EP3464213A1 - Use of plaster for manufacturing a self-leveling underlayment for hot countries - Google Patents

Use of plaster for manufacturing a self-leveling underlayment for hot countries

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Publication number
EP3464213A1
EP3464213A1 EP17724382.1A EP17724382A EP3464213A1 EP 3464213 A1 EP3464213 A1 EP 3464213A1 EP 17724382 A EP17724382 A EP 17724382A EP 3464213 A1 EP3464213 A1 EP 3464213A1
Authority
EP
European Patent Office
Prior art keywords
plaster
weight
use according
superplasticizer
screed
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP17724382.1A
Other languages
German (de)
French (fr)
Inventor
Alain Jacquet
Laurence Martin
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Holcim Technology Ltd
Original Assignee
Holcim Technology Ltd
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 Holcim Technology Ltd filed Critical Holcim Technology Ltd
Publication of EP3464213A1 publication Critical patent/EP3464213A1/en
Withdrawn legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/14—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements
    • C04B28/145—Calcium sulfate hemi-hydrate with a specific crystal form
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/60—Flooring materials
    • C04B2111/62—Self-levelling compositions
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/76—Use at unusual temperatures, e.g. sub-zero
    • C04B2111/763—High temperatures

Definitions

  • the present invention relates to the use of plaster for the manufacture of a fluid screed castable at temperatures greater than or equal to 30 ° C.
  • a screed is a layer of mortar made from hydraulic binder, sand, water and possibly adjuvant.
  • a screed is intended to level, level even uneven support and / or coat elements and then receive the floor covering.
  • a hydraulic binder is a material that picks up and hardens by hydration
  • Plaster usually used in the building industry, comes mainly from the calcination of gypsum, calcination which can lead to anhydrite if the temperature is high enough that the dehydration of the gypsum is total.
  • plasters and anhydrites calcium sulphate hemihydrate (plaster), calcium sulfate hemihydrate ⁇ (plaster), anhydrite I, anhydrite II and anhydrite III.
  • the type of compound formed depends on the calcination method used and the calcination temperature of the gypsum.
  • Calcium sulphate hemihydrate comes mainly from natural gypsum or sources of synthetic gypsum (phospho-gypsum, titano-gypsum, citro-gypsum, FGD (Flue Gas Desulphurization) gypsum or desulfogypsum).
  • Anhydrite can be obtained by calcination. It can be as natural (rock that must be ground before use) or synthetic (example: by-product during the manufacture of hydrofluoric acid). These compounds can be made with water by turning into gypsum.
  • Plaster or anhydrite is used in the building industry as a binder, particularly for the production of fluid screeds.
  • the anhydrite screed or calcium sulphate screed is well known to those skilled in the art. It is a mortar (mixture of sand, anhydride and adjuvant) fluid based on a binder based on calcium sulphate, whether or not fired, usually prepared in a production plant (concrete plants most often) for the realization of self-leveling screeds, and delivered on site by mixer truck or delivered directly on site by a transmix type distribution system.
  • Anhydrite screed materials are the subject of EN 13454-1 and EN 13813.
  • anhydrite is generally preferred, in particular type II anhydrite, so-called “non-so-so", in order to allow the rheological properties of the anhydrite-based self-sealing mortar to be preserved during its transport, from the site of manufacture at the emplacement site, and not water-soluble semi-hydrates or unstable type III anhydrites, rapidly transforming into semi-hydrates.
  • the screed must be fluid in the fresh state, which gives it a self-compacting character.
  • hot weather that is to say temperatures of 30 ° C or higher
  • the workability of cement-based screeds is difficult to manage in practice: the high temperature accelerates the hydration reactions. results in a reduction of setting times and a rapid degradation of the rheology of the screed.
  • Portland cement-based screeds often have problems with surface cracking and drying, exacerbated when the temperature is high.
  • the conventional anhydrite-based screeds are not usable when the temperature is higher than about 30 ° C because beyond this temperature, the kinetics of hydration (if the latter takes place) is so slow that the resistances reached at 28 days are very insufficient.
  • the object of the invention is to develop a screed which can be used at temperatures above 30 ° C. and which has the technical advantages of conventional anhydrite screeds:
  • plaster that is to say calcium sulfate hemihydrate, in its crystalline form ⁇ , as a hydraulic binder, allows the manufacture of screeds usable in time.
  • the characteristics of classic anhydrite screeds are expected to be warm: good workability, self-compacting, easy finishing and mechanical strength after hardening.
  • DE 20 2007 003 608 discloses a plaster based screed in its crystalline form which can be cast at a temperature of 0 ° C to 35 ° C.
  • a plaster based screed in its crystalline form which can be cast at a temperature of 0 ° C to 35 ° C.
  • the demand for admixtures, in particular for water reducing agents is less and thus the screed according to the invention is significantly more economical.
  • the invention thus relates to the use of plaster, in its crystalline form ⁇ , for the preparation of a floor screed composition, also comprising sand and a superplasticizer, intended to be cast at a temperature greater than or equal to 30 ° C.
  • the plaster-based screeds according to the invention can thus be used in hot countries, where the ambient temperature is greater than 30 ° C., possibly greater than 35 ° C., or even greater than 40 ° C.
  • adjuvant any compound that incorporated into a formulation allows to provide particular properties.
  • binder is meant according to the present invention any compound having the property of providing cohesion to the formulation in which it is incorporated, and makes it possible to provide mechanical characteristics to said formulation (for example compressive strength , in traction, adhesion).
  • This binder may also be intended to bind inert elements such as aggregates.
  • hydraulic binder is meant according to the present invention any compound having the property of hydrating in the presence of water and whose hydration makes it possible to obtain a solid having mechanical characteristics.
  • hydraulic binder also refers to water binders.
  • the hydraulic binder according to the invention is a binder based on plaster.
  • plaster also called calcium sulfate hemihydrate or hemi-hydrated calcium sulfate, of chemical formula CaSO 4 * 0.5 H 2 O, in which the crystalline form ⁇ is predominant in mass.
  • mass content is less than 5%, relative to the total weight of crystalline forms a and ⁇ , preferably less than 2%, preferably less than 1%.
  • the invention relates to the use of plaster, in its crystalline form ⁇ , for the preparation of a floor screed composition, also comprising sand and a superplasticizer, intended to be cast at a temperature greater than or equal to 30 ° C.
  • the floor screed according to the invention may be cast at a temperature greater than or equal to 30 ° C, at a temperature greater than or equal to 35 ° C, or even at a temperature greater than or equal to 40 ° C.
  • the invention is characterized by the use, as a hydraulic binder, of plaster in its crystalline form ⁇ .
  • This plaster also called calcium sulphate hemihydrate or calcium sulphate hemihydrate, chemical formula CaSO 4 * 0.5H 2 O, can exist in two crystalline forms: the form a or the form ⁇ .
  • the two crystalline forms can be used for the preparation of screeds, the ⁇ form however giving better quality screeds and especially for a lower financial cost.
  • the composition may comprise as hydraulic binder only plaster or a mixture of plaster and filler.
  • the hydraulic binder comprises at least 52% by weight of plaster and from 0% to 48% by weight, the sum of these two percentages varying from 80% to 100%.
  • the sum of these two percentages advantageously varies from 85% to 100%, more preferably from 90% to 100%, even more preferably from 95% to 100%).
  • the plaster being most often of natural origin, it is difficult to obtain a raw material comprising exclusively calcium sulphate semi-hydrate.
  • the plaster may comprise impurities such as quartz (Si0 2 ), celestine (SrS0 4 ), carbonate phases such as calcite (CaCO 3 ), dolomite (CaMg (CO 3 ) 2 ), clay or feldspathic phases such as chlorite ((Mg, Al) 6 (Si, Al) 4 O 10 (OH) 8 ), microcline (K (Si 0 , 75 Al 0 , 25 ) 4 O 8 ), phlogopite (KMg 2 , 75 Si 3 , 5 A 10, 5 OioF 2), kaolinite (Al 2 Si 2 0 5 (OH) 4), albite (Na (AlSi 3 O), muscovite (KAl 3 Si 3 Oio (OH) 2).
  • impurities such as quartz (Si0 2 ), celestine (SrS0 4 ), carbonate phases such as calcite (CaCO 3 ), dolomite (CaMg (CO 3
  • the plaster comprises less 5%) by weight, more preferably less than 2% by weight, based on the total weight of the plaster, impurities.
  • the plaster may also include gypsum or anhydrite. A plaster with the smallest possible amounts of gypsum or anhydrite will be used.
  • the plaster comprises less than 5% by weight, more preferably less than 2% by weight, and even more advantageously less than 1% by weight, relative to the total weight of plaster, of gypsum.
  • the plaster comprises less than 5% by weight, more preferably less than 2% by weight, and even more advantageously less than 1% by weight, based on the total weight of the plaster, of anhydrite.
  • the plaster comprises less than 5% by weight, more preferably less than 2% by weight, and even more advantageously less than 1% by weight, based on the total weight of the plaster, of plaster in its crystalline form a.
  • the particle size and the specific surface area of the plaster is not critical in the invention.
  • Fillers (filler) of different kinds limestone, siliceous, fly ash, silica fume can be used in addition to plaster.
  • Replacing part of the plaster with a load reduces the cost of raw materials. Such a replacement also makes it possible to reduce the mechanical strengths when they are greater than the target. Such a replacement also makes it possible to reduce the quantities by superplasticizer.
  • the load will be inert or will have a low reactivity compared to that of plaster.
  • the filler may be, for example, limestone, ground natural calcium carbonate (eg chalk, calcite, marble or other natural calcium carbonate), precipitated calcium carbonate (also known as calcium carbonate). synthetic calcium), barium carbonate, dolomite, talc, crystalline silica, pyrogenic titanium dioxide, iron oxide, manganese oxide, titanium dioxide, kaolin, clays, mica, calcium sulphate, basalt, barium sulfate, aluminum hydroxide, bauxite, a low reactivity filler such as blast furnace slag, or a mixture thereof. Limestone, ground calcium carbonate and precipitated calcium carbonate are preferred.
  • the pH is adjusted by adding lime (CaO or Ca (OH) 2 ). It is thus possible to add from 0.1 to 0.2% by weight of CaO equivalent, relative to the weight of the plaster.
  • the screed composition according to the invention comprises adjuvants, the purpose of which is to modify the rheological properties of the mortar. Adjuvants will also influence setting time.
  • the adjuvants are added for example either in the mortar, preferably in a water-soluble sachet, or with part of the water, or in the binder, or in several vectors.
  • a superplasticizer is added.
  • a superplasticizing agent is an additive which, by its addition to an aqueous calcium sulphate composition, reduces the water demand and maintains the fluidity / rheology of the dough.
  • Superplasticizers were broadly classified into four groups: sulfonated condensates of naphthalene formaldehyde (SNF) (usually a sodium salt); sulphonated condensates of melamine formaldehyde (SMF); modified lignosulfonates (MLS); And the others. More recent superplasticizers include polycarboxylic compounds such as polycarboxylates, for example polyacrylates. Acrylic copolymer superplasticizers can also be used, preferably they are polymers comprising a chain with a possibly salified polycarboxylic function, to which another group (for example of the polycarboxylate or polyoxyethylene type) is attached.
  • SNF naphthalene formaldehyde
  • SMF sulphonated condensates of melamine formaldehyde
  • MLS modified lignosulfonates
  • More recent superplasticizers include polycarboxylic compounds such as polycarboxylates, for example polyacrylates. Acrylic copolymer
  • a superplasticizer is preferably a new generation superplasticizer, for example a copolymer containing a polyethylene glycol as a grafted chain and carboxylic functions in the main chain as a polycarboxylic ether.
  • Polycarboxylates such as polycarboxylate ether (PCE)
  • PCE polycarboxylate ether
  • the superplasticizer is a polycarboxylate, in particular an ether or a polycarboxylate ester.
  • the superplasticizers are polycarboxylates which have at least the following three units which are repeated: an acrylic unit, a methacrylic acid unit and a unit formed of a long chain of polyethers
  • High dispersion efficiency also makes it possible to reduce the amount of superplasticizer used and to have an economic benefit since the carboxylate product is relatively expensive.
