• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The present invention relates to a hydraulic binder comprising at least 80% by weight of a crushed granulated blast furnace slag and at least one accelerator of the curing reaction, said accelerator comprising at least one source of calcium sulfate and at least one a nucleating agent in the form of particles whose BET specific surface area is greater than 1 m 2 / g and the size of which is such that 50% of the particles have an average diameter of less than 5 μm, the said particles being chosen from calcium carbonates, magnesium carbonates, calcium and magnesium carbonates, calcium silicate hydrates, aluminum silicate hydrates, alone or in admixture. This binder can be used in a mortar and concrete composition which, when spoiled with water provides building materials.
    公开号:FR3051461A1
    申请号:FR1654401
    申请日:2016-05-18
    公开日:2017-11-24
    发明作者:Udo Dudda；Franck Hesselbarth
    申请人:Saint Gobain Weber SA；
    IPC主号:
    专利说明:

    BINDER BASED ON CALCIUM ALUMIN09LICATE DERIVATIVES FOR CONSTRUCTION MATERIALS
    The present invention relates to a hydraulic binder based on calcium aluminosilicate derivatives, in particular based on blast furnace slags, used for building materials, mortar or concrete compositions comprising said binder, as well as building materials. obtained from these compositions.
    Most of the environmental problems related to the production of cement concern the manufacture of clinker which requires calcination and heating operations, especially at very high temperatures, of the order of 1450 ° C. The production of one ton of Portland cement generates between 0.7 and 1 ton of carbon dioxide. Many efforts are therefore made to reduce the carbon footprint of cement and one of the solutions envisaged is to use raw materials or substitute binders based on industrial waste. It is possible to reduce the clinker content of cement by incorporating cement additions such as pozzolanic fly centers, ground granulated blast furnace slag, silica fume or metakaolin to make composite cements, often referred to as blending cements. . Such cements are in particular described in standard EN197-1 which defines the specifications of 27 common cements and their constituents.
    Because of high reactivity and reduced carbon dioxide emissions, cements including slags and / or fly ash are particularly attractive. Blast furnace slag is a by-product of iron making from iron ore; it corresponds to the sterile gangue of iron ore, isolated from liquid iron by density difference. The molten slag is lighter and floats on the liquid steel bath. A blast furnace slag essentially comprises silicates or silicoaluminates of lime. The vitrified slag obtained by the sudden cooling of the molten slag using high-pressure water jets has a glassy structure. This allows him to develop hydraulic properties: it is called granulated slag with a particle diameter of less than 5 mm. Granulated slags can be finely ground after drying and used in the cement industry. Most milled granulated blast furnace slags have a fineness of between 3800 and 4500 cm2 / g (also expressed in Hate units).
    EMI / A-§ cements also referred to as PortIand slag cements contain 65 to 94% clinker and 6 to 35% ground granulated blast furnace slag. CEMIII / A-B-C cements or blast furnace cements contain 36 to 95% slag and 5 to 64% clinker. Recent work has shown that it is possible to replace more than 95% of Portland cement with ground granulated blast furnace slag, or even to use this slag as a binder for building materials. For example, patent FR-B-2 952 050 describes efficient binders based on ground granulated blast furnace slag, which can be used under "mild" conditions, that is to say without requiring the use of a strongly basic activator system and therefore dangerous to handle. The proposed solution is to use slag microparticles with a fineness greater than 6000 Haine as an activator, in the presence of a very small amount of base. However, with this type of system, especially in low temperature conditions combined with a relatively high humidity, the curing and curing times of the binder remain too low due to a slow rate of hydration.
    US-B1-6,451,105 discloses a cementitious composition comprising Portland cement optionally substituted with blast furnace slags and / or fly ash, in which a ground limestone setting accelerator is added at 150 μm. The type of activation proposed in this document is not sufficient, when the essential constituent of the binder is a dairy-type calcium aluminosilicate derivative and / or fly ash. Indeed, the systems described in this patent all contain at least 40% Portland cement, which therefore significantly contributes to the hydraulic setting mechanism of the mixture cements described.
