight reactive silicone resin having alkoxy and acyloxy groups (US -A- 4,554,187) = 5 to 100 parts of a high weight silicone resin insoluble in toluene (EP-A304 719) = 5 to 100 parts of a hydroxylated silicone resin consisting of units of formulas R'3SiO1 / 2 (M) and / or R'2SiO2 / 2 (D), associated with units of formulas R ' Si03 / 2 (T) and / or Si02 (Q), R 'being mainly a C1-C6 alkyl radical, vinyl and trifluoro-3,3,3 propyl and a hydroxyl group content by weight of between 0.1 and 10%.

Among these resins, there may be mentioned very particularly the resins MQ, MDQ, MDT, TD (FRA-2 638 166) = 1 to 20 parts of a silane of formula: (R ") u If X (4-u) formula in which R" is a monovalent organic radical, in particular methyl or vinyl, u is equal to 1 or 0, X is a condensable and / or hydrolyzable organic group of the same definition that the radical R of formula (I) above (alkoxy, alkenyloxy, acyloxy, ketiminoxy, alkylamino, alkylamido silanes described in particular in US-A-3,294,725; US-A-4,584,341; US-A-4 618,642; US-A-4,608,412; USA-4,525,565; EP-A-387,157; ​​EP-A-340,120; EP-A-364,375; FR-A-1,248,826; FR 1023477).

CA 02452306 2003-12-23 WO 03/002677 PCT / FR02 / 02286 12 As examples of crosslinking agent (B), mention may be made of:

- the following alkoxysilanes:

Si (OC2H5) 4; CH3Si (OCH3) 3; CH3Si (OC2H5) 3; (C2H50) 3Si (OCH3);

CH2 = CHSi (OCH3) 3; CH3 (CH2 = CH) Si (OCH3) 2; CH2 = CH (OC2H5) 3;

CH2 = CHSi [ON = C (CH3) C2H5]; CH3Si [ON = C (CH3) 2] 3 CH3Si [-C (CH3) = CH2] 3;

methyltri (N-methylacetamidosilane); methyltris (cyclohexylaminosilane) - or the following products:

a sodium silicate, an alkali metal organosiliconate, a silsesquioxane resin microemulsion, a low molecular weight reactive silicone resin having alkoxy and acyloxy groups, a high mass silicone resin insoluble in toluene, at least one hydroxylated silicone resin having , per molecule, at least two different siloxyl units chosen from those of M, D, T and Q type; at least one being a T or a Q, an alkoxysilane, an alkylaminosilane, an alkylamidosilane; siliconates, silicates, silicas (powder or colloidal).

According to a remarkable arrangement of the invention, the adhesion promoter (C) or (C '), acts as a crosslinking agent alone or in addition to the crosslinking agent (B) The dispersion comprises at least one filler (D ) chosen from:

1) reinforcing siliceous mineral fillers, preferably those chosen from the group comprising: colloidal silica, precipitated silica, combustion silica or mixtures thereof; combustion silica being preferred;

these siliceous powders having a BET specific surface area greater than 50 m2 / g, preferably between 150 and 350 inz / g;

2) semi-reinforcing mineral fillers or conventional fillers, for example those chosen from the group comprising diatomaceous earth, calcium carbonate, crushed quartz, carbon black, titanium dioxide, oxide of aluminum, hydrated alumina, expanded or non-expanded vermiculite, zinc oxide, mica, talc, iron oxide, barium sulfate, slaked lime, etc. ; these semi-reinforcing or stuffing mineral fillers having a particle size generally between 1 and 300 m and a BET surface area of ​​less than 50 mZ / g;

3) organic fillers, preferably constituted by organic copolymers in emulsion and known under the name “latex” or “nanolatex”; these “latex” or “nanolatex” being formed, for example, by aqueous dispersions of particles of polymers resulting from conventional processes of (co) polymerization in emulsion of one or more polymerizable organic monomers, advantageously chosen from:

CA 02452306 2003-12-23 WO 03/002677 PCT / FR02 / 02286 13 - a): alkyl (meth) acrylates in which the alkyl part preferably contains from 1 to 18 carbon atoms, in particular methyl acrylate, ethyl acrylate, propyl acrylate, n- acrylate butyl, isobutyl acrylate, amyl acrylate, lauryl acrylate, isolamyl acrylate, (2 ethyl-2 hexyl) acrylate, octyl acrylate, methacrylate methyl, chloroethyl methacrylate, butyl methacrylate, (3,3-dimethyl butyl) methacrylate, ethyl methacrylate, isobutyl methacrylate, isopropyl methacrylate, phenyl methacrylate, butyl chloroacrylate, methyl chloroacrylate, ethyl chloroacrylate, isopropyl chloroacrylate, cyclohexyl chloroacrylate;

- b): α, (3-ethylenically unsaturated esters of monocarboxylic acids, the acid part of which is non-polymerizable and the unsaturated part of which preferably contains 2 to 14 carbon atoms and the acid part of 2 to 12 carbon atoms, in particularly vinyl acetate, vinyl propionate, vinyl butyrate, alkyl acetate, vinyl versatate (registered trademark for esters of α-branched C9-C11 acids), vinyl laurate , vinyl benzoate, vinyl trimethylacetate, vinyl pivilat and vinyl trichloroacetate;

- c): esters and hemi-esters of polycarboxylic acids (X, (3ethylenically unsaturated having from 4 to 24 carbon atoms, in particular dimethyl, diethyl maleate, methyl and ethyl fumarate, (ethyl2hexyl) fumarate;

- d): vinyl halogens, in particular vinyl chloride, vinyl fluoride, vinylidene chloride, vinylidene fluoride;

- e): vinyl aromatics preferably having at most 24 carbon atoms and chosen in particular from styrene, α-methylstyrene, 4methylstyrene, 2-methylstyrene, 3-methylstyrene, 4-methoxystyrene, 2hydroxymethylstyrene, 4 -ethylstyrene, 4-ethoxystyrene, 3,4dimethylstyrene, 2-clilorostyrene, 3-chlorostyrene, 4-chloro-3methylstyrene, 4-tert-butylstryrene, 4-dichlorostyrene, 2,6dichlorostyrene, 2, 5-difluorostyrene, and 1-vinylnaphthalene;

- f): conjugated aliphatic dienes preferably having from 3 to 12 carbon atoms, in particular 1,3 -butadiene, isoprene and 2-chlorobutadiene;

- g): nitriles (x, (3-ethylenically unsaturated having preferably from 3 to 6 carbon atoms such as acrylonitrile and methacrylonitrile:

at least one of these main monomers a) to g) which can be copolymerized with up to 40% by weight of at least one other monomer of ionic nature, in particular:

CA 02452306 2003-12-23 WO 03/002677 PCT / FR02 / 02286 14 - an a, (3-ethylenically unsaturated carboxylic acid monomer mentioned above including mono and polycarboxylic acids (acrylic, methacrylic, maleic, itaconic, fumaric acid , ...), - an ethylenic monomer comprising secondary, tertiary or quaternized amine groups (vinyl-pyridines, diethyl-aminoethylmethacrylate,.) ~ - a sulfonated ethylenic monomer (vinylsulfonate, styrene-sulfonate, ...), - an ethylenic zwitterionic monomer (sulfopropyl (dimethylamino-propyl) acrylate or of a nonionic nature in particular, - amides of unsaturated carboxylic acids (acrylamide, methacrylainide, etc.), - esters of (meth ) acrylates and polyhydroxypropyl or polyhydroxyethylated alcohols, - vinyl and / or acrylic silanes (such as vinyltrimethoxysilane and vinyltrietlloxysilane);

4) in the case of the use of a siliceous mineral filler, said filler can advantageously be implemented in the form of:

-a) suspension of silica treated with organosilazane in a silicone matrix comprising a reactive linear polyorganosiloxane carrying for example at each chain end a hydroxy group, this suspension being obtained by a process consisting essentially of introducing the organosilazane in the preparation medium: on the one hand before and / or substantially simultaneously with the bringing together of at least part of the silicone matrix used with the particulate filler used, this introduction of the organosilazane taking place with a corresponding organosilazane fraction in a proportion ranging from 8 to 30% by dry weight relative to the silica filler, and on the other hand after this placing in the presence of the filler with all or part of the silicone material; this suspension and its preparation process being described in international patent application WO-A-00/37549;

-b) of aqueous dispersion obtained:

^ by kneading a mixture consisting of:

- 100 parts by weight of a silicone phase cps of dynamic viscosity at 25 C at least equal to 10 Pa.s, preferably at 50 Pa.s and, more preferably still at 70 Pa.s, cps comprising the oil or a mixture of oils (A) already polymerized (s) and optionally at least one of the constituents (B), (C) or (E);

- 0.5-20 parts by weight of at least one einulsifying agent (F), the HLB of said emulsifying agent or of the mixture of emulsifying agents being at least 10;

CA 02452306 2003-12-23 WO 03/002677 PCT / FR02 / 02286 - 0-100 parts by weight of filler (D);

- 2-20 parts by weight of water;

the water / water + surfactant (s) weight ratio being such that the viscosity of the water + surfactant (s) mixture is close to or greater than half that of the silicone phase (cps) ;

for a period of time and under shear conditions sufficient to obtain an “oil-in-water” emulsion with a particle size of the order of 0.1 to 5 micrometers;

^ by optional dilution with water until a dry extract of 25 to 97% is obtained;

^ then by addition:

= of the constituent (s) not present in the silicone phase cps = and / or of 0-100 parts by weight of filler (D);

the filler (D) being at least partly in the form of an aqueous suspension of colloidal silica which is introduced in full into the mixing chamber before obtaining the emulsion;

5) in the case of the example: of a non-siliceous mineral filler, said filler can advantageously be used in the form of a dispersion obtained:

= by making an emulsion by kneading a mixture consisting of:

. 100 parts by weight of a silicone phase (cps) of dynamic viscosity at C at least equal to 10 Pa.s, preferably at 50 Pa.s and, more preferably still at 70 Pa.s, cps comprising oil or a mixture of oils (A) already polymerized (s) and optionally at least one of the constituents (B), (C) or (E);

25 . 0.5-20 parts by weight of at least one emulsifying agent (F), the HLB of said emulsifying agent or mixture of emulsifying agents being at least 10;

. 0-100 parts by weight of filler (D);

. 2-20 parts by weight of water;

the water / water + surfactant (s) weight ratio being such that the viscosity of the water + surfactant (s) mixture is close to or greater than half that of the silicone phase (c) s );

for a period of time and under shear conditions sufficient to obtain an “oil-in-water” emulsion with a particle size of the order of 0.1 to 5 micrometers;

= by optional dilution with water until a dry extract of 25 to 97% is obtained;

= then by addition:

CA 02452306 2003-12-23 WO 03/002677 PCT / FR02 / 02286 16 = of the constituent (s) not present (s) in the silicone phase (cps) = and / or of 0-100 parts by weight of filler (D);

said filler (D) being introduced, in the process for obtaining the dispersion, in the form of an aqueous suspension (s) of at least one hydrophilic compound, with the condition that, in the case where the filler (D ) provided in the process for obtaining the dispersion, is at least partly constituted by at least one aqueous suspension of organic (co) polymer (s), then at least part of this (or these) aqueous suspension (s) of filler (D) is (are) introduced into the mixing chamber before obtaining the emulsion 6) and the mixtures of fillers (D) of type 1 / or type 2) defined above, type 1) and type 3) defined above or even type 2) and type 3) defined above.

Preferably, the fillers (D) are chosen from the group comprising:

- precipitated silica, combustion silica, carbonates and their mixtures;

- colloidal silica;

- aqueous suspensions of silica ("Slurry").