  • Sodium polycarboxylate polysulfonates and sodium polyacrylates can also be used. Phosphonic acid derivatives and polycarboxylates having phosphate groups may also be used. Sodium polycarboxylate polysulfonates and sodium polyacrylates may also be used.
  • the amount of superplasticizer is highly dependent on the nature of the superplasticizer and its dilution; however, 100% solids content will be given.
  • the superplasticizing agent (expressed as dry extract) is generally present in an amount of between 0.01% and 3%, preferably between 0.1% and 2.5%, relative to the weight of the plaster.
  • the superplasticizer is usually added as a powder, but an addition in liquid form is also possible.
  • the addition in liquid form generally allows an automated dosage of additives.
  • the composition also includes a retarder.
  • a retarder One or more set retarders may be used.
  • Such retarders are, for example, carboxylic acids such as citric acid, sugars and their derivatives, polyoxymethylene amino acid calcium salt, degraded polyamides.
  • Delayers are used to obtain a setting time (between the beginning and the end of the shot) that is compatible with the desired application. Viscosifiers and thickeners may also be used, in particular to avoid segregation and / or bleeding.
  • biopolymers such as gums: diutane gum, guar gum, xanthan gum
  • precipitated silica or cellulose derivatives such as methylcellulose, methylhydroxypropylcellulose, hydroxyethylcellulose, carboxymethylcellulose
  • a dye pigment in the mortar for screed, especially at the level of the additive in its bag.
  • the amount of retarder is very dependent on the nature of the retarder and its dilution; however, 100% solids content will be given.
  • the retarding agent (expressed as dry extract) is generally present in an amount of between 0.01% and 3%, preferably between 0.05% and 2%, relative to the weight of plaster.
  • the amount of retarder will also be adjusted according to the ambient temperature: quantity to decrease when the ambient temperature increases.
  • the amount of retarder can be increased with respect to a formula comprising siliceous sand.
  • a formula comprising siliceous sand For example, at 40 ° C., 0.30%> retarder, based on the weight of plaster, with calcareous sand and 0.20%) retarder, based on the weight of plaster, with a siliceous sand can be used. .
  • the retarder is usually added as a powder, but addition in liquid form is also possible.
  • the addition in liquid form generally allows an automated dosage of additives.
  • the composition also comprises an antifoaming agent.
  • antifoaming agent is varied. It may especially be based on silicone, fatty alcohols, esters, polypropylene glycol.
  • the anti-foam agent may be chosen in the following classes:
  • Antifoam based on oil which has an oil as a vehicle.
  • This oil can be mineral, vegetable (except silicone).
  • the antifoam also comprises a wax and / or a hydrophobic silica.
  • waxes are ethylene bis stearamide (EBS), paraffin waxes, ester waxes and waxes based on fatty alcohols. Surfactants may also be present;
  • Antifoam powder These agents correspond to these oil-based agents but on a particulate support such as silica;
  • oils or waxes dispersed in an aqueous base.
  • the oils are white oils or vegetable oils and the waxes are fatty alcohols, fatty acids, esters or soaps thereof;
  • the agent antifoam may be a polydimethylsiloxane. Particularly suitable are silicones comprising (RSiOo, s) and (R 2 SiO) groups. In these formulas, the R radicals, which may be the same or different, are preferably a hydrogen atom or an alkyl group of 1 to 8 carbon atoms, the methyl group being preferred. The number of units is preferably from 30 to 120;
  • Anti-foam glycol type include polyethylene glycol and polypropylene glycol copolymers. They are available on oily or aqueous base or emulsions;
  • the amount of this agent is typically between 0.01% and 5%, preferably 0.11% and 5%, calculated with respect to the solids content of the superplasticizer.
  • the defoamer is usually added as a powder, but addition in liquid form is also possible.
  • the addition in liquid form generally allows an automated dosage of additives.
  • the composition further comprises an adjuvant chosen from setting accelerators, thickening agents, viscosity agents and / or water retenters, air entraining agents, anti-film agents, tracers, hydrophobing agents and coloring agents. and mixtures thereof, in particular viscosifiers and / or thickeners.
  • an adjuvant chosen from setting accelerators, thickening agents, viscosity agents and / or water retenters, air entraining agents, anti-film agents, tracers, hydrophobing agents and coloring agents. and mixtures thereof, in particular viscosifiers and / or thickeners.
  • the amount of water is adjusted to obtain the consistency and the mechanical strengths required for the application of the composition on site.
  • the amount of water is generally capable of being expressed relative to the binder, and the water / binder ratio is generally between 0.27 and 0.70, preferably between 0.35 and 0.70, advantageously between 0, 40 and 0.70.
  • the spreading values of the compositions according to the invention are conventional. In particular, they have a spread of at least 22 cm, preferably at least 24 cm, advantageously at least 25 cm.
  • the screed according to the invention generally meets the requirements of the European standards EN 13454-1 of February 2005 (binder), EN 13813 of June 2003 (mortar), and according to the test methods described in standard NF EN 13454-2 + A1 of September 2007 relating to binders and mortars based on calcium sulphate for fluid screeds.
  • the amount of binder, especially calcium sulphate, in the screed advantageously varies from 400 to 700 kg / m 3 , typically of the order of 650 kg / m 3 .
  • the binder is present in a customary amount, in particular to achieve and maintain the minimum qualities specified in the standards above.
  • the sands which are used in the formulation according to the invention are conventional aggregates in accordance with EN 12620 (sands for concrete).
  • the Dmax is less than 4 mm, and in general the sand has particle sizes substantially between 0 and 4 mm (which are generally referred to as 0-4 sands).
  • Sands include calcareous, siliceous and silico-calcareous materials.
  • the sand can be of different origins, alluvial washed (rolled, semi-crushed or crushed), sands of marine origin, crushed calcareous sand (dry or washed), sands of magmatic origin (porphyry, granite), aggregates of recycling resulting crushing concrete or other building materials
  • inertants are compounds that reduce or prevent the harmful effects of clays on the properties of hydraulic binders. Inerting clays include those described in FR 2 948 1 18, WO 2006/032785 and WO 2006/032786.
  • the sands are sands of calcareous or silico-calcareous nature, more preferably of limestone nature.
  • the screed composition comprises, per cubic meter of composition in the fresh state:
  • the screed composition advantageously comprises from 0.5 to 2.5% of superplasticizer, percentages expressed by weight of dry extract of superplasticizer relative to the weight of the plaster.
  • the screed composition advantageously comprises from 0.05 to 0.2% of retarder, percentages expressed by weight of dry extract of retarder relative to the weight of the plaster.
  • the screed composition advantageously comprises from 0.1 to 0.2% of CaO, percentages expressed by weight of retarder solids relative to the weight of the plaster.
  • the screed composition advantageously comprises from 0.01% to 0.5%, based on the dry extract of the superplasticizer, of an antifoaming agent.
  • the floor screed composition according to the invention has the advantage of being self-placing. It can easily be poured by means of a pump, for example a screw pump or a piston pump.
  • the compressive strengths are measured on cubic test pieces 15 ⁇ 15 ⁇ 15 cm after curing for two days at 20 ° C. and then after drying for several days at 45 ° C. maximum. Drying at 90 ° C in the long term would lead to dehydration of the gypsum and therefore a decrease in mechanical strength, so drying should be recommended at 40-45 ° C until the mass of the test piece is constant.
  • the force applied to the sample is increased at a rate of 3.85 kN / s during the test;
  • the principle of the spreading measurement consists in filling a truncated cone of spreading measurement with the hydraulic composition to be tested and then in releasing said composition from said truncated cone of spreading measurement so as to to determine the disc surface obtained when the hydraulic composition has finished spreading.
  • Viscosity measurement method (flow): The measurement of the viscosity consists in measuring the flow time of the hydraulic composition to be tested through a viscosity measurement truncated cone.
  • the viscosity measuring truncated cone has the following dimensions:
  • the viscosity measurement truncated cone further comprises first and second indicia which may be parallel marks provided on the wall of the truncated cone and defining planes perpendicular to the truncated cone axis.
  • the first mark is closer to the base of larger diameter than the second mark.
  • the distance between the two marks is 60 mm, the first mark being 12 mm from the larger diameter base.
  • the hydration reaction of the semi-hydrates is an exothermic reaction which will cause an increase in the temperature of the screeds. This increase in temperature will be recorded thanks to a TESTO temperature recorder.
  • the graph of the evolution of temperature as a function of time is plotted and the setting time is read at the abscissa where the peak of the curve is maximum.
  • Effective water is the water required for the hydration of a hydraulic binder and the fluidity of a hydraulic composition in the fresh state.
  • Total water represents all of the water present in the mixture (at the time of mixing) and includes the effective water and the water absorbed by the aggregates. Efficient water and its method of calculation are discussed in the EN 206-1 standard of October 2005, page 17, paragraph 3.1.30.
  • the amount of absorbable water is deduced from the absorption coefficient of the aggregates which is measured according to standard NF EN 1097-6 of June 2001 page 6 paragraph 3.6 and the associated appendix B.
  • the water absorption coefficient is the ratio of the mass increase of a sample of aggregates to its dry mass, the sample being initially dry and then immersed for 24 hours in water. The increase in mass is due to the penetration of water into the pores of the aggregates accessible to water.
  • Vinapor antifoam Vinapor ® DF9010, manufactured by BASF
  • PCE239 superplasticizer Melflux PCE239L, manufactured by
  • compositions based on calcareous sand are more economical.
  • the amount of admixture is less important (about 40% decrease) than with siliceous sand.
  • the mechanical strengths are also more important with the calcareous sand.
  • Example 3 Impact of the amount of binder The effect of varying the amount of binder was analyzed by not modifying the amount of water. The results are reported in the following table: 30 ° C
  • PCE 239 (% / plaster) 0.63 0.60 0.57 0.58
  • the sand is a cut 73/27 of sand 0 / 1.6 Cassis and sand 1.6 / 3 Cassis.
  • Plaster is a French plaster, Prestia 2500, crystalline form ⁇ .
  • the decrease in the amount of binder does not change the amount of water increases the ratio Eff / plaster and allows to make screeds that fall within the specifications at the level of rheology while reducing the amount of adjuvant.
  • the reduction in the amount of plaster reduces the mechanical resistance.
  • the formulator may vary the amount of binder by increasing it to increase the mechanical properties or by decreasing it to reduce the mechanical properties.
  • Example 4 Replacement of a part of the plaster with a load
  • the sand is a cut 73/27 of sand 0 / 1.6 Cassis and sand 1.6 / 3 Cassis.
  • Plaster is a French plaster, Prestia 2500, crystalline form ⁇ .
  • pH regulator CaO powder
  • a homogeneous product A self-placing product. Product appearance very correct after pouring. A nice finish after the passage of the "bar”.

Abstract

The invention relates to the use of plaster, in the crystalline β form, for preparing a floor underlayment composition, also comprising sand and superplasticizer, to be cast at a temperature of at least 30°C.

Description

UTILISATION DE PLATRE POUR LA FABRICATION D'UNE CHAPE FLUIDE DESTINEE AUX PAYS CHAUDS  USE OF PLASTER FOR THE MANUFACTURE OF A FLUID CAP FOR HOT COUNTRIES
DOMAINE DE L'INVENTION FIELD OF THE INVENTION
La présente invention concerne l'utilisation de plâtre pour la fabrication d'une chape fluide pouvant être coulée à des températures supérieures ou égales à 30°C.  The present invention relates to the use of plaster for the manufacture of a fluid screed castable at temperatures greater than or equal to 30 ° C.
Une chape est une couche de mortier réalisée à partir de liant hydraulique, de sable, d'eau et éventuellement d'adjuvant. Une chape est destinée à aplanir, niveler un support même irrégulier et/ou enrober des éléments pour ensuite recevoir le revêtement de sol.  A screed is a layer of mortar made from hydraulic binder, sand, water and possibly adjuvant. A screed is intended to level, level even uneven support and / or coat elements and then receive the floor covering.