    We have therefore sought to develop an activation system that effectively activates slags, known to be unreactive compared to other hydraulic binders.
    The present invention relates to a hydraulic binder comprising predominantly a calcium aluminosilicate derivative and at least one accelerator of the binder hardening reaction which is not classified in the group of irritating or corrosive products according to Directive 91/155 / EEC and which keeps its accelerator properties, even in low temperature conditions. Another subject of the invention concerns a mortar or concrete composition comprising such a binder. The binder according to the present invention advantageously makes it possible to obtain in the short term (start of setting) good mechanical performance.
    The present invention also relates to building materials such as adhesives for tiles, jointing mortars, masonry mortars, screeds, coatings or wall coverings obtained from the mortar or concrete compositions above.
    The hydraulic binder according to the present invention comprises at least 80% by weight of a ground granulated blast furnace slag and at least one accelerator of the hardening reaction comprising at least one calcium sulphate source and at least one nucleating agent. in the form of particles whose BEI "surface area is greater than 1 m 2 / g and the size of which is such that 50% of the particles have an average diameter of less than 5 μm, the said particles being chosen from calcium carbonates, carbonates from magnesium, calcium and magnesium carbonates, calcium silicate hydrates, aluminum silicate hydrates, alone or as a mixture.
    The nucleating agents advantageously make it possible to accelerate the hydration of the hydraulic binder, especially at a relatively low temperature, without requiring the addition of other often toxic additives. It is necessary that at least 50% of the nucleating agent particles have an average diameter of less than 5 μm. These nucleating agents play their role of germs all the better because they are as thin as possible and have a high specific surface area greater than 1 m 2 / g.
    Part of the crushed granulated blast furnace slag may be substituted by another derivative of calcium aluminosilicates and in particular F class (silico-aluminous) and / or class C (co-aluminous alcohols) fly ash. ), or expanded or calcined clay dust. The difference between class F and class C fly ash lies in their respective calcium content. Class F fly ash contains less than 8% calcium and is less reactive than Class C fly ash. Up to 50% by weight of the ground granulated blast furnace slag in the binder can be substituted. by Class F or C fly ash.
    In one embodiment, the binder according to the invention comprises at least 80% by weight, preferably between 85 and 98% by weight of a mixture consisting of ground granulated blast furnace slag and class C or F fly ash. This mixture can be 50/50 type. Preferably, when a portion of the crushed granulated blast furnace slag is replaced by fly ash, the ratio of slag to fly ash varies between 50/50 and 90/10. A ratio of milk to fly ash of 70/30 is particularly advantageous.
    In another embodiment, the binder according to the invention comprises at least 80% by weight, preferably between 85 and 98% by weight of ground granulated blast furnace slag.
    The binder according to the present invention may further comprise up to 15% by weight of another hydraulic binder selected from Portland cements, aluminous cements, sulfoaluminous cements, belitic cements, pozzolanic mix cements, taken alone or in mixed. Preferably, the amount of this type of hydraulic binder is less than or equal to 10% by weight, or even less than or equal to 5% by weight.
    The binder according to the present invention also comprises at least one accelerator of the curing reaction. Indeed, it is necessary, since the binders based on calcium aluminosilicate derivatives are binders considered to be not very hydraulic, to add an accelerator which comprises at least one source of calcium sulphate and at least one dehydrating agent. nucleation which promotes the hydration of the binder due to the presence of germs acting as activator.
    The source of calcium sulphate is chosen from gypsum, calcium sulfate hemihydrate, anhydrite and phosphogypsum, alone or as a mixture, in an amount of between 1 and 5% by weight relative to the total weight of binder. . Preferably, the amount of calcium sulphate source is between 2 and 4% by weight of the total weight of binder. The source of calcium sulphate, in such an amount, makes it possible to control the activation at the beginning of the reaction and to ensure sufficient entrapment of the water, while avoiding a too much late formation of ettringite which would result in a weakening of the material after the steps of setting the binder.
