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
  • C04B28/18—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 mixtures of the silica-lime type
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B28—WORKING CEMENT, CLAY, OR STONE
  • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
  • B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
  • B28B11/04—Apparatus or processes for treating or working the shaped or preshaped articles for coating or applying engobing layers
  • B28B11/042—Apparatus or processes for treating or working the shaped or preshaped articles for coating or applying engobing layers with insulating material
  • B28B11/043—Apparatus or processes for treating or working the shaped or preshaped articles for coating or applying engobing layers with insulating material filling cavities or chambers of hollow blocks
• • E—FIXED CONSTRUCTIONS
  • E04—BUILDING
  • E04B—GENERAL BUILDING CONSTRUCTIONS; WALLS, e.g. PARTITIONS; ROOFS; FLOORS; CEILINGS; INSULATION OR OTHER PROTECTION OF BUILDINGS
  • E04B2/00—Walls, e.g. partitions, for buildings; Wall construction with regard to insulation; Connections specially adapted to walls
  • E04B2/02—Walls, e.g. partitions, for buildings; Wall construction with regard to insulation; Connections specially adapted to walls built-up from layers of building elements
• • 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
  • C04B2111/20—Resistance against chemical, physical or biological attack
  • C04B2111/27—Water resistance, i.e. waterproof or water-repellent materials
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
  • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
  • Y02W30/00—Technologies for solid waste management
  • Y02W30/50—Reuse, recycling or recovery technologies
  • Y02W30/91—Use of waste materials as fillers for mortars or concrete

Definitions

• the present invention relates to a honeycomb structural brick comprising a magneso-silico-calcareous porous material and can be used in the construction of high insulation wall.
• Terracotta bricks called “monomur”, or cement, called “cinderblock”, honeycomb structure, are widely used for the construction of walls, floors, partitions or other elements of buildings.
• These bricks are usually composed of empty cells (not filled) more or less large, more or less different shape, to increase the thermal insulation.
• These structures are composed of cells of reduced size to limit thermal convection and have low wall thicknesses to limit the conduction effect.
• the interior space of the cells of these building bricks is usually empty. When a temperature gradient exists within a cell, the air contained in this cell moves by convection. The direct consequence is a decrease in the thermal resistance of the system.
• One of the solutions implemented to minimize the convective effects is to increase the number of cells, but this solution is limited by (i) a technical implementation of bricks more and more complex, (ii) quantities of material more (iii) the appearance of more important conduction phenomena.
• this inorganic material is due to its microstructure to give a "mechanical strength to air or vacuum", namely to trap air (or vacuum) so as to minimize the effects of convection.
• the document FR 2 876 400 describes the use of hollow bricks filled "with an insulating material based on porous product (s) in bulk".
• the so-called natural material for filling is based on expanded perlite or expanded vermiculite in which starch is used as a thickener.
• This document also mentions the use of other components such as colloidal silica, hydrophobic agents, or dispersed plastic.
• the disadvantage of this solution is the low mechanical strength of the agglomerates, which entails a risk of deterioration of these packing masses during transport and assembly of these elements. It should be noted the low cohesive power of this structure inducing particular risks of loss of material during drilling, cutting, ... walls for example. It is also worth noting the settlement of the grains several years after the laying of the building elements, which ultimately leads to the reduction of the insulating power. Also the use of organic binders or hydrophobic agent substantially reduces the thermal resistance of these materials and increases the risk of fire resistance.
• Such a structure has the disadvantage of having a low mechanical strength, which limits the reduction of the number of walls of the clay brick and entails risks of degradation of the porous material during the laying of the building elements. Therefore, a problem that arises is to provide a building brick that does not have the disadvantages mentioned above.
• a solution of the present invention is a structural brick 1 with a cellular structure comprising a porous material 2 comprising 25% by mass to 75% by mass of silica, from 75% by weight to 25% by mass of calcium hydroxide, and from 0 to 5% by weight. mass% of magnesia and having a micro-structure composed of nodules and / or crystals in the form of needles 3 so as to provide pores with an average diameter D 50 of between 0, 1 and 10 ⁇ , and so that said material porous has a porosity of between 60 and 95%.