ETAT DE LA TECHNIQUE STATE OF THE ART
Un liant hydraulique est un matériau qui prend et durcit par hydratation A hydraulic binder is a material that picks up and hardens by hydration
Par les termes suivants, on entend selon la présente invention :  By the following terms is meant according to the present invention:
- Gypse ou sulfate de calcium hydraté : CaS04*2(Fl2C)) ; - Gypsum or hydrated calcium sulphate: CaSO 4 * 2 (Fl 2 C));
- Plâtre ou sulfate de calcium semihydrate ou sulfate de calcium hémihydraté ou sulfate de calcium partiellement anhydre: CaSO4 »0.5H2O ; - Gypsum or calcium sulphate hemihydrate or calcium sulfate hemihydrate or calcium sulfate partially anhydrous: CaSO 4 "0.5H 2 O;
- Sulfate de calcium anhydre ou anhydrite (type II ou type III) ou sulfate de calcium totalement anhydre : CaS04. - Anhydrous or anhydrite calcium sulphate (type II or type III) or totally anhydrous calcium sulphate: CaSO 4 .
Le plâtre, utilisé habituellement dans l'industrie du bâtiment provient principalement de la calcination du gypse, calcination qui peut conduire à l'anhydrite si la température est suffisamment élevée pour que la déshydratation du gypse soit totale. Il existe différents types de plâtres et d'anhydrites : le sulfate de calcium semi-hydrate a (plâtre), le sulfate de calcium semi-hydrate β (plâtre), l'anhydrite I, l'anhydrite II et l'anhydrite III. Le type de composé formé dépend du procédé de calcination mis en œuvre et de la température de calcination du gypse. Plaster, usually used in the building industry, comes mainly from the calcination of gypsum, calcination which can lead to anhydrite if the temperature is high enough that the dehydration of the gypsum is total. There are different types of plasters and anhydrites: calcium sulphate hemihydrate (plaster), calcium sulfate hemihydrate β (plaster), anhydrite I, anhydrite II and anhydrite III. The type of compound formed depends on the calcination method used and the calcination temperature of the gypsum.
Le sulfate de calcium semi-hydrate provient principalement du gypse naturel ou de sources de gypse synthétique (le phospho-gypse, le titano-gypse, le citro-gypse, le gypse FGD (Flue Gas Desulphurisation) ou désulfogypse).  Calcium sulphate hemihydrate comes mainly from natural gypsum or sources of synthetic gypsum (phospho-gypsum, titano-gypsum, citro-gypsum, FGD (Flue Gas Desulphurization) gypsum or desulfogypsum).
L'anhydrite peut être obtenue par calcination. Elle peut être aussi naturelle (roche qui doit être broyée avant utilisation) ou synthétique (exemple : sous-produit lors de la fabrication de l'acide fluorhydrique). Ces composés peuvent faire prise avec l'eau en se transformant en gypse. Anhydrite can be obtained by calcination. It can be as natural (rock that must be ground before use) or synthetic (example: by-product during the manufacture of hydrofluoric acid). These compounds can be made with water by turning into gypsum.
Le plâtre ou l'anhydrite sont utilisés dans l'industrie du bâtiment comme liant, notamment pour la fabrication de chape fluide. Plaster or anhydrite is used in the building industry as a binder, particularly for the production of fluid screeds.
II existe principalement deux types de chapes de sol ; soit à base de ciment Portland, soit à base d'anhydrite.  There are mainly two types of floor screeds; either based on Portland cement or based on anhydrite.
La chape anhydrite ou chape sulfate de calcium est bien connue de l'homme du métier. C'est un mortier (mélange de sable, d'anhydride et d'adjuvant) fluide à base d'un liant base sulfate de calcium, fîbré ou non, généralement préparé en centrale de production (centrales à béton le plus souvent) pour la réalisation de chapes autonivelantes, et livré sur chantier en camion malaxeur ou livré directement sur chantier par un système de distribution type transmix. Les matériaux pour chape anhydrite sont le sujet des normes EN 13454-1 et EN 13813.  The anhydrite screed or calcium sulphate screed is well known to those skilled in the art. It is a mortar (mixture of sand, anhydride and adjuvant) fluid based on a binder based on calcium sulphate, whether or not fired, usually prepared in a production plant (concrete plants most often) for the realization of self-leveling screeds, and delivered on site by mixer truck or delivered directly on site by a transmix type distribution system. Anhydrite screed materials are the subject of EN 13454-1 and EN 13813.
Les principaux avantages de ces mortiers à base anhydrite ou de plâtre, comparés aux mortiers à base de ciment, sont : la faible épaisseur des chapes qu'ils peuvent réaliser, le long maintien de leur rhéologie, leur caractère autonivellant (excellent planéité), leur faible retrait, leur facilité de pompage.  The main advantages of these anhydrite-based or plaster-based mortars, compared to cement-based mortars, are: the small thickness of the screeds they can produce, the long maintenance of their rheology, their self-leveling character (excellent flatness), their low shrinkage, their ease of pumping.
Parmi les avantages mentionnés précédemment, on retiendra notamment qu'en raison de son très faible retrait par rapport à une chape de ciment ou de mortier à base de ciment, la chape plâtre ou anhydrite ne présentera pas de fissuration et l'on peut donc couler des dalles de très grandes surface en une seule opération (plusieurs centaines de mètres carrés).  Among the advantages mentioned above, it should be noted in particular that because of its very small shrinkage compared to a cement screed or cement-based mortar, the plaster or anhydrite screed will not present any cracking and it is therefore possible to sink slabs of very large area in a single operation (several hundred square meters).
En France, ces mortiers plâtre ou anhydrite doivent satisfaire aux exigences mécaniques suivantes :  In France, these plaster or anhydrite mortars must meet the following mechanical requirements:
- Résistance à la compression, Rc, supérieure ou égale à 20 MPa à 28j  - Resistance to compression, Rc, greater than or equal to 20 MPa to 28j
- Résistance à la flexion, Rf, supérieure ou égale à 4 MPa à 28j  - Flexural strength, Rf, greater than or equal to 4 MPa at 28j
Pour la fabrication de chapes, on préfère généralement l'anhydrite, en particulier l'anhydrite de type II dite « non so lubie », afin de permettre une conservation des propriétés rhéologiques du mortier autoplaçant à base d'anhydrite lors de son transport, du site de fabrication au site de mise en place, et non des semi- hydrates solubles dans l'eau ou des anhydrites de type III instables, se transformant rapidement en semi-hydrates. For the production of screeds, anhydrite is generally preferred, in particular type II anhydrite, so-called "non-so-so", in order to allow the rheological properties of the anhydrite-based self-sealing mortar to be preserved during its transport, from the site of manufacture at the emplacement site, and not water-soluble semi-hydrates or unstable type III anhydrites, rapidly transforming into semi-hydrates.
La chape doit être fluide à l'état frais, ce qui lui confère un caractère autoplaçant. Par temps chaud, c'est-à-dire à des températures supérieures ou égales à 30°C, l'ouvrabilité des chapes à base de ciment est difficile à gérer en pratique : la température élevée accélère les réactions d'hydrations, ce qui se traduit par une réduction des temps de prise et une dégradation rapide de la rhéologie de la chape. Par ailleurs, les chapes à base de ciment Portland présentent aussi souvent des problèmes de fissuration et de séchage de surface, exacerbés lorsque la température est élevée. Les chapes conventionnelles à base d'anhydrite ne sont pas utilisables lorsque la température est supérieure à environ 30°C car au-delà de cette température, la cinétique d'hydratation (si cette dernière a lieu) est si lente que les résistances atteintes à 28 jours sont très insuffisantes. The screed must be fluid in the fresh state, which gives it a self-compacting character. In hot weather, that is to say temperatures of 30 ° C or higher, the workability of cement-based screeds is difficult to manage in practice: the high temperature accelerates the hydration reactions. results in a reduction of setting times and a rapid degradation of the rheology of the screed. In addition, Portland cement-based screeds often have problems with surface cracking and drying, exacerbated when the temperature is high. The conventional anhydrite-based screeds are not usable when the temperature is higher than about 30 ° C because beyond this temperature, the kinetics of hydration (if the latter takes place) is so slow that the resistances reached at 28 days are very insufficient.
L'objet de l'invention est de développer une chape utilisable à des températures supérieures à 30°C et qui présente les avantages techniques des chapes anhydrites classiques : The object of the invention is to develop a screed which can be used at temperatures above 30 ° C. and which has the technical advantages of conventional anhydrite screeds:
Bonne ouvrabilité,  Good workability,
- Mise en place aisée (autop laçant)  - Easy setting up (autopiling)
Finition de surface facile  Easy surface finish
Bon durcissement de la chape après la prise.  Good curing of the screed after setting.
D'une manière surprenante, il a été découvert que l'utilisation de plâtre, c'est-à-dire de sulfate de calcium semihydrate, sous sa forme cristalline β, en tant que liant hydraulique, permettait la fabrication de chapes utilisables par temps chaud qui présentent les caractéristiques attendues des chapes anhydrites classiques : bonne ouvrabilité, autoplaçant, finition facile et résistances mécaniques après durcissement. Surprisingly, it has been discovered that the use of plaster, that is to say calcium sulfate hemihydrate, in its crystalline form β, as a hydraulic binder, allows the manufacture of screeds usable in time. The characteristics of classic anhydrite screeds are expected to be warm: good workability, self-compacting, easy finishing and mechanical strength after hardening.
Les chapes obtenues présentent les caractéristiques mécaniques recherchées :  The screeds obtained have the desired mechanical characteristics:
- Résistance à la compression, Rc, supérieure ou égale à 20 MPa à 28j  - Resistance to compression, Rc, greater than or equal to 20 MPa to 28j
- Résistance à la flexion, Rf, supérieure ou égale à 4 MPa à 28j  - Flexural strength, Rf, greater than or equal to 4 MPa at 28j
La demande DE 20 2007 003 608 décrit une chape à base de plâtre sous sa forme cristalline a pouvant être coulée à une température allant de 0°C à 35°C. Toutefois, lorsque l'on souhaite couler une telle chape à des températures supérieures ou égales à 30°C, pour obtenir une rhéologie acceptable, il convient d'ajouter des quantités augmentées d'adjuvants, dont des agents réducteurs d'eau, onéreux. En comparaison, avec la chape selon l'invention la demande en adjuvants, en particulier en agents réducteurs d'eau, est moindre et ainsi la chape selon l'invention est signifïcativement plus économique. EXPOSE DE L'INVENTION DE 20 2007 003 608 discloses a plaster based screed in its crystalline form which can be cast at a temperature of 0 ° C to 35 ° C. However, when it is desired to pour such a screed at temperatures greater than or equal to 30 ° C, to obtain an acceptable rheology, it is necessary to add increased amounts of adjuvants, including water reducing agents, expensive. In comparison, with the screed according to the invention the demand for admixtures, in particular for water reducing agents, is less and thus the screed according to the invention is significantly more economical. SUMMARY OF THE INVENTION
L'invention a ainsi pour objet l'utilisation de plâtre, sous sa forme cristalline β, pour la préparation d'une composition de chape de sol, comprenant également du sable et un superplastifiant, destinée à être coulée à une température supérieure ou égale à 30°C. The invention thus relates to the use of plaster, in its crystalline form β, for the preparation of a floor screed composition, also comprising sand and a superplasticizer, intended to be cast at a temperature greater than or equal to 30 ° C.
Les chapes à base de plâtre selon l'invention peuvent ainsi être utilisées dans des pays chauds, où la température ambiante est supérieure à 30°C, éventuellement supérieure à 35°C, voire supérieure à 40°C.  The plaster-based screeds according to the invention can thus be used in hot countries, where the ambient temperature is greater than 30 ° C., possibly greater than 35 ° C., or even greater than 40 ° C.
Dans ces pays, où la température ambiante est chaude, les chapes traditionnelles à base de ciment fissurent et les chapes à base d'anhydrite ne s'hydratent pas.  In these countries, where the ambient temperature is hot, traditional cement-based screeds crack and anhydrite-based screeds do not hydrate.
DESCRIPTION DETAILLEE DE L'INVENTION DETAILED DESCRIPTION OF THE INVENTION
Par le terme « adjuvant », on entend selon la présente invention tout composé qui incorporé dans une formulation permet d'apporter des propriétés particulières. By the term "adjuvant" is meant according to the present invention any compound that incorporated into a formulation allows to provide particular properties.