    The amount of nucleating agent present in the hydraulic binder according to the present invention is between 0.1 and 20% of the total weight of the binder. The nucleating agent is a powdery agent whose particle size is such that 50% of the particles have an average diameter of less than 5 μm. Activation is particularly enhanced when the particles are small. Indeed, the more the germs are fine, the more they are reactive. They are chosen from calcium carbonates, magnesium carbonates, calcium and magnesium carbonates, calcium silicate hydrates, aluminum silicate hydrates, alone or as a mixture. These seeds can be obtained for example by precipitation and / or grinding.
    The nucleating agent particles are characterized by their specific surface area (BET surface expressed in m 2 / g) and by the median diameter D 50 which corresponds to the size for which 50% of the population of particles has a size less than D 50.
    Advantageously, the nucleating agent is chosen from ground or precipitated natural calcium and / or magnesium carbonates whose BET specific surface area is greater than 4 m 2 / g. precipitated calcium and / or magnesium carbonates are preferred.
    It can also be a hydrated calcium silicate hydrate whose BET surface area is greater than 2.5 m 2 / g. The nucleating agent may also be a finely ground zeolite. By choosing a nucleating agent as described above, it is possible to obtain an activation system that functions quite well for binders that are considered to be poorly hydraulic and therefore not very reactive.
    When the nucleating agent is chosen from calcium silicate hydrates and aluminum silicate hydrates, the amount of nucleating agent is advantageously between 0.2 and 3% by weight relative to the total weight of the binder. . This amount is relatively small compared to the activation systems known in the prior art and in particular with respect to the solution proposed in the patent application WO 2011/055063 which provides for adding up to 11% by weight, relative to to the total weight of binder, slag microparticles.
    When the activating agent is of carbonate type, it may be necessary to add up to 20% of the total weight of the binder to obtain a satisfactory activation. The amount of calcium and / or magnesium carbonates therefore varies between 0.2 and 20% by weight relative to the weight of the total binder. The accelerator may also comprise one or more alkali metal sulphates, chosen from lithium, sodium and / or potassium, preferably in an amount of less than or equal to 0.5% by weight relative to the total weight of the binder. Even more preferentially, the accelerator comprises between 0.2 and 0.4% by weight relative to the total weight of the binder of alkali metal sulphates. The sulphates advantageously promote the binding of the binder and are particularly favorable when they are associated with a source of calcium sulphate. The activator may optionally comprise a small amount of a pH regulating agent chosen from alkali metal silicates or carbonates, in an amount of less than or equal to 0.5% by weight relative to the total weight of the binder, and preferably in an amount between 0.2 and 0.4% of the total weight of the binder. The activator may comprise an additive acting as a chemical activator, especially chosen from calcium nitrate, calcium formate or hydraulic binders such as Portland cement or aluminous and / or sulfoaluminous cements as mentioned above. The amount of chemical activator is less than or equal to 5% of the total weight of the binder, preferably less than or equal to 4% of the total weight of the binder. If the chemical activator is a hydraulic binder, it can be added in addition to the amount that can be introduced as the hydraulic binder mentioned above.
    The activation system according to the present is a gentle activation system, based on products in powder form easily to make pre-mixtures or premixes ready for use and containing no irritating and corrosive substances.
    The hydraulic binder according to the present invention can be hydrated at low temperatures (winter conditions) or at high temperatures, depending on the desired applications.