According to one variant, these dispersions used in the context of the invention may comprise, in addition to the hydrophilic filler (D) provided in the form of an aqueous suspension, a filler (D ') which is involved in the process for obtaining the. dispersion, in powder form.

This filler (D ') brought into powder in the mixture leading to the dispersion is distinguished from the dry hydrophilic filler (D), through its specific surface area Ss (m2 / g) which is reduced, namely:

Ss <5, preferably Ss <3 As examples of pulverulent fillers (D '), mention may be made of: CaCO3, Si02, Ti02, A1203 / H2O.

Advantageously, the filler (D ') can represent 5 to 100 parts by dry weight per 100 parts by weight of cps silicone phase.

The "oil in water" emulsion of the silicone phase is carried out:

- By introducing silicone oil (A) into a mixture of water and / or aqueous suspension (s) of filler (D) + emulsifying agent (s) (F);

- or by introducing water and / or aqueous suspension (s) of filler (D) in a silicone phase mixture (cps) + emulsifying agent (s) (F) and kneading at a temperature of around 10 to 50 C.

CA 02452306 2003-12-23 WO 03/002677 PCT / FR02 / 02286 17 The viscosity of the aqueous silicone dispersion used in the context of the process according to the invention is between 0.1 and 1000 Pa.s, from preferably between 10 and 100 Pa.s.

These fillers (D) are introduced into the einulsion in the form of a dry powder or in the form of an aqueous dispersion, for example, by simple mixing.

Catalytic curing compounds (E) are well known to those skilled in the art; these are the salts of carboxylic acids and the halides of metals such as, for example, lead, zinc, zirconium, titanium, iron, barium, calcium, manganese and very particularly tin.

We can cite :

= reaction products of tin dicarboxylates and ethyl polysilicate (US-A-3,862,919), = reaction products of dibutyltin diacetate and an alkyl silicate or an alkyltrialkoxysilane (BE -A - 842 305), = tin bischelates (EP - A-147 323; 235 049), = diorgano tin dicarboxylates (GB -A-1 289 900).

They can be used in amounts which can range up to approximately 3 parts by weight, preferably close to 0.05 to 1 part by weight per 100 parts of oil (A).

As regards the emulsifiers (F), they can be ionic or non-ionic surfactants or water-soluble polymers.

Preferably, they are nonionic surfactants. By way of examples, mention may be made of alkoxylated fatty acids, polyalkoxylated alkylphenols, polyalkoxylated fatty alcohols, polyalkoxylated or polyglycerolated fatty amides, polyglycerolated alcohols and alphadiols, block polymers of ethylene oxide-propylene oxide as well as alkylglucosides, alkylpolyglucosides, sucroethers, sucroesters, sucroglycerides, sorbitan esters and ethoxylated compounds of these sugar derivatives.

According to one variant, the emulsifiers (F) are selected from anionic surfactants such as, for example, alkylbenzenesulphonates, alkylsulphates, alkylethersulphates, alkylarylethersulphates, dioctylsulphosuccinates, of alkali metals.

The (The mixture of) emulsifier (s) is chosen according to the nature of the silicone oil (A) to be emulsified; an HLB of the order of 11 to 15 is generally chosen to emulsify a silicone oil (A) consisting of an a, cobis (hydroxy) polydimethylsiloxane polymer.

The water / water + emulsifier (s) (F) weight ratio depends on the viscosity of the silicone phase (cps) and on the nature of the (mixture of) surfactant (s); this ratio is for example of the order of 20/100 to 70/100, preferably of the order of 25/100 to 60/100 to stabilize an emulsion of a silicone phase consisting of an α, co-dihydroxylated oil of viscosity CA 02452306 2003-12-23 WO 03/002677 PCT / FR02 / 02286 18 of the order of 30 to 500 Pa.s, using a nonylphenol having 9 or 10 ethoxy units as the sole emulsifying agent (F) .

As regards the other functional additives (G) capable of being used, these are in particular plasticizers and / or salts and / or thickening agents and / or fillers dispersing agents, the latter preferably being selected from the group of products with anionic hydrophilic function (s) and more preferably still from the group comprising polyacrylates and / or (poly) phosphates.