Par le terme « liant », on entend selon la présente invention tout composé ayant la propriété d'apporter de la cohésion à la formulation dans laquelle il est incorporé, et permet d'apporter des caractéristiques mécaniques à ladite formulation (par exemple résistance en compression, en traction, adhérence). Ce liant peut également être destiné à lier des éléments inertes tels que des granulats.  By the term "binder" is meant according to the present invention any compound having the property of providing cohesion to the formulation in which it is incorporated, and makes it possible to provide mechanical characteristics to said formulation (for example compressive strength , in traction, adhesion). This binder may also be intended to bind inert elements such as aggregates.
Par l'expression « liants hydrauliques », on entend selon la présente invention tout composé ayant la propriété de s'hydrater en présence d'eau et dont l'hydratation permet d'obtenir un solide ayant des caractéristiques mécaniques. L'expression liant hydraulique désigne également les liants hydriques. Le liant hydraulique selon l'invention est un liant à base de plâtre.  By the term "hydraulic binders" is meant according to the present invention any compound having the property of hydrating in the presence of water and whose hydration makes it possible to obtain a solid having mechanical characteristics. The term hydraulic binder also refers to water binders. The hydraulic binder according to the invention is a binder based on plaster.
Par l'expression « plâtre sous sa forme cristalline β » ou « plâtre β », on entend selon la présente invention du plâtre, encore appelé sulfate de calcium semi-hydrate ou sulfate de calcium hemi-hydraté, de formule chimique CaSO4*0.5H2O, dans lequel la forme cristalline β est majoritaire en masse. Particulièrement, si la forme cristalline a est présente, sa teneur massique est inférieure à 5%, par rapport au poids total des formes cristallines a et β, avantageusement inférieure à 2%, avantageusement inférieure à 1%. By the expression "plaster in its crystalline form β" or "plaster β" is meant according to the present invention plaster, also called calcium sulfate hemihydrate or hemi-hydrated calcium sulfate, of chemical formula CaSO 4 * 0.5 H 2 O, in which the crystalline form β is predominant in mass. Especially, if the crystalline form has is present, its mass content is less than 5%, relative to the total weight of crystalline forms a and β, preferably less than 2%, preferably less than 1%.
L'invention a pour objet l'utilisation de plâtre, sous sa forme cristalline β, pour la préparation d'une composition de chape de sol, comprenant également du sable et un superplastifiant, destinée à être coulée à une température supérieure ou égale à 30°C. The invention relates to the use of plaster, in its crystalline form β, for the preparation of a floor screed composition, also comprising sand and a superplasticizer, intended to be cast at a temperature greater than or equal to 30 ° C.
La chape de sol selon l'invention peut être coulée à une température supérieure ou égale à 30°C, à une température supérieure ou égale à 35°C, voire à une température supérieure ou égale à 40°C. The floor screed according to the invention may be cast at a temperature greater than or equal to 30 ° C, at a temperature greater than or equal to 35 ° C, or even at a temperature greater than or equal to 40 ° C.
L'invention se caractérise par l'utilisation, en tant que liant hydraulique, de plâtre sous sa forme cristalline β.  The invention is characterized by the use, as a hydraulic binder, of plaster in its crystalline form β.
Ce plâtre, encore appelé sulfate de calcium semi-hydrate ou sulfate de calcium hemi- hydraté, de formule chimique CaSO4*0.5H2O, peut exister sous deux formes cristallines: la forme a ou la forme β. Les deux formes cristallines peuvent être utilisées pour la préparation de chapes, la forme β donnant toutefois des chapes de meilleure qualité et surtout pour un coût financier moindre. This plaster, also called calcium sulphate hemihydrate or calcium sulphate hemihydrate, chemical formula CaSO 4 * 0.5H 2 O, can exist in two crystalline forms: the form a or the form β. The two crystalline forms can be used for the preparation of screeds, the β form however giving better quality screeds and especially for a lower financial cost.
Dans le cadre de la présente invention, la composition peut comprendre à titre de liant hydraulique seulement du plâtre ou un mélange de plâtre et de charge.  In the context of the present invention, the composition may comprise as hydraulic binder only plaster or a mixture of plaster and filler.
Avantageusement, le liant hydraulique comprend en masse au moins 52% de plâtre et de 0% à 48% de charge, la somme de ces deux pourcentages variant de 80%> à 100%.  Advantageously, the hydraulic binder comprises at least 52% by weight of plaster and from 0% to 48% by weight, the sum of these two percentages varying from 80% to 100%.
La somme de ces deux pourcentages varie avantageusement de 85% à 100%, plus avantageusement de 90% à 100%, encore plus avantageusement de 95% à 100%). Le plâtre étant le plus souvent d'origine naturelle, il est difficile d'obtenir une matière première comprenant exclusivement du sulfate de calcium semi-hydrate. Le plâtre peut comprendre des impuretés telles du quartz (Si02), de la celestine (SrS04), des phases carbonatées comme la calcite (CaC03), la dolomite (CaMg(C03)2), des phases argileuses ou feldspathiques comme la chlorite ((Mg,Al)6(Si,Al)4Oio(OH)8), microcline (K(Si0,75Al0,25)4O8), phlogopite (KMg2,75Si3,5A10,5OioF2), kaolinite (Al2Si205(OH)4), albite (Na(AlSi3Os), muscovite (KAl3Si3Oio(OH)2). Avantageusement, le plâtre comprend moins de 5%) en poids, plus avantageusement moins de 2% en poids, par rapport au poids total du plâtre, d'impuretés. Le plâtre peut également comprendre du gypse ou de l'anhydrite. On utilisera un plâtre comprenant les quantités les plus faibles possibles en gypse ou en anhydrite. Avantageusement, le plâtre comprend moins de 5% en poids, plus avantageusement moins de 2% en poids, encore plus avantageusement moins de 1% en poids, par rapport au poids total du plâtre, de gypse. Avantageusement, le plâtre comprend moins de 5% en poids, plus avantageusement moins de 2% en poids, encore plus avantageusement moins de 1% en poids, par rapport au poids total du plâtre, d'anhydrite. Avantageusement, le plâtre comprend moins de 5% en poids, plus avantageusement moins de 2% en poids, encore plus avantageusement moins de 1% en poids, par rapport au poids total du plâtre, de plâtre sous sa forme cristalline a. The sum of these two percentages advantageously varies from 85% to 100%, more preferably from 90% to 100%, even more preferably from 95% to 100%). The plaster being most often of natural origin, it is difficult to obtain a raw material comprising exclusively calcium sulphate semi-hydrate. The plaster may comprise impurities such as quartz (Si0 2 ), celestine (SrS0 4 ), carbonate phases such as calcite (CaCO 3 ), dolomite (CaMg (CO 3 ) 2 ), clay or feldspathic phases such as chlorite ((Mg, Al) 6 (Si, Al) 4 O 10 (OH) 8 ), microcline (K (Si 0 , 75 Al 0 , 25 ) 4 O 8 ), phlogopite (KMg 2 , 75 Si 3 , 5 A 10, 5 OioF 2), kaolinite (Al 2 Si 2 0 5 (OH) 4), albite (Na (AlSi 3 O), muscovite (KAl 3 Si 3 Oio (OH) 2). Advantageously, the plaster comprises less 5%) by weight, more preferably less than 2% by weight, based on the total weight of the plaster, impurities. The plaster may also include gypsum or anhydrite. A plaster with the smallest possible amounts of gypsum or anhydrite will be used. Advantageously, the plaster comprises less than 5% by weight, more preferably less than 2% by weight, and even more advantageously less than 1% by weight, relative to the total weight of plaster, of gypsum. Advantageously, the plaster comprises less than 5% by weight, more preferably less than 2% by weight, and even more advantageously less than 1% by weight, based on the total weight of the plaster, of anhydrite. Advantageously, the plaster comprises less than 5% by weight, more preferably less than 2% by weight, and even more advantageously less than 1% by weight, based on the total weight of the plaster, of plaster in its crystalline form a.
La granulométrie et la surface spécifique du plâtre n'est pas critique dans l'invention.  The particle size and the specific surface area of the plaster is not critical in the invention.
Des charges (fïllers) de différentes natures (calcaires, siliceux, cendres volantes, fumées de silice) peuvent être utilisés en complément du plâtre. Fillers (filler) of different kinds (limestone, siliceous, fly ash, silica fume) can be used in addition to plaster.
Remplacer une partie du plâtre par une charge permet de réduire les coûts des matières premières. Un tel remplacement permet également de réduire les résistances mécaniques lorsqu'elles sont supérieures à la cible. Un tel remplacement permet également de réduire les quantités en superplastifiant.  Replacing part of the plaster with a load reduces the cost of raw materials. Such a replacement also makes it possible to reduce the mechanical strengths when they are greater than the target. Such a replacement also makes it possible to reduce the quantities by superplasticizer.
Par définition, la charge sera inerte ou aura une réactivité faible par rapport à celle du plâtre.  By definition, the load will be inert or will have a low reactivity compared to that of plaster.
La charge peut être, par exemple du calcaire, un carbonate de calcium naturel broyé (par exemple la craie, la calcite, le marbre ou un autre carbonate de calcium naturel), un carbonate de calcium précipité (également connu sous le nom de carbonate de calcium synthétique), le carbonate de baryum, la dolomite, le talc, la silice cristalline, le dioxyde de titane pyrogéné, un oxyde de fer, un oxyde de manganèse, le dioxyde de titane, le kaolin, les argiles, le mica, le sulfate de calcium, le basalte, le sulfate de baryum, l'hydroxyde d'aluminium, la bauxite, une charge de faible réactivité telle que le laitier de haut fourneau, ou un de leurs mélanges. Le calcaire, le carbonate de calcium broyé et le carbonate de calcium précipité sont préférés.  The filler may be, for example, limestone, ground natural calcium carbonate (eg chalk, calcite, marble or other natural calcium carbonate), precipitated calcium carbonate (also known as calcium carbonate). synthetic calcium), barium carbonate, dolomite, talc, crystalline silica, pyrogenic titanium dioxide, iron oxide, manganese oxide, titanium dioxide, kaolin, clays, mica, calcium sulphate, basalt, barium sulfate, aluminum hydroxide, bauxite, a low reactivity filler such as blast furnace slag, or a mixture thereof. Limestone, ground calcium carbonate and precipitated calcium carbonate are preferred.
Avantageusement, la composition ne comprend pas de ciment. Si du ciment devait être présent, ce serait avantageusement en une quantité inférieure à 20% en poids, plus avantageusement inférieure à 10% en poids, plus avantageusement inférieure à 5% en poids, par rapport au poids total de la composition. Il a été constaté que le pH du mortier, c'est-à-dire du mélange sable et liant hydraulique, avait un impact sur la fluidité de la composition. Pour assurer une fluidité optimale, le pH du plâtre dans l'eau, mesuré à un rapport massique eau/poudre de plâtre = 0,487, est avantageusement ajusté à un pH allant de 10 à 13. Plus on se rapproche de 12 et meilleurs sont les résultats de fluidité. Advantageously, the composition does not comprise cement. If cement were to be present, it would be advantageously in an amount of less than 20% by weight, more preferably less than 10% by weight, more preferably less than 5% by weight, based on the total weight of the composition. It has been found that the pH of the mortar, that is to say of the sand and hydraulic binder mixture, has an impact on the fluidity of the composition. To ensure optimum fluidity, the pH of the plaster in the water, measured at a mass ratio water / plaster powder = 0.487, is advantageously adjusted to a pH ranging from 10 to 13. The closer we get to 12, the better are the fluidity results.
Avantageusement, le pH est ajusté par ajout de chaux (CaO ou Ca(OH)2). On peut ainsi ajouter de 0,1 à 0,2% en poids d'équivalent CaO, par rapport au poids du plâtre. Advantageously, the pH is adjusted by adding lime (CaO or Ca (OH) 2 ). It is thus possible to add from 0.1 to 0.2% by weight of CaO equivalent, relative to the weight of the plaster.
L'ajout d'une quantité trop importante de CaO peut raccourcir le temps de prise.  Adding too much CaO can shorten the setting time.
La composition de chape selon l'invention comprend des adjuvants, ayant pour objectif de modifier les propriétés rhéologiques du mortier. Les adjuvants vont également influencer sur le temps de prise. The screed composition according to the invention comprises adjuvants, the purpose of which is to modify the rheological properties of the mortar. Adjuvants will also influence setting time.