    The present invention also relates to a mortar or concrete composition comprising the binder described above in association with fillers, films, sand and / or granulates. The fillers can be low density, mineral or organic leaching fillers such as expanded perlite, expanded vermiculite, expanded glass beads, hollow glass microspheres, cenospheres, expanded clays, expanded shales, pumice stones , expanded polystyrene. The films are conventionally of the siliceous, limestone and / or silico-calcareous type and have a particle size of up to 150 μm. aggregates or sands whose particle size varies between 100 pm and 5 mm allow to play on the thickness, the hardness, the final appearance and the permeability of the mortar.
    The mortar or concrete composition according to the present invention may also further comprise one or more additives, chosen from rheological agents, water-retaining agents, air-entraining agents, thickening agents, biocidal protection agents, dispersants, pigments, accelerators and / or retarders. The rheological agents may especially be plasticizers, for example products based on polycarboxylic acids such as polycarboxylic ethers, lignosulphonates, polynaphthalenesulfonates, melamine superplasticizers, polyacrylates and / or vinyl copolymers, ethers. optionally modified cellulose. These additives when present each represent less than 1% of the total weight of the mortar composition.
    The present invention also relates to building materials, particularly adhesive mortars or adhesives for tiles, obtained by mixing the mortar composition described above with water. The adhesives thus obtained very advantageously have a very satisfactory short-term (that is to say after 24 hours) curing. The adhesion strength performance of adhesives according to the present invention meet the specifications for being classified as C2TE-S1 according to EN 12004: 2007.
    Building materials can also be grouting mortars that fill existing gaps between different masonry elements. They may also be screeds, facings mortars such as patching mortars, under-plaster, monolayer coatings, organic facing mortars and waterproofing mortars.
    The examples below illustrate the invention without limiting its scope.
    Example 1
    A tile adhesive formulation comprising a binder whose main constituent is a ground granulated blast furnace slag with an accelerator system comprising hydrated calcium silicate seeds according to the present invention has been prepared by mixing the various constituents given in the present invention. Table 1 below.
    Table 1
    A pasty preparation of creamy consistency is obtained by adding 25% of water to this powdery composition at a temperature of about 22.1 ° C.
    Various tensile strength tests to determine adhesion of the adhesive mortar thus obtained have been made according to the EN 1348 standard.
    Tile pieces are fixed on a flat support by applying a layer of the obtained adhesive mortar. The tearing resistance expressed in N / mm 2 is measured by tearing after 1 day, 7 days and 28 days of storage under standard conditions, that is to say at a temperature of 23 ° C., with a 50% relative humidity A so-called "wet immersion" measurement is also performed by measuring the tearing after 7 days of storage under standard conditions, followed by 21 days of immersion in water at 23 ° C. A so-called "after freeze-thaw cycle" adhesion measurement is carried out in accordance with EN 12004: 2007, which itself refers to the EN1348: 2007 standard. The samples are subjected to successive cycles of freeze-thaw. A measurement called "after exposure to heat" is performed after 14 days of storage under standard conditions, followed by 14 days of storage at 70 ° C, and again 1 day under standard conditions.
    An adhesion force test was also performed on a piece of earthenware tile which is placed on a flat support, 20 minutes after the application of a layer of mortar adhesive on the tile part and / or on the support plan ; the peel strength is measured by peeling the sample after 28 days of storage under standard conditions. This measure is entitled "after open time 20 min".
    The values obtained for these different measurements are compared with the minimum values required to obtain the desired certification (EN 12004 standard).
    Measurements were also made to measure the deformation resistance of the adhesive mortar used and were compared with the expected values according to EN 12002. All the results obtained are given in Table 2 below.
    Table 2
    The values obtained show that the tests meet the criteria required by the standard.
    Example 2
    A tile adhesive formulation comprising a binder whose main constituent is a ground granulated blast furnace slag with an accelerator system comprising ultrafine particles of magnesium and calcium carbonates according to the present invention has been prepared by mixing the various constituents given in Table 3 below.
    Table 3
    Adhesion tests are carried out as in Example 1. The results obtained are shown in Table 4 below:
    Table 4
    The values obtained show that the tests meet the criteria required by the standard.