• the porous material has a porosity of between 70 and
• micro structure of the porous material composed of nodules more or less spherical and interconnected by crystals having the shape of needles, result of a crystallographic growth occurring during a hydrothermal synthesis, is shown in Figure 1 It should also be noted the potential presence of unreacted raw material grains or during chemical reactions.
• the total porosity of the porous material can be measured using a mercury porosimeter.
• the thermal conductivity can be measured using a device of the type Paque Chaude Guarded at an average temperature between 0 and 70 ° C.
• the compressive strength can be measured by developing a cube of 100 x 100 mm 2 porous material and applying on the upper face thereof a pressure force while it is held against a horizontal metal plate. This force corresponds to the pressure (in kg / cm 2 or MPa) from which the material begins to crack.
• FIG. 2 shows the compressive strength curves of several porous materials with chemical formulations as described in the invention but with different operating conditions, in particular temperature (T), pressure (P), rise and fall ramps; in temperature (° C / min) and the duration (t) of the hydrothermal synthesis.
• T temperature
• P pressure
• t duration
• FIG. 2 shows the compressive strength curves of several porous materials with chemical formulations as described in the invention but with different operating conditions, in particular temperature (T), pressure (P), rise and fall ramps; in temperature (° C / min) and the duration (t) of the hydrothermal synthesis.
• T temperature
• P pressure
• t duration
• the building brick according to the invention has one or more of the following characteristics:
• the porous material has a micro-structure composed of nodules and / or crystals in the form of needles and optionally elementary grains so as to provide pores with an average diameter D50 of between 0.1 and ⁇ ;
• the porous material has a mechanical strength of between 5 and 40 kg / cm 2, preferably between 10 and 30 kg / cm 2 and a thermal conductivity of between 50 and 150 mW / ° Km, preferably less than 100 mW / ° Km;
• the porous material comprises at least 70% by weight of crystalline phase
• the crystalline phase additionally contains one or more silico-calcareous phases representing 0 to 50% of the weight of the porous material;
• the silico-calcareous phases are chosen from xonotlite, foshagite, tobermorite 11A, tobermorite 9A, Riversideite 9A, Trabzonite [Ca 4 Si30O, 2H 2 O], Rosenhahnite [Ca3Si30s (OH) 2 ], Kilalaite [Ca 6 Si 4 O 4 , H 2 O], and Gyrolite.
• the porous material may contain carbon fibers and / or glass and / or cellulose fibers or any other fibrous fillers.
• said brick comprises: a honeycomb structure of terracotta or cement; and said porous material contained in at least a portion of the alveoli of the honeycomb structure.
• crystalline phase may contain in addition:
• the present invention also relates to a method of manufacturing a building block according to one of claims 1 to 8, comprising the following successive steps:
• a step e) of hydrothermal synthesis of the brick by heating at a temperature of between 80 ° C. and 200 ° C., and under a saturated steam pressure of between 1.10 5 Pa and 25 ⁇ 10 5 Pa, for a period of time between 1 and 40 hours to obtain a ceramic mass, and
• the manufacturing method according to the invention has one or more of the following characteristics:
• the mixture comprises a germinating agent and is prepared in such a way that the mass ratio (CaO + SiO 2 + germinating agent) / H 2 O is between 15 and 30% and the weight ratio ( CaO + germinating agent) / Si0 2 is between 0.8 and 1.2;
• the germination agent is chosen between magnesia and colloidal silica
• step b) comprises, between step b) and step d), a step b1) of storing the mixture prepared in step b);
• step b1) the mixture is stirred
• said method comprises after step f) a step g) of waterproofing the faces of the brick where the porous material is apparent by the addition of an organic compound, a silicone or an organic compound.
• the step a) of neutralization makes it possible to overcome the influence of the porosity of the honeycomb structure of the brick.
• Terracotta bricks have a porosity between 10 and 30%. This porosity, if not neutralized, can absorb by capillarity the water of the mixture after filling, it will then result in a drop in level within the channels of a brick of the porous mass which is a source of defects.
• the brick can either be immersed in a pool in order to saturate it in water, or be covered inside the channels by an organic material (silicone, teflon, ...) which will limit the phenomena of capillarity, a mixture of 2 solutions namely protection of a waterproof or semi-waterproof coating and immersion in a pool to saturate water brick.