Les adjuvants sont ajoutés par exemple soit dans le mortier, de préférence dans un sachet hydrosoluble, soit avec une partie de l'eau, soit dans le liant, soit dans plusieurs vecteurs.  The adjuvants are added for example either in the mortar, preferably in a water-soluble sachet, or with part of the water, or in the binder, or in several vectors.
Dans l'invention, on ajoute un superplastifiant. Un agent superplastifiant est un additif permettant, par son addition à une composition aqueuse de sulfate de calcium, de réduire la demande en eau et de maintenir la fluidité/rhéologie de la pâte. In the invention, a superplasticizer is added. A superplasticizing agent is an additive which, by its addition to an aqueous calcium sulphate composition, reduces the water demand and maintains the fluidity / rheology of the dough.
Les superplastifiants ont été globalement classés en quatre groupes : les condensais sulfonés de naphtalène formaldéhyde (SNF) (généralement un sel de sodium) ; les condensais sulfonés de mélamine formaldéhyde (SMF) ; les lignosulfonates modifiés (MLS) ; et les autres. Des superplastifiants plus récents incluent des composés polycarboxyliques comme les polycarboxylates, par exemple les polyacrylates. Des superplastifiant à base de copolymère acrylique peuvent aussi être utilisés, de préférence ce sont des polymères comprenant une chaîne avec une fonction polycarboxylique, éventuellement salifiée, à laquelle un autre groupe (par exemple du type polycarboxylate ou polyoxyéthylène) est attaché. Un superplastifiant est de préférence un superplastifiant nouvelle génération, par exemple un copolymère contenant un polyéthylène glycol comme chaîne greffée et des fonctions carboxyliques dans la chaîne principale comme un éther polycarboxylique. Les polycarboxylates, tels que l'éther de polycarboxylate (PCE), sont particulièrement adaptés. Avantageusement, le superplastifiant est un polycarboxylate, en particulier un éther ou un ester de polycarboxylate. Avantageusement, les superplastifiants sont des polycarboxylates qui ont au moins les trois unités suivantes qui se répètent : une unité acrylique, une unité d'acide méthacrylique et une unité formée d'une longue chaîne de polyéthers Ces types de dispersants ou superplastifiants sont très efficaces, spécialement pour améliorer la fluidité. Une haute efficacité de dispersion permet aussi de diminuer la quantité de superplastifiants utilisés et d'avoir un bénéfice économique étant donné que le produit à base de carboxylate sont relativement coûteux. Les polycarboxylates- polysulfonates de sodium et les polyacrylates de sodium peuvent aussi être utilisés. Les dérivés d'acide phosphonique et les polycarboxylates présentant des groupements phosphates, peuvent aussi être utilisés. Des polycarboxylate-polysulfonates de sodium et des polyacrylates de sodium peuvent également être utilisés. Superplasticizers were broadly classified into four groups: sulfonated condensates of naphthalene formaldehyde (SNF) (usually a sodium salt); sulphonated condensates of melamine formaldehyde (SMF); modified lignosulfonates (MLS); And the others. More recent superplasticizers include polycarboxylic compounds such as polycarboxylates, for example polyacrylates. Acrylic copolymer superplasticizers can also be used, preferably they are polymers comprising a chain with a possibly salified polycarboxylic function, to which another group (for example of the polycarboxylate or polyoxyethylene type) is attached. A superplasticizer is preferably a new generation superplasticizer, for example a copolymer containing a polyethylene glycol as a grafted chain and carboxylic functions in the main chain as a polycarboxylic ether. Polycarboxylates, such as polycarboxylate ether (PCE), are particularly adapted. Advantageously, the superplasticizer is a polycarboxylate, in particular an ether or a polycarboxylate ester. Advantageously, the superplasticizers are polycarboxylates which have at least the following three units which are repeated: an acrylic unit, a methacrylic acid unit and a unit formed of a long chain of polyethers These types of dispersants or superplasticizers are very effective, especially to improve fluidity. High dispersion efficiency also makes it possible to reduce the amount of superplasticizer used and to have an economic benefit since the carboxylate product is relatively expensive. Sodium polycarboxylate polysulfonates and sodium polyacrylates can also be used. Phosphonic acid derivatives and polycarboxylates having phosphate groups may also be used. Sodium polycarboxylate polysulfonates and sodium polyacrylates may also be used.
La quantité de superplastifiant est très dépendante de la nature du superplastifiant et de sa dilution ; on donnera néanmoins des dosages à 100% d'extrait sec. L'agent superplastifiant (exprimé en extrait sec) est en général présent en une quantité comprise entre 0,01% et 3%, de préférence entre 0,1 % et 2,5%, par rapport au poids du plâtre.  The amount of superplasticizer is highly dependent on the nature of the superplasticizer and its dilution; however, 100% solids content will be given. The superplasticizing agent (expressed as dry extract) is generally present in an amount of between 0.01% and 3%, preferably between 0.1% and 2.5%, relative to the weight of the plaster.
Le superplastifiant est généralement ajouté sous forme de poudre, mais un ajout sous forme liquide est aussi possible. L'ajout sous forme liquide permet de façon générale un dosage automatisé-des additifs.  The superplasticizer is usually added as a powder, but an addition in liquid form is also possible. The addition in liquid form generally allows an automated dosage of additives.
Dans un mode de réalisation, la composition comprend également un retardateur. Un ou plusieurs retardateurs de prise peuvent être utilisés. De tels retardateurs sont par exemple les acides carboxyliques tels que l'acide citrique, les sucres et leurs dérivés, le sel de calcium de polyoxymethylene amino-acide, des polyamides dégradées. In one embodiment, the composition also includes a retarder. One or more set retarders may be used. Such retarders are, for example, carboxylic acids such as citric acid, sugars and their derivatives, polyoxymethylene amino acid calcium salt, degraded polyamides.
Les retardateurs sont utilisés pour obtenir un temps de prise (entre le début et la fin de la prise) qui est compatible avec l'application souhaitée. Des agents viscosifîants et des épaississants peuvent aussi être utilisés, notamment pour éviter la ségrégation et/ou le ressuage. Par exemple on peut utiliser des biopolymères (tels que les gommes : la gomme de diutane, la gomme de guar, la gomme xanthane) notamment obtenus par fermentation, la silice précipitée ou les dérivés de cellulose (tels que le méthylcellulose, le méthylhydroxypropylcellulose, l'hydroxyéthylcellulose, le carboxyméthylcellulose), et les mélanges de ces composés. Il est possible d'ajouter un colorant (pigment) dans le mortier pour chape, notamment au niveau de l'additif dans son sachet. La quantité de retardateur est très dépendante de la nature du retardateur et de sa dilution ; on donnera néanmoins des dosages à 100% d'extrait sec. L'agent retardateur (exprimé en extrait sec) est en général présent en une quantité comprise entre 0,01% et 3%, de préférence entre 0,05%> et 2%, par rapport au poids de plâtre. Delayers are used to obtain a setting time (between the beginning and the end of the shot) that is compatible with the desired application. Viscosifiers and thickeners may also be used, in particular to avoid segregation and / or bleeding. For example, it is possible to use biopolymers (such as gums: diutane gum, guar gum, xanthan gum), especially obtained by fermentation, precipitated silica or cellulose derivatives (such as methylcellulose, methylhydroxypropylcellulose, hydroxyethylcellulose, carboxymethylcellulose), and mixtures of these compounds. It is possible to add a dye (pigment) in the mortar for screed, especially at the level of the additive in its bag. The amount of retarder is very dependent on the nature of the retarder and its dilution; however, 100% solids content will be given. The retarding agent (expressed as dry extract) is generally present in an amount of between 0.01% and 3%, preferably between 0.05% and 2%, relative to the weight of plaster.
La quantité de retardateur sera également ajustée en fonction de la température ambiante : quantité à diminuer quand la température ambiante augmente.  The amount of retarder will also be adjusted according to the ambient temperature: quantity to decrease when the ambient temperature increases.
En utilisant un sable calcaire, on peut augmenter la quantité de retardateur par rapport à une formule comprenant un sable siliceux. Par exemple, à 40°C, on pourra utiliser 0,30%> de retardateur, par rapport au poids de plâtre, avec un sable calcaire et 0,20%) de retardateur, par rapport au poids de plâtre, avec un sable siliceux.  By using calcareous sand, the amount of retarder can be increased with respect to a formula comprising siliceous sand. For example, at 40 ° C., 0.30%> retarder, based on the weight of plaster, with calcareous sand and 0.20%) retarder, based on the weight of plaster, with a siliceous sand can be used. .
Le retardateur est généralement ajouté sous forme de poudre, mais un ajout sous forme liquide est aussi possible. L'ajout sous forme liquide permet de façon générale un dosage automatisé-des additifs. Dans un mode de réalisation, la composition comprend également un agent antimousse.  The retarder is usually added as a powder, but addition in liquid form is also possible. The addition in liquid form generally allows an automated dosage of additives. In one embodiment, the composition also comprises an antifoaming agent.
Le type d'agent anti-mousse est varié. Il peut notamment être à base de silicone, d'alcools gras, esters, de polypropylène glycol. Notamment l'agent anti-mousse peut être choisi dans les classes suivantes :  The type of antifoaming agent is varied. It may especially be based on silicone, fatty alcohols, esters, polypropylene glycol. In particular, the anti-foam agent may be chosen in the following classes:
- Anti-mousse à base d'huile, qui a une huile comme véhicule. Cette huile peut être minérale, végétale (sauf silicone). L'anti-mousse comprend aussi une cire et/ou une silice hydrophobe. Des cires sont par exemples éthylène bis stéaramide (EBS), cires paraffmiques, cires ester et les cires à base d'alcools gras. Des tensio-actifs peuvent aussi être présents ; - Antifoam based on oil, which has an oil as a vehicle. This oil can be mineral, vegetable (except silicone). The antifoam also comprises a wax and / or a hydrophobic silica. Examples of waxes are ethylene bis stearamide (EBS), paraffin waxes, ester waxes and waxes based on fatty alcohols. Surfactants may also be present;
- Anti-mousse en poudre. Ces agents correspondent à ces agents à base d'huile mais sur un support particulaire tel que de la silice ; - Antifoam powder. These agents correspond to these oil-based agents but on a particulate support such as silica;
- Anti-mousse sur base aqueuse. Ce sont en général des huiles ou des cires dispersées dans une base aqueuse. Les huiles sont des huiles blanches ou des huiles végétales and les cires sont des alcools gras, des acides gras, des esters ou des savons de ceux-ci ;  - Anti-foam on aqueous base. These are usually oils or waxes dispersed in an aqueous base. The oils are white oils or vegetable oils and the waxes are fatty alcohols, fatty acids, esters or soaps thereof;
- Anti-mousse silicone. Ces anti-mousses ont un silicone comme agent actif. On peut en disposer sur base huile ou sur base aqueuse. Une silice hydrophobe peut être dispersée dans le milieu silicone. Des émulsifïants peuvent être utilisés. Des silicones modifiés comme des silicones glycols ou des fluorosilicones peuvent aussi être utilisés. L'agent anti-mousse peut être un polydiméthylsiloxane. Particulièrement adaptés sont les silicones comprenant des groupements (RSiOo,s) et (R2SiO). Dans ces formules, les radicaux R, qui peuvent être identiques ou différents, sont de préférence un atome d'hydrogène ou un groupe alkyle de 1 à 8 atomes de carbone, le groupe méthyle étant préféré. Le nombre de motifs est de préférence de 30 à 120 ; - Silicone antifoam. These antifoams have a silicone as active agent. It can be available on oil base or aqueous base. A hydrophobic silica may be dispersed in the silicone medium. Emulsifiers can be used. Modified silicones such as silicone glycols or fluorosilicones can also be used. The agent antifoam may be a polydimethylsiloxane. Particularly suitable are silicones comprising (RSiOo, s) and (R 2 SiO) groups. In these formulas, the R radicals, which may be the same or different, are preferably a hydrogen atom or an alkyl group of 1 to 8 carbon atoms, the methyl group being preferred. The number of units is preferably from 30 to 120;
- Anti-mousse du type glycol. Ces agents comprennent des copolymères polyéthylène glycol et polypropylène glycol. Ils sont disponibles sur base huileuse ou aqueuse ou émulsions ;  - Anti-foam glycol type. These agents include polyethylene glycol and polypropylene glycol copolymers. They are available on oily or aqueous base or emulsions;
- Anti-mousse du type alkylpolyacrylate. Ces agents sont généralement disponibles dans un solvant pétrolier ;  - Antifoam of the alkylpolyacrylate type. These agents are generally available in a petroleum solvent;
- les mélanges de ces composés.  mixtures of these compounds.