    It is also noted for these two examples according to the invention that the measurements of resistance to short times (that is to say, 1 day) are greater than 0.5 N / mm 2, which is particularly interesting for appli cat i ons sought.
    权利要求:
    Claims (16)
    [1" id="c-fr-0001]
    A hydraulic binder comprising at least 80% by weight of a crushed granulated blast furnace slag and at least one accelerator of the hardening reaction characterized in that said accelerator comprises at least one source of calcium sulfate and at least one agent nucleating in the form of particles whose BEI "surface area is greater than 1 m 2 / g and the size is such that 50% of the particles have an average diameter of less than 5 pm, said particles being chosen from calcium carbonates, carbonates magnesium, calcium and magnesium carbonates, calcium silicate hydrates, aluminum silicate hydrates, alone or in admixture.
    [2" id="c-fr-0002]
    2. Binder according to one of the preceding claims characterized in that it comprises between 85 and 98% by weight of a ground granulated blast furnace slag.
    [3" id="c-fr-0003]
    3. Binder according to one of the preceding claims characterized in that an amount of up to 50% of the slag is replaced by fly ash, such as aluminous aluminous fly ash and fly ash if li co-cal co -aluminous, or by dust of calcined or expanded clay.
    [4" id="c-fr-0004]
    4. Binder according to one of the preceding claims characterized in that it further comprises up to 15% by weight of another hydraulic binder selected from Portland cements, aluminous cements, sulfoaluminous cements, belitic cements, pozzolanic mixture cements, taken alone or as a mixture.
    [5" id="c-fr-0005]
    Binder according to one of the preceding claims, characterized in that the amount of nucleating agent represents between 0.1 and 20% of the total weight of the binder.
    [6" id="c-fr-0006]
    Binder according to one of the preceding claims, characterized in that the accelerator further comprises a pH regulating agent chosen from alkali metal silicates or carbonates, in an amount equal to or less than 0.5% of the total weight. binder, preferably from 0.2 to 0.4% by weight of the binder.
    [7" id="c-fr-0007]
    7. hydraulic binder according to one of the preceding claims characterized in that the accelerator further comprises an alkali metal sulfate selected from lithium, sodium and / or potassium in an amount less than or equal to 0.5% total weight, preferably between 0.2 and 0.4% of the weight early al.
    [8" id="c-fr-0008]
    8. Binder according to one of the preceding claims characterized in that the accelerator further comprises a chemical activator selected by calcium nitrate, calcium formate, PortIand cement, calcium sulfoaluminate cement, cement of Calcium aluminate, alone or in admixture, in an amount not exceeding 5% of the total weight.
    [9" id="c-fr-0009]
    9. hydraulic binder according to one of the preceding claims characterized in that the source of calcium sulfate comprises one or more of the elements selected from gypsum calcium sulfate hemihydrate, anhydrite and phosphogypsum, in an amount of between 1 and 5% of the weight early al, preferably between 2 and 4% of the weight early al.
    [10" id="c-fr-0010]
    Binder according to one of the preceding claims, characterized in that the nucleating agent is chosen from ground and precipitated natural calcium and / or magnesium carbonates whose BET specific surface area is greater than or equal to 4 m 2 / g, preferably in an amount of between 0.2 and 20% by weight relative to the weight of the total binder.
    [11" id="c-fr-0011]
    11. Binder according to the preceding claim characterized in that the nucleating agent is a precipitated calcium carbonate and / or magnesium carbonate.
    [12" id="c-fr-0012]
    12. Binder according to one of claims 1 to 9 characterized in that the nucleating agent is a zeolite.
    [13" id="c-fr-0013]
    13. Binder according to one of claims 1 to 9 characterized in that the nucleating agent is a hydrated calcium silicate hydrate whose BET surface area is greater than or equal to 2.5 m2 / g, preferably in a amount between 0.2 and 3% by weight relative to the weight of the total binder.