• Step b) of preparing a mixture comprising lime, silica and water comprises:
• a first substep of synthesis of quicklime by calcination at a temperature greater than or equal to 800 ° C. of limestone blocks of average size of between 1 mm and 15 mm having a purity of at least 90% by weight and an open porosity greater than 0% to less than or equal to 25%, to obtain particles of quicklime;
• a germinating agent such as magnesia for example
• this third sub-step can be included in the second sub-step.
• Step b) of preparation of a mixture may lead to "all-in” mixtures or "2-step” mixtures.
• the inorganic and optionally organic materials are premixed to dryness.
• the assembly is then introduced into hot water whose temperature is between 30 and 50 ° C.
• the lime is initially extinguished with part of the water, then all the other constituents are added together with the complementary water.
• the choice of the order of introduction will be fixed by those skilled in the art depending on the specific properties of the lime (reactivity, viscosity, decantation). These specific properties are derived from the raw material (limestone) and the transformation history (roasting) of it.
• Tables 1 and 2 the proportions of the raw materials and the ratio of raw materials to solvent are fixed. This ratio and its proportions are at the base of the properties of the porous mass synthesized under hydrothermal conditions.
• the mixture is conventionally made in a disperser (speed of rotation of the axis up to 1400 rpm) equipped with a bidirectional tri-blade whose diameter is ideally between 1/3 and 1/2 of the diameter of the tank in which the mixing takes place.
• the mixing time is between 10 and 40 minutes.
• the sizing of the appliances is related to the volume of bricks to be filled and will therefore depend on the production line on which they will be installed.
• FIG. 4 shows an example of disperser making it possible to carry out the mixing.
• Step b1) of storage of said mixture consists of transferring the mixture (suspension) into a buffer tank with stirring to avoid settling of the latter.
• the injection system will be implanted on this buffer tank.
• Step c) of sealing the underside of the brick allows to fill the suspension channels and maintain the mixture within the cells.
• the brick can then optionally be placed in a system (wagon, slideway ...) in order to facilitate its subsequent charging in a low pressure / low temperature autoclave in which the hydrothermal synthesis will take place. It should be noted that this technique is very powerful if the brick to be filled has been rectified during the manufacturing process.
• Figure 5 shows an example of a plastic film system for sealing a brick before filling the mixture.
• Step d) of filling consists of filling the bricks with the mixture.
• a system consisting of pumps and an injection nozzle allows the filling of the chain or parallel of one or more bricks. It can be installed if necessary a vibrating system so as to shear the dough during filling and thus allow better homogenization of the mixture.
• the hydrothermal synthesis step e) consists in carrying out a hydrothermal synthesis at a temperature of between approximately 80 and 200 ° C., preferably between 100 and 160 ° C., for a duration ranging from 2 to 40 hours, preferably from 5 to 24 hours. .
• the pressure inside the autoclave is the saturation vapor pressure which according to the cooking conditions can vary between 10 5 Pa and 25.10 5 Pa (1 and 25 bar), preferably between 1.10 5 Pa and 10.10 5 Pa (1 and 10 bar).
• the drying step f) serves to evacuate the residual water trapped after the synthesis in the pores of the micro structure formed.
• This operation is carried out in a traditional electric oven or gas (which may or may not be the same as that used for the hydrothermal synthesis operation), the drying takes place at atmospheric pressure.
• the drying cycle takes place between 100 and 450 ° C, preferably between 100 ° C and 250 ° C for a period of between 1 and 30 hours, preferably between 2 and 24 hours.
• the drying cycle may have ramps and bearings at intermediate temperatures.
• Step g) of waterproofing consists in applying a waterproofing agent (silicone, chemical hardener, Si-based sol-gel deposit, varnish based on cellulose) either by spraying or with the aid of rollers on the faces or the mass porous is apparent in order to make the latter hydrophobic.
• a waterproofing agent silicone, chemical hardener, Si-based sol-gel deposit, varnish based on cellulose
• the bricks lined with porous material may first be rectified if necessary and / or sanded on the surface.
• the present invention also relates to an assembly comprising one or more building bricks 1 according to the invention.
• the bricks have a shape that allows the construction of building elements, such as walls, floors, ceilings, roofs.
• Example 1 relates to the lining of bricks from a mixture called “in two steps”.