La quantité de cet agent est comprise typiquement entre 0,01% et 5%, de préférence 0,11% et 5%, calculé par rapport en extrait sec du superplastifiant.  The amount of this agent is typically between 0.01% and 5%, preferably 0.11% and 5%, calculated with respect to the solids content of the superplasticizer.
L'agent anti-mousse est généralement ajouté sous forme de poudre, mais un ajout sous forme liquide est aussi possible. L'ajout sous forme liquide permet de façon générale un dosage automatisé-des additifs.  The defoamer is usually added as a powder, but addition in liquid form is also possible. The addition in liquid form generally allows an automated dosage of additives.
Selon un mode de réalisation, la composition comprend en outre un adjuvant choisi parmi les accélérateurs de prise, agents épaississants, agents de viscosité et/ou rétenteurs d'eau, entraîneurs d'air, agents anti pellicule, traceurs, agents hydrophobants, agents colorants et leurs mélanges, en particulier les agents viscosifïants et/ou les épaississants. According to one embodiment, the composition further comprises an adjuvant chosen from setting accelerators, thickening agents, viscosity agents and / or water retenters, air entraining agents, anti-film agents, tracers, hydrophobing agents and coloring agents. and mixtures thereof, in particular viscosifiers and / or thickeners.
La quantité d'eau est ajustée en vue d'obtenir la consistance et les résistances mécaniques requises pour l'application de la composition sur chantier. The amount of water is adjusted to obtain the consistency and the mechanical strengths required for the application of the composition on site.
La quantité d'eau est généralement susceptible d'être exprimée par rapport au liant, et le ratio eau/liant est généralement compris entre 0,27 et 0,70, de préférence entre 0,35 et 0,70, avantageusement entre 0,40 et 0,70.  The amount of water is generally capable of being expressed relative to the binder, and the water / binder ratio is generally between 0.27 and 0.70, preferably between 0.35 and 0.70, advantageously between 0, 40 and 0.70.
Les valeurs d'étalement des compositions selon l'invention sont classiques. Elles présentent notamment un étalement d'au moins 22cm, de préférence au moins 24cm, avantageusement au moins 25 cm. La chape selon l'invention remplit généralement les exigences des normes européennes EN 13454-1 de février 2005 (liant), EN 13813 de juin 2003 (mortier), et selon les méthodes d'essais décrits dans la norme NF EN 13454-2+A1 de septembre 2007 relatives aux liants et mortiers à base de sulfate de calcium pour chapes fluides. La quantité de liant notamment sulfate de calcium dans la chape varie avantageusement de 400 à 700 kg/m3, typiquement de l'ordre de 650 kg/m3. Le liant est présent en une quantité usuelle, notamment pour atteindre et conserver les qualités minimales spécifiées dans les normes ci-dessus. The spreading values of the compositions according to the invention are conventional. In particular, they have a spread of at least 22 cm, preferably at least 24 cm, advantageously at least 25 cm. The screed according to the invention generally meets the requirements of the European standards EN 13454-1 of February 2005 (binder), EN 13813 of June 2003 (mortar), and according to the test methods described in standard NF EN 13454-2 + A1 of September 2007 relating to binders and mortars based on calcium sulphate for fluid screeds. The amount of binder, especially calcium sulphate, in the screed advantageously varies from 400 to 700 kg / m 3 , typically of the order of 650 kg / m 3 . The binder is present in a customary amount, in particular to achieve and maintain the minimum qualities specified in the standards above.
Dans les cas où les résistances mécaniques sont trop importantes, pour se rapprocher de la cible, il suffit de diminuer la quantité de sulfate de calcium semi- hydrate en diminuant la quantité de liant ou en remplaçant une partie de sulfate de calcium semi- hydrate par une charge inerte.  In cases where the mechanical strengths are too high, to get closer to the target, it is sufficient to reduce the amount of calcium sulphate semi-hydrate by decreasing the amount of binder or replacing a portion of calcium sulphate semi-hydrate by an inert load.
Les sables qui sont utilisés dans la formulation selon l'invention sont des granulats classiques conformes à la norme EN 12620 (sables pour béton). En pratique, le Dmax est inférieur à 4mm, et en général le sable présente des tailles de particules sensiblement entre 0 et 4mm (qui sont dénommés généralement sables 0-4). Les sables incluent des matériaux calcaires, siliceux et silico-calcaires. Le sable peut être de différentes origines, alluvionnaires lavés (roulés, semi-concassés ou concassés), sables d'origine marine, sables concassés calcaires (sec ou lavés), sables d'origine magmatique (porphyre, granité), granulats de recyclage issus du concassage de bétons ou d'autres matériaux de construction Lorsque le sable comprend de l'argile, il est avantageux d'ajouter des inertants. Les inertants des argiles sont des composés qui permettent de réduire ou de prévenir les effets néfastes des argiles sur les propriétés des liants hydrauliques. Les inertants des argiles incluent ceux décrits dans FR 2 948 1 18, WO 2006/032785 et WO 2006/032786. The sands which are used in the formulation according to the invention are conventional aggregates in accordance with EN 12620 (sands for concrete). In practice, the Dmax is less than 4 mm, and in general the sand has particle sizes substantially between 0 and 4 mm (which are generally referred to as 0-4 sands). Sands include calcareous, siliceous and silico-calcareous materials. The sand can be of different origins, alluvial washed (rolled, semi-crushed or crushed), sands of marine origin, crushed calcareous sand (dry or washed), sands of magmatic origin (porphyry, granite), aggregates of recycling resulting crushing concrete or other building materials When the sand comprises clay, it is advantageous to add inertants. Inerting clays are compounds that reduce or prevent the harmful effects of clays on the properties of hydraulic binders. Inerting clays include those described in FR 2 948 1 18, WO 2006/032785 and WO 2006/032786.
Selon un mode de réalisation avantageuse, les sables sont des sables de nature calcaire ou silico calcaire, plus avantageusement de nature calcaire.  According to an advantageous embodiment, the sands are sands of calcareous or silico-calcareous nature, more preferably of limestone nature.
Avantageusement, la composition de chape comprend, par mètre cube de composition à l'état frais : Advantageously, the screed composition comprises, per cubic meter of composition in the fresh state:
— De 450 à 700 kg d'un liant hydraulique comprenant en masse au moins 52% de plâtre et de 0% à 48% de charge, la somme de ces deux pourcentages variant de 80%> à 100% — de 250 à 350 litres d'eau, le rapport entre la masse d'eau et la masse de liant hydraulique étant de 0,4 à 0,7; - From 450 to 700 kg of a hydraulic binder comprising in mass at least 52% of plaster and from 0% to 48% of filler, the sum of these two percentages varying from 80%> to 100% From 250 to 350 liters of water, the ratio between the mass of water and the mass of hydraulic binder being from 0.4 to 0.7;
— un superplastifiant,  - a superplasticizer,
— un retardateur,  - a self-timer,
— éventuellement de la chaux  - possibly lime
— éventuellement un agent antimousse  Optionally an antifoaming agent
— du sable en une quantité suffisante pour avoir 1 m3 - sand in sufficient quantity to have 1 m 3
La composition de chape comprend avantageusement de 0,5 à 2,5% de superplasitifîant, pourcentages exprimés en poids d'extrait sec de superplastifiant par rapport au poids du plâtre. The screed composition advantageously comprises from 0.5 to 2.5% of superplasticizer, percentages expressed by weight of dry extract of superplasticizer relative to the weight of the plaster.
La composition de chape comprend avantageusement de 0,05 à 0,2% de retardateur, pourcentages exprimés en poids d'extrait sec de retardateur par rapport au poids du plâtre.  The screed composition advantageously comprises from 0.05 to 0.2% of retarder, percentages expressed by weight of dry extract of retarder relative to the weight of the plaster.
La composition de chape comprend avantageusement de 0,1 à 0,2%> de CaO, pourcentages exprimés en poids d'extrait sec de retardateur par rapport au poids du plâtre.  The screed composition advantageously comprises from 0.1 to 0.2% of CaO, percentages expressed by weight of retarder solids relative to the weight of the plaster.
La composition de chape comprend avantageusement de 0,01% à 0,5%>, calculé par rapport en extrait sec du superplastifiant, d'agent antimousse.  The screed composition advantageously comprises from 0.01% to 0.5%, based on the dry extract of the superplasticizer, of an antifoaming agent.
La composition de chape de sol selon l'invention présente l'avantage d'être auto- plaçante. Elle peut facilement être coulée à l'aide d'une pompe, par exemple une pompe à vis ou une pompe à piston. The floor screed composition according to the invention has the advantage of being self-placing. It can easily be poured by means of a pump, for example a screw pump or a piston pump.
Dans la présente description, y compris les revendications qui l'accompagnent :In the present description, including the claims that accompany it:
- les résistances en compression sont mesurées sur des éprouvettes cubiques 15 x 15 x 15 cm après durcissement pendant deux jours à 20°C, puis après séchage pendant plusieurs jours à 45 °C maximum. Un séchage à 90°C entraînerait à long terme une déshydratation du gypse donc une diminution des résistances mécaniques, le séchage doit donc être préconisé à 40-45°C jusqu'à ce que la masse de l'éprouvette soit constante. La force appliquée à l'échantillon est augmentée à une vitesse de 3,85 kN/s pendant l'essai ; the compressive strengths are measured on cubic test pieces 15 × 15 × 15 cm after curing for two days at 20 ° C. and then after drying for several days at 45 ° C. maximum. Drying at 90 ° C in the long term would lead to dehydration of the gypsum and therefore a decrease in mechanical strength, so drying should be recommended at 40-45 ° C until the mass of the test piece is constant. The force applied to the sample is increased at a rate of 3.85 kN / s during the test;
- les résistances à la flexion sont mesurées après durcissement tel que décrit ci-avant the flexural strengths are measured after hardening as described above
(2 jours de séchage à 45°C suffisent avec cette géométrie d'éprouvette) pour les résistances à la compression sur éprouvettes prismatiques de dimensions 4 x 4 x 16 cm supportées en deux points, la force étant appliquée au milieu, et la force appliquée à l'échantillon étant élevée à une vitesse de 0,05 kN/s pendant l'essai ; (2 days of drying at 45 ° C suffice with this specimen geometry) for the compressive strengths on prismatic specimens of dimensions 4 x 4 x 16 cm supported in two points, the force being applied to the medium, and the force applied to the sample being raised at a rate of 0.05 kN / s during the test;
- les pourcentages, sauf indication contraire, sont en masse ;  - the percentages, unless otherwise indicated, are in mass;
- Méthode de mesure de l'étalement :Le principe de la mesure d'étalement consiste à remplir un tronc de cône de mesure d'étalement avec la composition hydraulique à tester puis à libérer ladite composition dudit tronc de cône de mesure d'étalement afin de déterminer la surface du disque obtenu quand la composition hydraulique a fini de s'étaler. On remplit soigneusement à ras un moule tronconique en acier (diamètre intérieur haut = 70 mm, diamètre intérieur bas = 100 mm, hauteur = 60 mm) centré sur la plaque de l'étalomètre en moins de 25 secondes. On retire lentement le moule après 25 secondes et on lit la valeur d'étalement à 30 secondes à l'aide d'une règle graduée par la moyenne des deux diamètres perpendiculaires représentatifs.  - Method of measurement of spreading: The principle of the spreading measurement consists in filling a truncated cone of spreading measurement with the hydraulic composition to be tested and then in releasing said composition from said truncated cone of spreading measurement so as to to determine the disc surface obtained when the hydraulic composition has finished spreading. A steel frustoconical mold (high inner diameter = 70 mm, low inner diameter = 100 mm, height = 60 mm) centered on the plate of the meter in less than 25 seconds is carefully filled flush. The mold is slowly removed after 25 seconds and the spreading value is read at 30 seconds using a ruler graduated by the average of the two representative perpendicular diameters.