These additives (G) can also or more precisely be:

= plasticizers such as, for example, polydimethylsiloxane oils with a viscosity of the order of 300 to 10,000 mPa.s., dioctylphthalates, dialkylbenzenes optionally in aqueous emulsion, in amounts of 0 to 70 parts by weight per 100 parts by weight of oil (A);

= thickening agents such as water-soluble polymers with a molecular mass greater than 10,000 g./mole, such as, for example, alkali metal polyacrylates, polyvinyl alcohols, polyethylene glycols, polyvinylpyrrolidones, carrageenans, alginates, methylcelluloses, hydroxyalkylcelluloses, xanthan gum in amounts which can range up to 10% by weight of the final aqueous dispersion;

= agents dispersing fillers such as, for example, polyacrylates of alkali metals with a molecular mass of less than 5,000, inorganic phosphates in amounts which may range up to 10% by weight of the final aqueous dispersion;

= optionally inorganic or organic pigments in an amount of less than 4%, preferably 2% by weight relative to the total mass of the dispersion.

These additives (G) can be introduced either into the silicone phase before it is emulsified, or into the emulsion before dilution.

The aqueous silicone dispersion (A / B / C / D / E / F / G / H) used in the process according to the invention can, for example, be that described in FR-A-2 753 708 ( = WO-A-98/13410).

After having detailed the characteristics of the adhesive and of the aqueous silicone dispersion used in the process according to the invention, it will be specified that the outer coating is advantageously chosen from tiles, preferably from clay-based tiles, terracotta, white quartz, inorganic resin additives (binder of marble powder, cement, sand, sandstone, earthenware and / or pigments).

CA 02452306 2009-04-30 19 On a remarkable characteristic of the invention, and taking into account the interesting performances of the surface coating produced according to the invention, it is possible to envisage that the superposition of layers constituting the coating does not include primers, as long as the surface to be coated is made of wood.

If the primer proves necessary, it is preferably chosen from the group: polysiloxane resins, amino organosilanes, organosilanes with an epoxy function, organosilanes with an isocyanurate function or organosilanes with an acrylate function or mixtures of organosilanes with polyacrylates , or mixtures thereof, the products of the above-defined group being in solution in solvents such as toluene, butanol or glycol ether.

A suitable primer consists, for example, of a solution of polymethylsiloxane resin in toluene sold by WITCO under the name SILQUEST * AP 134.

According to another of its aspects, the present invention relates to an adhesive for waterproof surface coating of buildings (floor / wall / ceiling), capable of being used for the implementation as described above, this adhesive being characterized by that it is based on cement and on a binder and further comprises at least one adhesion promoter C ′, also defined above.

For more details on the other characteristics of the adhesive according to the invention, reference will be made to the description of the adhesive given above with reference to the process according to the invention.

In practice, the adhesive according to the invention is intended for exterior covers, for example of the tiling type, fixed to one or more polymeric sealing membranes.

The mixing of these ingredients is carried out using any suitable means of homogenization, eg: single or multiple screw extruder, planetary mixer, hook mixer, slow disperser, static mixer, paddle mixer, propeller, arm mixer or at anchor.

Advantageously, the mixture of cement, water and the adhesion promoter is carried out just before application.

* (trademark) CA 02452306 2009-04-30 In practice, the general methodology is as follows:

- the surface of the support to be coated is made smooth and dust-free, - the surface is optionally coated with a primer solution, - allowed to dry for several tens of minutes, - the aqueous silicone dispersion is deposited using a brush, to form a film, with a deposition rate of 200 to 2000 g / m2, preferably 600 to 1000 g / m2, - the crosslinking / curing is allowed to take place for several hours at room temperature, - we prepare the tile adhesive with adhesion promoter C ', - we spread the layer of adhesive with the adhesion promoter C' on the silicone elastomer waterproofing membrane, and - the outer covering is applied , that is to say for example the tiles, on the adhesive layer.