• Example 2 relates to the lining of bricks from a mixture called "all in one”.
• the choice of the mixing protocol ("all in one" or “in two steps") will be determined by those skilled in the art according to the specific properties of the lime (reactivity, viscosity of the milk of lime, settling).
• a brick was immersed in water for 2 hours in order to saturate the shards with water and thus prevent capillary diffusion of water from the suspension into the walls of the brick.
• the filled brick in this example has a porosity of the order of 10-15%.
• the total porosity being between 15 and 25% the immersion time will be lengthened.
• Figure 6 illustrates the immersion of a brick in a container containing water.
• the mixture is carried out in two stages. In a first step, the quicklime is extinguished in water heated to 43 ° C., mixing is carried out at 900 rpm for 20 minutes. Then, in a second step, the silica and the other constituents (magnesia, organic compounds) are introduced with water at room temperature. In order to homogenize the mixture, kneading at 900 rpm is carried out for 20 minutes.
• the brick before being filled with the mixture is wrapped with a plastic film so as to seal the bottom.
• the brick is then placed in a wagon which will be directly placed in a slide in the autoclave.
• the brick is placed on a vibrating table to allow optimum filling of the cells by lowering the viscosity of the mixture by shearing.
• Figure 7 shows an example of vibrating table allowing homogenization during filling of the brick and Figure 8 shows a brick before charging in the autoclave for hydrothermal synthesis.
• the packed brick was placed in an autoclave under hydrothermal synthesis conditions at 150 ° C or a saturation vapor pressure of 4 bar relative.
• Figure 9 represents the hydro-thermal synthesis cycle.
• the initial system lime, silica and water can not spontaneously crystallize, which is why a hydrothermal synthesis is necessary as part of the lining of the bricks.
• the modification of the pressure and temperature conditions during a determined period allows the energy input which is consumed by the system to cross the energy barrier of crystallization.
• so-called germination agents such as magnesia and / or colloidal silica makes it possible to reduce the hydro-thermal synthesis times.
• the brick is then dried according to the cycle shown in FIG. 10 to a maximum temperature of 235 ° C. and for a period of 24 hours at atmospheric pressure. 1H. finishes
• Figure 11 shows a brick after grinding and applying a waterproofing agent.
• the mixture of inorganic and organic compounds are made in the desired proportions to dryness.
• the constituents are introduced into the tank of the kneader in the following order: water heated to 43 ° C, then a pH modifying agent (soda or quicklime) the objective being to obtain a water with pH included between 9 and 14, preferably between 11 and 12.5.
• a pH modifying agent sodium or quicklime
• the powder mixture is then introduced, the mixture being kneaded at 900 rpm for 40 minutes.

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• Engineering & Computer Science (AREA)
• Chemical & Material Sciences (AREA)
• Structural Engineering (AREA)
• Ceramic Engineering (AREA)
• Architecture (AREA)
• Civil Engineering (AREA)
• Physics & Mathematics (AREA)
• Electromagnetism (AREA)
• Mechanical Engineering (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Inorganic Chemistry (AREA)
• Materials Engineering (AREA)
• Organic Chemistry (AREA)
• Compositions Of Oxide Ceramics (AREA)
• Porous Artificial Stone Or Porous Ceramic Products (AREA)
• Curing Cements, Concrete, And Artificial Stone (AREA)

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• 2012
  • 2012-04-19 FR FR1253605A patent/FR2989707B1/fr not_active Expired - Fee Related
• 2013
  • 2013-04-15 WO PCT/FR2013/050822 patent/WO2013156722A1/fr active Application Filing
  • 2013-04-15 EP EP13742665.6A patent/EP2838865A1/de not_active Withdrawn
  • 2013-04-15 BR BR112014026178A patent/BR112014026178A2/pt not_active IP Right Cessation
  • 2013-04-15 MA MA37540A patent/MA20150103A1/fr unknown
  • 2013-04-15 CA CA 2868442 patent/CA2868442A1/fr not_active Abandoned
  • 2013-04-15 RU RU2014146295A patent/RU2641154C2/ru not_active IP Right Cessation
• 2014
  • 2014-09-25 TN TNP2014000404A patent/TN2014000404A1/fr unknown

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