- Méthode de mesure de la viscosité (écoulement) : La mesure de la viscosité consiste à mesurer le temps d'écoulement de la composition hydraulique à tester au travers d'un tronc de cône de mesure de viscosité. Le tronc de cône de mesure de viscosité a les dimensions suivantes :  - Viscosity measurement method (flow): The measurement of the viscosity consists in measuring the flow time of the hydraulic composition to be tested through a viscosity measurement truncated cone. The viscosity measuring truncated cone has the following dimensions:
diamètre haut (grand diamètre) = 149 mm  high diameter (large diameter) = 149 mm
diamètre bas (petit diamètre) = 17 mm  low diameter (small diameter) = 17 mm
Hauteur = 190 mm  Height = 190 mm
Le tronc de cône de mesure de viscosité comprend en outre des premier et second repères qui peuvent être des marques parallèles prévues sur la paroi du tronc de cône et définissant des plans perpendiculaires à l'axe du tronc de cône. La première marque est plus proche de la base de plus grand diamètre que la seconde marque. La distance entre les deux repères est de 60 mm, le premier repère se trouvant à 12 mm de la base de plus grand diamètre.  The viscosity measurement truncated cone further comprises first and second indicia which may be parallel marks provided on the wall of the truncated cone and defining planes perpendicular to the truncated cone axis. The first mark is closer to the base of larger diameter than the second mark. The distance between the two marks is 60 mm, the first mark being 12 mm from the larger diameter base.
- Méthode de mesure du temps de prise : la réaction d'hydratation des semi-hydrates est une réaction exothermique qui va entraîner une élévation de la température des chapes. Cette augmentation de température sera enregistrée grâce à un enregistreur de température TESTO. On trace le graphique de l'évolution de la température en fonction du temps et le temps de prise se lit à l'abscisse où le pic de la courbe est maximum.  - Method of measuring the setting time: the hydration reaction of the semi-hydrates is an exothermic reaction which will cause an increase in the temperature of the screeds. This increase in temperature will be recorded thanks to a TESTO temperature recorder. The graph of the evolution of temperature as a function of time is plotted and the setting time is read at the abscissa where the peak of the curve is maximum.
L'eau efficace est l'eau requise pour l'hydratation d'un liant hydraulique et la fluidité d'une composition hydraulique à l'état frais. L'eau totale représente la totalité de l'eau présente dans le mélange (au moment du malaxage) et comprend l'eau efficace et l'eau absorbée par les granulats. L'eau efficace et son mode de calcul sont discutés dans la norme EN 206-1 d'octobre 2005, page 17, paragraphe 3.1.30. Effective water is the water required for the hydration of a hydraulic binder and the fluidity of a hydraulic composition in the fresh state. Total water represents all of the water present in the mixture (at the time of mixing) and includes the effective water and the water absorbed by the aggregates. Efficient water and its method of calculation are discussed in the EN 206-1 standard of October 2005, page 17, paragraph 3.1.30.
La quantité d'eau absorbable se déduit du coefficient d'absorption des granulats qui est mesuré selon la norme NF EN 1097-6 de juin 2001 page 6 paragraphe 3.6 et l'annexe B associée. Le coefficient d'absorption d'eau est le rapport de l'augmentation de masse d'un échantillon de granulats par rapport à sa masse sèche, l'échantillon étant initialement sec puis immergé pendant 24 heures dans l'eau. L'augmentation de masse est due à la pénétration de l'eau dans les pores des granulats accessibles à l'eau.  The amount of absorbable water is deduced from the absorption coefficient of the aggregates which is measured according to standard NF EN 1097-6 of June 2001 page 6 paragraph 3.6 and the associated appendix B. The water absorption coefficient is the ratio of the mass increase of a sample of aggregates to its dry mass, the sample being initially dry and then immersed for 24 hours in water. The increase in mass is due to the penetration of water into the pores of the aggregates accessible to water.
Les exemples suivants, non-restrictifs, illustrent des exemples de réalisation de l'invention. The following non-restrictive examples illustrate exemplary embodiments of the invention.
EXEMPLES EXAMPLES
Sable 0/1,6 Cassis Lafarge, site de Cassis, France  Sand 0 / 1.6 Cassis Lafarge, Cassis site, France
Sable 1,6/3 Cassis Lafarge, site de Cassis, France  Sand 1.6 / 3 Cassis Lafarge, Cassis site, France
TiBP antimousse, tri phosphate butylique  TiBP antifoam, triphosphate butyl
Vinapor antimousse, Vinapor ® DF9010, fabriqué par BASF Vinapor antifoam, Vinapor ® DF9010, manufactured by BASF
R&D retardateur, HYCON R 7200, fabriqué par BASFR & D self-timer, HYCON R 7200, manufactured by BASF
PCE239 superplastifiant, Melflux PCE239L, fabriqué par PCE239 superplasticizer, Melflux PCE239L, manufactured by
BASF  BASF
qsp quantité suffisante pour qsp sufficient quantity for
Exemple 1 : comparaison de formules comprenant du plâtre β ou de l'anhydrite Example 1 Comparison of Formulas Comprising Plaster β or Anhydrite
Tableau 1  Table 1
' après agitation pour simuler le camion toupie  'after shaking to simulate the truck spinning
Cet exemple illustre l'importance du degré de déshydratation du sulfate de calcium.  This example illustrates the importance of the degree of dehydration of calcium sulphate.
Lorsque le sulfate de calcium est totalement hydraté (l'anhydrite), il n'est pas possible de formuler une composition pour chape. En effet, la rhélogie de la composition n'est pas acceptable puisque le mélange ségrège et les résistances mécaniques sont très faibles et bien en dessous des valeurs requises en utilisation. Exemple 2 : Impact de la nature du sable When calcium sulfate is fully hydrated (anhydrite), it is not possible to formulate a screed composition. Indeed, the rhelogy of the composition is not acceptable since the mixture segregates and the mechanical strengths are very low and well below the values required in use. Example 2: Impact of the nature of the sand
Deux sables, un calcaire et un siliceux, ont été testés. Le tableau ci-dessous compare les deux sables dans une formule chape : Two sands, a limestone and a siliceous, were tested. The table below compares the two sands in a screed formula:
Tableau 2  Table 2
' après agitation pour simuler le camion toupie  'after shaking to simulate the truck spinning
Les deux formulations permettent de préparer des chapes répondant aux spécifications. On note toutefois que les compositions à base de sable calcaire sont plus économiques. En effet, avec le sable calcaire, la quantité d'adjuvant est moins importante (baisse d'environ 40%>) qu'avec le sable siliceux. Les résistances mécaniques sont en outre plus importantes avec le sable calcaire.  Both formulations make it possible to prepare screeds that meet the specifications. However, it is noted that compositions based on calcareous sand are more economical. In fact, with calcareous sand, the amount of admixture is less important (about 40% decrease) than with siliceous sand. The mechanical strengths are also more important with the calcareous sand.
Exemple 3 : Impact de la quantité de liant On a analysé l'effet de la variation de la quantité de liant en ne modifiant pas la quantité d'eau. Les résultats sont reportés dans le tableau suivant : 30°C Example 3 Impact of the amount of binder The effect of varying the amount of binder was analyzed by not modifying the amount of water. The results are reported in the following table: 30 ° C
sable (kg/m ) 1325,8 1406,3 1457,9 1507,8 plâtre β (kg/m ) 575 500 450 400 sand (kg / m) 1325.8 1406.3 1457.9 1507.8 plaster β (kg / m) 575 500 450 400
PCE 239 (%/plâtre) 0,63 0,60 0,57 0,58  PCE 239 (% / plaster) 0.63 0.60 0.57 0.58
R&D (%/plâtre) 0,15 0,20 0,20 0,20  R & D (% / plaster) 0.15 0.20 0.20 0.20
CaO (%/plâtre) 0,1 0,1 0,1 0,1  CaO (% / plaster) 0.1 0.1 0.1 0.1
TiBP (%> superplastifïant sec) Qqs gouttes 4,3 4,3 4,3  TiBP (%> superplasticizer dry) Qq drops 4.3 4.3 4.3
Eeffïcace (Eeff) 273,2 272,8 272,6 272,3 Eeffïcace (E eff) 273.2 272.8 272.6 272.3
Eeff/Plâtre 0,475 0,546 0,606 0,681  Eeff / Plaster 0.475 0.546 0.60 0.681
Eau totale (L/m3) 280 280 280 280 Total water (L / m 3 ) 280 280 280 280
Propriétés rhéo logiques à 5 min(1) Rheological properties at 5 min (1)
Etalement (mm) 255 270 230 240  Spreading (mm) 255 270 230 240
Ecoulement (s) 15 15 18 16  Flow 15 15 18 16
Temps de prise (h) 12,6 13,2 11 8,5  Set time (h) 12.6 13.2 11 8.5
Résistances mécaniques à 28j  Mechanical resistances at 28 days
Flexion (MPa) 6,4 5,9 5,1 3,8  Flexion (MPa) 6.4 5.9 5.1 3.8
Compression (MPa) 28 22 17 14  Compression (MPa) 28 22 17 14
Densité  Density
2,04 2,05 2,02 2,02  2.04 2.05 2.02 2.02
Tableau 3  Table 3
' après agitation pour simuler le camion toupie  'after shaking to simulate the truck spinning
Le sable est une coupure 73/27 de sable 0/1,6 Cassis et de sable 1,6/3 Cassis. Le plâtre est un plâtre français, Prestia 2500, de forme cristalline β. La diminution de la quantité de liant ne changeant pas la quantité d'eau fait augmenter le rapport Eff/plâtre et permet de réaliser des chapes qui rentrent dans le cahier des charges au niveau de la rhéologie tout en diminuant la quantité d'adjuvant. La diminution de la quantité de plâtre fait baisser les résistances mécaniques. Ainsi, en fonction des propriétés mécaniques recherchées, le formulateur pourra faire varier la quantité de liant en l'augmentant pour augmenter les propriétés mécaniques ou en la diminuant pour diminuer les propriétés mécaniques. Exemple 4 : remplacement d'une partie du plâtre par une charge The sand is a cut 73/27 of sand 0 / 1.6 Cassis and sand 1.6 / 3 Cassis. Plaster is a French plaster, Prestia 2500, crystalline form β. The decrease in the amount of binder does not change the amount of water increases the ratio Eff / plaster and allows to make screeds that fall within the specifications at the level of rheology while reducing the amount of adjuvant. The reduction in the amount of plaster reduces the mechanical resistance. Thus, depending on the desired mechanical properties, the formulator may vary the amount of binder by increasing it to increase the mechanical properties or by decreasing it to reduce the mechanical properties. Example 4: Replacement of a part of the plaster with a load
On a analysé l'effet de la substitution d'une partie du plâtre par une charge calcaire. Les résultats sont reportés dans le tableau suivant : The effect of replacing part of the plaster by a calcareous load was analyzed. The results are reported in the following table:
Tableau 4  Table 4
' après agitation pour simuler le camion toupie  'after shaking to simulate the truck spinning
Le sable est une coupure 73/27 de sable 0/1,6 Cassis et de sable 1,6/3 Cassis. Le plâtre est un plâtre français, Prestia 2500, de forme cristalline β. The sand is a cut 73/27 of sand 0 / 1.6 Cassis and sand 1.6 / 3 Cassis. Plaster is a French plaster, Prestia 2500, crystalline form β.
Il est possible de formuler des chapes comprenant une substitution de 275kg de charge pour 300kg de plâtre. Les résistances diminuent en conséquence. En fonction des résistances recherchées, une substitution avec une charge peut ainsi être envisagée. La substitution permet également de diminuer la quantité en superplastifïant. Ainsi, pour diminuer les propriétés mécaniques, le formulateur pourra substituer une partie du liant par une charge inerte. Exemple 5 : Coulage de 50m2 à une température ambiante de 39°C It is possible to formulate screeds comprising a substitution of 275kg of load for 300kg of plaster. The resistances diminish accordingly. Depending on the resistances sought, a substitution with a load can thus be envisaged. The Substitution also reduces the amount of superplasticizer. Thus, to reduce the mechanical properties, the formulator may substitute a portion of the binder with an inert filler. Example 5: Pouring 50m 2 at an ambient temperature of 39 ° C.