    [14" id="c-fr-0014]
    14. Concrete composition or mortar characterized in that it comprises at least one binder according to one of the preceding claims, optionally leaching loads, sand, granules, fillers.
    [15" id="c-fr-0015]
    15. Composition according to claim 14, characterized in that it further comprises one or more additives, chosen from rheological agents, water-retaining agents, air-entraining agents, thickening agents and biocidal protection agents. dispersants, pigments, accelerators and / or retarders.
    [16" id="c-fr-0016]
    16. Building materials such as tile adhesives, jointing mortars, masonry mortars, screeds, smoothing mortars, sub-coatings, single-ply coatings, organic facing mortars, waterproofing mortars obtained by mixing with water of the mortar or concrete composition according to one of claims 14 or 15.
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    引用文献:
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    US2987407A|1957-08-19|1961-06-06|Casius Corp Ltd|Method for accelerating the setting of hydraulic binders|CN108892401A|2018-08-23|2018-11-27|天津水泥工业设计研究院有限公司|A kind of method and clinker of ardealite calcining belite sulphoaluminate cement clinker|
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    AT413535B|2004-04-05|2006-03-15|Holcim Ltd|HYDRAULIC BINDER AND METHOD FOR THE PRODUCTION THEREOF|
    FR2891270B1|2005-09-28|2007-11-09|Lafarge Sa|HYDRAULIC BINDER COMPRISING A TERNAIRE ACCELERATION SYSTEM, MORTARS AND CONCRETES COMPRISING SUCH A BINDER|
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    CN111620577A|2019-04-04|2020-09-04|北新集团建材股份有限公司|Machine-sprayed surface layer plastering gypsum with purification function and preparation method thereof|
    FR3096365B1|2019-05-24|2021-09-03|Saint Gobain Weber|Dry composition of mortar, especially adhesive mortar for tile adhesive|
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    WO2021180594A1|2020-03-13|2021-09-16|Sika Technology Ag|Slag-based hydraulic binder, dry mortar composition comprising same and system for activating a slag-based binder|
    FR3108055A1|2020-03-13|2021-09-17|Norper|Earth-based mortar|
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    法律状态:
    2017-05-24| PLFP| Fee payment|Year of fee payment: 2 |
    2017-11-24| PLSC| Search report ready|Effective date: 20171124 |
    2018-05-22| PLFP| Fee payment|Year of fee payment: 3 |
    2019-05-22| PLFP| Fee payment|Year of fee payment: 4 |
    2020-05-28| PLFP| Fee payment|Year of fee payment: 5 |
    2021-05-31| PLFP| Fee payment|Year of fee payment: 6 |
    优先权:
    申请号 | 申请日 | 专利标题
    FR1654401A|FR3051461B1|2016-05-18|2016-05-18|BINDER BASED ON CALCIUM ALUMINOSILICATE DERIVATIVES FOR CONSTRUCTION MATERIALS|
    FR1654401|2016-05-18|FR1654401A| FR3051461B1|2016-05-18|2016-05-18|BINDER BASED ON CALCIUM ALUMINOSILICATE DERIVATIVES FOR CONSTRUCTION MATERIALS|
    RU2018140505A| RU2715583C1|2016-05-18|2017-05-11|Binder based on calcium alumino-silicate derivatives for construction materials|
    BR112018071455A| BR112018071455A2|2016-05-18|2017-05-11|calcium aluminosilicate derivative based binder for building materials|
    EP17727653.2A| EP3458426A1|2016-05-18|2017-05-11|Binder based on calcium aluminosilicate derivatives for construction materials.|
    PCT/FR2017/051134| WO2017198930A1|2016-05-18|2017-05-11|Binder based on calcium aluminosilicate derivatives for construction materials.|
    SG11201809746SA| SG11201809746SA|2016-05-18|2017-05-11|Binder based on calcium aluminosilicate derivatives for construction materials.|
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