According to yet another of its objects, the present invention relates to a ready-to-use kit for implementing the method as defined above.

This kit includes in particular:

= optionally at least one composition of adhesion primer, = at least one aqueous dispersion of silicone oil (s) coinprenant:

-A- 100 parts by weight of at least one organopolysiloxane oil (A) having a viscosity greater than or equal to 10 Pa.s. and capable of crosslinking by condensation, if necessary in the presence of a crosslinking agent (B), into an elastomer;

-A'- optionally up to 30 parts by weight of at least one non-reactive organopolysiloxane oil;

-B- if necessary from 0.1 to 100 parts by weight of at least one crosslinking agent (B);

-C- optionally, up to 50 parts by weight of at least one adhesion promoter (C);

-D- up to 200 parts by dry weight of a filler (D);

CA 02452306 2009-04-30 21 -E- a catalytically effective amount of a catalytic curing compound (E) which can range up to 3 parts by weight;

-F- at least one emulsifier (F);

-G- optionally at least one functional additive (G);

-H- and water;

said dispersion making it possible to obtain, after coating on a support and crosslinking, a waterproof membrane;

= at least one adhesive based on cement, binder and at least one adhesion promoter (C ') as defined above = and optionally at least one outer covering.

The outer covering, that is to say for example the tiles, may or may not form part of the kit according to the invention.

This kit, which includes at least the products making it possible to make the surface coating adhere and make it watertight, is in the form of a packaging bringing together in a single commercial unit these elements making it possible to produce the surface coating. waterproof.

According to one variant, the products for implementing the method according to the invention could be packaged and sold separately.

The invention also relates to the use of:

- an aqueous dispersion of silicone oil comprising:

-A- 100 parts by weight of at least one organopolysiloxane oil (A) having a viscosity greater than or equal to 10 Pa.s. and capable of crosslinking by condensation, if necessary in the presence of a crosslinking agent (B), into an elastomer;

-A'- optionally up to 30 parts by weight of at least one unreactive organopolysiloxane oil;

-B- if necessary, from 0.1 to 100 parts by weight of at least one crosslinking agent (B);

CA 02452306 2009-04-30 22 -C- optionally, up to 50 parts by weight of at least one adhesion promoter (C);

-D- up to 200 parts by dry weight of a filler (D);

-E- a catalytically effective amount of a catalytic curing compound (E) of up to 3 parts by weight;

-F- at least one emulsifier (F);

-G- optionally at least one functional additive (G);

-H- and water;

and an adhesive for the outer covering (for example tiles) based on cement and binder and further comprising at least one adhesion promoter C ′ as defined above;

for producing a waterproof surface coating for buildings (floor / wall / ceiling), said coating consisting of a superposition comprising, from the surface to be coated:

- ~ optionally at least one layer of adhesion primer, ~ at least one waterproof polymer membrane, - ~ (optionally at least one web of fibrous material, woven or not), - ~ at least one layer of glue, - ~ at least one outer cover.

The adhesive for tiling and the aqueous silicone dispersion making it possible to obtain the waterproof silicone elastomer membrane are as defined in the above description.

Thanks to the operating methods and the products offered in accordance with the invention, the production of a waterproof surface coating can be carried out quickly, easily and with a guarantee of good adhesion and of maintaining the seal over time, without involving ecotoxicity and allowing easy washing with water of the tools used for the application.

The latter can moreover be envisaged even in the presence of water appearing only three hours after the coating of the waterproof elastomeric silicone film during curing / crosslinking.

CA 02452306 2009-04-30 23 The invention will be better understood and its advantages will emerge from the examples which follow and which describe the preparation of the aqueous silicone dispersion used in the process to obtain the waterproof silicone elastomer membrane.

These examples also show a concrete case of producing a waterproof surface coating using the above-mentioned aqueous silicone dispersion of an adhesive added with an adhesion promoter and of an exterior covering of the tiling type.