On a réalisé 4m3 de chape dans un camion toupie à la centrale en dry batch (discontinu à sec). 4m 3 of screed was made in a dry truck at the central dry batch (dry batch).
La formulation est la suivante :  The wording is:
- 680 kg de sulfate de calcium semi- hydrate, β, au m3 - 680 kg of calcium sulphate semihydrate, β, m 3
300 litres d'eau totale au m3 300 liters of total water per m 3
28 litres de superplastifïant BASF MasterGlenium Sky 504 au m3 (Extrait sec : 48% 2,35% de superplastifïant sec/plâtre) 28 liters of BASF MasterGlenium Sky 504 superplasticizer per m 3 (dry extract: 48% 2.35% dry superplasticizer / plaster)
0,5 kg de retardateur Plastretard PE (poudre) de la société Sicit 2000 au m3 (0,074%> de retardateur sec/plâtre) 0.5 kg of retarder PE plastard (powder) from Sicit 2000 to m 3 (0.074%> dry retarder / plaster)
0,65 kg d'agent antimousse BASF Master Roc DF 880 au m3 (4,3% / superplastifïant sec) 0.65 kg of antifoam BASF Master Roc DF 880 per m 3 (4.3% / dry superplasticizer)
1 ,35 kg de CaO au m3 (0,2%/plâtre) 1.35 kg of CaO per m 3 (0.2% / plaster)
1195 kg de sable humide (5,1% d'humidité) (sable siliceux)  1195 kg wet sand (5.1% moisture) (siliceous sand)
Les composants sont ajoutés directement dans le camion dans l'ordre suivant : The components are added directly to the truck in the following order:
80%) de l'eau à ajouter moins 50 litres  80%) of the water to add less 50 liters
le superplastifïant  the superplasticizer
le retardateur  the self-timer
- Γ antimousse  - Γ antifoam
50%) de sulfate de calcium semi- hydrate  50%) of calcium sulphate semi-hydrate
le régulateur de pH : CaO poudre  pH regulator: CaO powder
50%o de sulfate de calcium semi- hydrate  50% o calcium sulphate semi-hydrate
50 litres d'eau pour le rinçage de la trémie du camion  50 liters of water for rinsing the truck hopper
- le sable humide  - wet sand
20%o de l'eau restant  20% o of the remaining water
Résultats (T0 =premier contact eau/plâtre) : O A T0+40min, sur un prélèvement à la sortie du camion, une température de pâte à 38°C et un produit homogène Results (T0 = first contact water / plaster): OA T0 + 40min, on a sample at the end of the truck, a paste temperature at 38 ° C and a homogeneous product
Etalement = 265mm Spread = 265mm
Temps d'écoulement (viscosité) de l'ordre de 16 secondes  Flow time (viscosity) of the order of 16 seconds
Une fluidité correcte et une bonne stabilité de la pâte (pas de ségrégation).  Correct fluidity and good stability of the dough (no segregation).
A T0=50min, réalisation de plusieurs cube 15x15cm pour des mesures des résistances mécaniques (après séchage).  At T0 = 50min, realization of several 15x15cm cube for measurements of the mechanical strengths (after drying).
O A T0+1H, sur le même prélèvement ayant subi un malaxage haute énergie (simulation d'une pompe à vis). Une température de pâte à 38°C O TO T0 + 1H, on the same sample having undergone high energy mixing (simulation of a screw pump). Paste temperature at 38 ° C
Etalement = 200mm Spread = 200mm
Temps d'écoulement de l'ordre de 23 secondes.  Flow time of about 23 seconds.
Un produit homogène  A homogeneous product
Une arrivée sur le chantier à T0+2H30  An arrival on the building site at T0 + 2H30
O A T0+2H50, sur un prélèvement à la sortie du camion, une température de pâte à 38,5°C et un produit homogène O A T0 + 2H50, on a sample at the end of the truck, a paste temperature at 38.5 ° C and a homogeneous product
Etalement = 265mm Spread = 265mm
Temps d'écoulement de l'ordre de 24 secondes  Flow time of about 24 seconds
Un produit homogène et ayant une bonne stabilité. A homogeneous product with good stability.
O Un début de coulage à la centrale à T0+3H : O A pouring start at the plant at T0 + 3H:
Un passage dans une pompe à piston (diamètre sortie pompe = 7cm) sans problème Etalement après pompage à T0+3H05 = 250mm A passage in a piston pump (pump outlet diameter = 7cm) without problem Spreading after pumping at T0 + 3H05 = 250mm
Temps d'écoulement (viscosité) à T0+3H05 de l'ordre de 19 secondes Flow time (viscosity) at T0 + 3H05 of the order of 19 seconds
Un produit homogène. Un produit autoplaçant. Aspect de produit très correct après coulage. Une belle finition après le passage de la « barre ». A homogeneous product. A self-placing product. Product appearance very correct after pouring. A nice finish after the passage of the "bar".
Prélèvement une heure après le début du coulage : Etalement = 250mm ; Tps d'Ecoulement = 24s (Température 39°C).  Sampling one hour after start of pouring: Spread = 250mm; Flow time = 24s (Temperature 39 ° C).
Fin du coulage à T0+4H10. End of the casting at T0 + 4H10.
Prise de la chape le lendemain soit un temps de prise < 24H  Taking the screed the next day is a setting time <24H
Aspect après prise : Très correct Résultats résistances mécaniques : résistance à la compression sur cube 15x15x15 cm: Rc à 11 jours (échantillons non séchés) =10 MPa Appearance after taking: Very correct Mechanical resistance results: compressive strength on cube 15x15x15 cm: Rc at 11 days (samples not dried) = 10 MPa
Rc à 28 jours (séchage complet atteint après 11 jours en étuve à 45°C) = 25 MPa  Rc at 28 days (complete drying after 11 days in an oven at 45 ° C) = 25 MPa

Claims

REVENDICATIONS
Utilisation de plâtre, sous sa forme cristalline β, pour la préparation d'une composition de chape de sol, comprenant également du sable et un superplastifiant, destinée à être coulée à une température supérieure ou égale à 30°C. Use of plaster, in its crystalline form β, for the preparation of a floor screed composition, also comprising sand and a superplasticizer, intended to be cast at a temperature greater than or equal to 30 ° C.
Utilisation selon la revendication 1 , dans laquelle la composition comprend un liant hydraulique comprenant en masse au moins 52% de plâtre et de 0% à 48% de charge, la somme de ces deux pourcentages variant de 80%> à 100%. Use according to claim 1, wherein the composition comprises a hydraulic binder comprising at least 52% by weight of plaster and from 0% to 48% filler, the sum of these two percentages varying from 80%> to 100%.
Utilisation selon l'une quelconque des revendications précédentes, dans laquelle le pH du plâtre dans l'eau, mesuré à un rapport massique eau/poudre de plâtre = 0,487, est ajusté à un pH allant de 10 à 13. Use according to any one of the preceding claims, wherein the pH of the plaster in water, measured at a mass ratio water / plaster powder = 0.487, is adjusted to a pH ranging from 10 to 13.
Utilisation selon l'une quelconque des revendications précédentes, dans laquelle le superplastifiant est un éther de polycarboxylate. Use according to any one of the preceding claims, wherein the superplasticizer is a polycarboxylate ether.
Utilisation selon l'une quelconque des revendications précédentes, dans laquelle la composition comprend également un retardateur. Use according to any one of the preceding claims, wherein the composition also comprises a retarder.
Utilisation selon l'une quelconque des revendications précédentes, dans laquelle la composition comprend également un agent antimousse. Use according to any one of the preceding claims, wherein the composition also comprises an antifoaming agent.
Utilisation selon l'une quelconque des revendications précédentes, dans laquelle la composition comprend de la chaux. Use according to any one of the preceding claims, wherein the composition comprises lime.
Utilisation selon l'une quelconque des revendications précédentes, dans laquelle la composition de chape comprend, par mètre cube de composition à l'état frais : Use according to any one of the preceding claims, wherein the screed composition comprises, per cubic meter of composition in the fresh state:
— De 450 à 700 kg d'un liant hydraulique comprenant en masse au moins 52%> de plâtre et de 0%> à 48%> de charge, la somme de ces deux pourcentages variant de 80%> à 100% — de 250 à 350 litres d'eau, le rapport entre la masse d'eau et la masse de liant hydraulique étant de 0,4 à 0,7; 450 to 700 kg of a hydraulic binder comprising in mass at least 52% gypsum and 0% to 48% by weight, the sum of these two percentages varying from 80% to 100% From 250 to 350 liters of water, the ratio between the mass of water and the mass of hydraulic binder being from 0.4 to 0.7;
— un superplastifiant,  - a superplasticizer,
— un retardateur,  - a self-timer,
— éventuellement de la chaux  - possibly lime
— éventuellement un agent antimousse  Optionally an antifoaming agent
— du sable en une quantité suffisante pour avoir 1 m3 - sand in sufficient quantity to have 1 m 3
9. Utilisation selon l'une quelconque des revendications précédentes, dans laquelle la composition de chape comprend, de 0,5 à 2,5% de superplasitifîant, pourcentages exprimés en poids d'extrait sec de superplastifiant par rapport au poids du plâtre. 9. Use according to any one of the preceding claims, wherein the screed composition comprises, from 0.5 to 2.5% superplasticizer, percentages by weight of superplasticizer solids by weight of plaster.
10. Utilisation selon l'une quelconque des revendications précédentes, dans laquelle la composition de chape comprend de 0,05 à 0,2%> de retardateur, pourcentages exprimés en poids d'extrait sec de retardateur par rapport au poids du plâtre. 10. Use according to any one of the preceding claims, wherein the screed composition comprises from 0.05 to 0.2%> retarder, percentages expressed by weight of retarder dry extract relative to the weight of the plaster.
11. Utilisation selon l'une quelconque des revendications précédentes, dans laquelle la composition de chape comprend de 0,1 à 0,2%> de CaO, pourcentages exprimés en poids d'extrait sec par rapport au poids du plâtre. 11. Use according to any one of the preceding claims, wherein the screed composition comprises from 0.1 to 0.2% of CaO, percentages expressed by weight of dry extract relative to the weight of the plaster.
EP17724382.1A 2016-05-23 2017-05-23 Use of plaster for manufacturing a self-leveling underlayment for hot countries Withdrawn EP3464213A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR1654591A FR3051462A1 (en) 2016-05-23 2016-05-23 USE OF PLASTER FOR THE MANUFACTURE OF A FLUID CAP FOR HOT COUNTRIES
PCT/EP2017/062326 WO2017202801A1 (en) 2016-05-23 2017-05-23 Use of plaster for manufacturing a self-leveling underlayment for hot countries

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Publication Number Publication Date
EP3464213A1 true EP3464213A1 (en) 2019-04-10

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EP (1) EP3464213A1 (en)
CA (1) CA3025254A1 (en)
FR (1) FR3051462A1 (en)
MA (1) MA45085A (en)
WO (1) WO2017202801A1 (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3937431A1 (en) * 1989-11-10 1991-05-16 Knauf Westdeutsche Gips Wear layer for working floors - comprises sand-limestone aggregate and binder contg. alpha-hemi:hydrate, low-alumina cement, plastic dispersion, fine silica and additives
ES2376778T3 (en) 2004-09-21 2012-03-16 Lafarge Impurity inertization procedure
ATE532757T1 (en) 2004-09-21 2011-11-15 Lafarge Sa COMPOSITIONS FOR INERTIFYING CONTAMINANTS
DE202007003608U1 (en) * 2007-03-10 2008-07-24 Knauf Gips Kg Dry mortar for the production of a quick screed
FR2948118A1 (en) 2009-07-17 2011-01-21 Coatex Sas Additive, useful as dispersing agent and inerting agent of clays, for aqueous suspensions of calcium sulfate hemihydrate containing clay and for the manufacture of natural gypsum board, comprises an anionic and cationic comb polymer
FR2995604B1 (en) * 2012-09-17 2017-04-21 La Chape Liquide NEW HYDRAULIC BINDER-BASED CAP WITH ENHANCED THERMAL CONDUCTIVITY

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WO2017202801A1 (en) 2017-11-30
CA3025254A1 (en) 2017-11-30
MA45085A (en) 2019-04-10

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