Example 1:

Preparation of a crosslinkable aqueous silicone dispersion (ABCDEFGH) and obtaining a waterproof silicone elastomer membrane using this dispersion.

In an anchor mixer of 21, are charged -A- 347.7 g of α, co-hydroxylated polydimethylsiloxane oil with a viscosity of 135,000 mPa.s, -A ′-26.2 g of polydimethylsiloxane oil blocked by methyl groups with a viscosity of 100 mPa. s, -B- 3.7g of hydroxylated MDT resin with a viscosity of 1000 mPa.s (containing 0.5% by weight of hydroxyl groups, 62% by weight of trifunctional units, 24% by weight of di-functional units and 14% by weight of mono units functional), -F- 26.4 g of .Rhodasurf * ROX (85% aqueous solution of a polyethoxylated C13 aliphatic alcohol containing approximately 8 oxyethyl units) and -H- 7.9 g of demineralized water.

Mixing at 100 rpm until a fine O / W emulsion is obtained (average diameter 0.6 m).

Diluted with -H- 8.2 g of demineralized water and then added, with stirring at 100 rpm, D- 7.9 g of precolor pigment V5639 marketed by Wünsiedel predispersed in 9 g of sodium polyacrylate - dispersant marketed by Coatex under the name Coatex * P50 or by Protex under the name Prox A11 - and -C- 24.3 g of an aqueous solution at 77% by weight of a T (OH) resin aminated with aminopropyl groups marketed by WITCO under the name VS 142.

In the mixture thus obtained -D- 186.9 g of combustion carbonate marketed by OMYA under the name BLR3 and 186.9 g of carbonate from * (trademarks) CA 02452306 2009-04-30 23a are dispersed precipitation marketed by SOLVAY under the name Socal * 312, with stirring at 100 rpm.

Finally, we introduce -G- 0.4 g of antifungal then -H- 9 g of demineralized water and -E- 1.2 g of a solution at 60% by weight of dioctyltin dilaurate, and mixing under vacuum (4600 Pa) under moderate agitation of 100 rpm.

The dry extract of such a formula is 79%.

A film is prepared using a 2.5mm doctor blade which is filled with the desired product.

This method makes it possible to obtain a film 2 mm thick (+/- 0.3).

The product is left to crosslink for 7 days at 23 ° C. and 50% relative humidity.

The mechanical properties obtained on this 2 mm film under such conditions are as follows:

TABLE I Acrylic meinbrane BAL-WP1 elastomeric membrane of the silicone art used in the prior invention Breaking strength (MPa) 0.25 0.65 (standard NF T 46-002) Elongation at break (%) 90 560 (standard NF T 46-002) 100% modulus (MPa) 0.20 0.32 (standard NF T 46-002) Shore A hardness 38 20 (standard NF T 51-109 The silicone elastomer membrane according to the invention has mechanical properties clearly superior to the membrane acrylic sealant marketed by the BAL Company under the name BAL-WP 1 according to the prior art.

Example 2:

In an anchor mixer of 21, are charged -A- 348.8 g of a, ù) hydroxylated polydimethylsiloxane oil with a viscosity of 135000 mPa.s, -A'- 26.3 g of polydimethylsiloxane oil blocked by methyl groups with a viscosity of 100 mPa .s, -B- 3.8 g of MDT * resin (trademarks) CA 02452306 2009-04-30 23b hydroxylated with a viscosity of 1000 niPa.s (containing 0.5% of hydroxyl groups, 60% of trifunctional units, 25% of units difunctional and 15% mono functional units), -F- 26.4 g of Rhodasurf ROX (85% aqueous solution of a polyethoxylated C13 aliphatic alcohol containing approximately 8 oxyethyl units and -H- 7.9 g of demineralized water).

CA 02452306 2003-12-23 WO 03/002677 PCT / FR02 / 02286 24 Mixing at 100 rpm until a fine O / W emulsion is obtained (average diameter: 9 0.6 m).

Diluted with -H- 8.25 g of demineralized water and then added, with stirring at 100 rev / min, -D- 4.9 g of precolor pigment V5672 marketed by Wünsiedel predispersed in 9 g of sodium polyacrylate - dispersant, marketed by Coatex under the name Coatex P50 or by Protex under the name Prox A11 - and -C- 24.4 g of an aqueous solution at 77% by weight of a T (OH) resin aminated with aminopropyl groups marketed by WITCO under the name VS 142.

-D- 187.5 g of combustion carbonate marketed by OMYA under the name BLR3 and 187.5 g of precipitated carbonate marketed by SOLVAY under the name Socal 312, with stirring at 100 rev / min.

Finally, one introduces -G- 0.4 g of antifungal then -H- 9 g of demineralized water and -E- 1.2 g of a 60% solution of dioctyltin dilaurate, and mixing under vacuum (46 mbar) under moderate agitation of 100 rpm.

The dry extract of such a formula is 79%.

The mechanical properties obtained on a 2 mm film of this product under the same conditions as Example 1 are as follows:

TABLE II Silicone elastomer membrane used in the invention Tensile strength (MPa) 0.63 (standard NF T 46-002) Elongation at break (%) 550 (standard NF T 46-002) Modulus at 100% (MPa) 0.34 (NF T 46-002 standard) Shore A 22 hardness (NF T 51-109 standard) Example 3:

About 0.1 g of an adhesion primer consisting of a solution of polymethylsiloxane resin in toluene sold by WITCO under the name Silquest AP 134 is applied to a concrete plate of dimensions 75x50x20 mm using a brush.

After drying for 30 minutes, the aqueous silicone dispersion prepared in Example 1 is deposited using a brush.

The consumption, per layer, can CA 02452306 2003-12-23 WO 03/002677 PCT / FR02 / 02286 vary from 600 to 1000 g / m2 depending on the porosity, the roughness of the support and depending on the nature of the parts to be treated.

In this case, the deposition rate is 800 g / m2.

It is left to dry for 24 hours in an environment at 23 ° C. and 50% relative humidity, then the tile adhesive is applied with an 8% addition of an adhesion promoter (C) consisting of an aqueous solution at 77% by weight. of a T (OH) resin aminated by aminopropyl groups marketed by WITCO under the name VS 142 on which the tile of dimensions 50x50 mm is deposited.

Preparation and application of the glue:

In 100 g of base for glue marketed by the company BAL under the name BAL-SINGLE PART FLEXIBLE, 10 g of an aqueous solution at 77% by weight of a T (OH) resin aminated by aminopropyl groups marketed by WITCO under the name VS 142 and 8 g of water.

A layer of approximately 2 to 6 mm of glue is deposited using a spatula (notched or not), which represents 5 to 6 kg / m2.

15 The whole is left to dry for 48 hours in a room conditioned at 23 ° C. and 50% relative humidity, then the tear-off force of the tile is measured.

To do this, a dynamometer is used having jaws capable of holding specimens of such dimensions.

An anodized aluminum plate is glued to the tiling so as to be able to impose a tensile force on the system.

The traction speed is 5.5mm / min 20 (according to ISO 8339).

The measured force is 0.6Mpa, greater than the required force of 0.5 MPa.

Example 4:

About 0.1 g of an adhesion primer consisting of a solution of polymethylsiloxane resin in toluene sold by WITCO under the name Silquest AP 134 is applied to a concrete plate of dimensions 75x50x20 mm using a brush.

After drying for 30 minutes, the aqueous silicone dispersion prepared in Example 1 is deposited using a brush.

The consumption, per layer, can vary from 600 to 1000 g / m 2 depending on the porosity, the roughness of the support and depending on the nature of the parts to be treated.

In this case, the deposition rate is 800 g / m2.

It is left to dry for 24 hours in an environment at 23 ° C. and 50% relative humidity.

This system is placed under a water column 220 mm high and 10 mm in diameter for 5 days.

The movement of the water level in the column is observed after this conditioning.

The water level in the column did not drop in 5 days; this means that the polymer membrane offers a good seal.