WO1989007518A1

WO1989007518A1 - Process for obtaining a construction material, installation for implementation of said process and construction material thus obtained

Info

Publication number: WO1989007518A1
Application number: PCT/FR1989/000054
Authority: WO
Inventors: Henri G. Lievremont
Original assignee: Lievremont Henri G
Priority date: 1988-02-11
Filing date: 1989-02-13
Publication date: 1989-08-24
Also published as: AU3067789A; EP0387306A1; FR2627177A1

Abstract

The installation for implementation of the process and for obtaining a construction material comprises a mixing tank and a unit for delivering the products mixed in the tank to a mould for shaping the construction material. The mixing tank (1) receives and kneads doses of phenolic resin and of powder products of various materials, such a mica, schist, talc, etc., and a screw-type unit (11) conveys the kneaded products to an intermediate hopper (2) for stabilizing the temperature, and which feeds a supply unit (3), which delivers them to a mixing and extrusion head (4), into which also opens a pipe (32) for the supply of a hardening catalyst. Application to the production of a uniform material, which can easily be machined with wood working tools and which is resistant to fire and to corrosive substances.

Description

PROCESS FOR OBTAINING A CONSTRUCTION MATERIAL, INSTALLATION FOR IMPLEMENTING THE SAME, AND CONSTRUCTION MATERIAL THUS OBTAINED

The present invention relates to a process and an installation for obtaining a building material resistant to fire, cold, thermal shock, acids and bases and also relates to the building materials thus obtained. There is currently no building material on the market which is practically insensitive to fire, cold, thermal shock, acids and bases. None of the materials currently available meets all of the above conditions. Not only does the new process and installation according to the present invention lead to this surprising and perfectly unexpected result of making it possible to obtain a building material having these properties, but also making it possible to obtain a material further having the advantage of being homogeneous, of being easily machinable with tools used for woodworking, of being assembled by gluing or using cement, of being an excellent sound insulator and of being light while with a density lower than that of wood. In addition, this material is inert towards acids or bases.

The present invention relates to a process for obtaining a building material consisting of: a.- mixing the phenolic resin and the pulverulent fillers by controlling the viscosity of the mixture obtained so as to obtain a viscosity mass constant; b.- discharge, under pressure by sucking in the occluded air, the mass of phenolic resin and of powdery fillers resulting from step a.-; c- introducing the mass obtained and the polymerization catalyst into a mixing and extrusion head; d.- extruding the mass resulting from step c- and adding it to the mixture of the expanded products or spheroid in an impregnator in which a homogeneous mixture of the mass and the mixture of expanded products or sphero mentioned above is formed; e.- send, via mobile distribution means, the mixture resulting from the aforementioned step d.- to a forming and setting zone. According to another embodiment of the process, the pulverulent fillers are chosen from the group comprising magnesium silicate, aluminum silicate, TiO 4, talc, mica, phosphogypsum, aluminum sulphate, a mine, silica, shales, magnesia, magnesium sulfate. The expanded products or spheroids are chosen from a group comprising spheres of expanded clay, perli vermiculite, spherules of expanded glass or ceramic fibers.

Preferably, according to the invention, the total volume of the aggregates therefore of the pulverulent fillers and of the expsed products or spheroids incorporated in the composite product formed from 80 to 90% of the total volume of the said product and the “polymerization catalyst consists in that the polymerization catalyst consists of methanol and sulfuric acid or hydrochloride

The installation for obtaining a building material comprising a mixing tank and a delivery block for products mixed in the tank to a mold formed from the building material, is characterized in that the mixing tank receives and mixes doses of phenolic res and pulverulent or weight products of various materials such as micas, shales, talc, etc., that a blowing screw blows pushes the kneaded products towards a intermediate temperature stabilization hopper fed to a discharge block which discharges into an extrusion mixture head into which also leads a discharge line of a curing catalyst and in that said installation comprises a mixer assembly of expanded charges or spheroids which pours these charges into a screw impregnator connected to a mixer of the mixing head capable of extruding the mixture of phenolic resin, of pulverulent products and of catalyst prepared in this head, the outlet of the impregnator being arranged above molding tanks receiving, before hardening, the pasty and sticky final product consisting of expanded fillers or spheroids impregnated with said mixture.

The mixing tank has at its base the screw delivery block connected to the intermediate hopper via a motorized cut-off valve and to a recirculation line via a motorized cut-off valve, these motorized valves being coupled via a regulating member to a tank temperature sensor and a pressure and / or tank discharge flow sensor.

According to another embodiment of the installation, the intermediate hopper comprises at least one level probe and one temperature probe and delivers, via a motorized valve, the mixture of phenolic resin and fillers maintained at suitable viscosity and temperature, at its base to the delivery block which is connected to a suction chamber for air and occluded gases and in which rotates a feeding screw at adjustable speed. The mixing and extrusion head is connected from upstream to downstream in the direction of its injection: a suction line for air and occluded gases, to the delivery block for the kneaded and conditioned mixture of phenolic resin and of pulverulent products, then to the pipe for discharging a curing catalyst and finally to a pipe for possibly supplying a liquid for rinsing the injector after stopping the injection of catalyst.

According to yet another embodiment of the installation, the charge mixer assembly consists of a screw mixer connected from downstream to upstream, respectively a hopper for feeding large balls of expanded products or spheroids, to a hopper for feeding small balls of expanded products or spheroids, and finally to a hopper for supplying refractory cement intended to give cohesion to these products expanded.

The screw impregnator and the injection head are preferably made integral and are carried by a mobile carriage on a rolling track in order to allow the final product to be output from the impregnator into a mold. According to another embodiment of the invention, further improving the resistance of the product obtained, the outlet nozzle of the screw impregnator is connected to an orifice for injecting cut son or filaments made of a material having good resistance. mechanical and heat. The building material according to the invention contains from 80 to 90% of its total volume of pulverulent fillers, of expanded products, of refractory cement, and possibly of son or filaments of fibers.

According to one embodiment of the invention, for 100 lmes of filler, this material contains from 25 to 125 volumes of mineral fillers and from 900 to 1275 volumes of pulverulent products.

According to another embodiment of this material, the powder fillers are chosen from the group consisting of magnesium silicate, aluminum silicate, TiO 2, talc, mica, phosphogypsum, aluminum sulphate, a mine, silica, shales, magnesia and magnesium sulfate.

According to yet another embodiment of the invention, the expanded products or spheroids are chosen from the group comprising spheres of expanded clay, perli vermiculite, spherules of expanded glass or ceramic fibers.

According to yet another embodiment of the invention, the son or filaments of fibers are chosen from the group comprising glass fibers, carbon fibers, metallic threads, flame-retardant threads, etc. The material is more often in the form of flat plates or suitable boards be sawn or machined by tools intended for working hardwood.

Other objects, advantages and characteristics will appear on reading the description of various embodiments of the invention, given without limitation and with reference to the appended drawing where:

- Figure 1 schematically shows an installation according to the present invention for obtaining the building material, object of the invention;

- Figure 2 is a schematic representation of another embodiment of the installation of Figure 1, in which the impregnator and the circuits which surround it have been modified.

The installation represented in FIG. 1 comprises, as main elements arranged according to the order of their intervention in the process, a mixing tank 1, an inte cal hopper 2 a block for delivery and suction of occluded air 3 , a mixing and extrusion head 4, a mixer assembly of the expanded charges or spheroids 5 and, finally, an impregnator of these expanded products or spheroids 6.

The mixing tank 1 receives, via a loading opening 7, doses of phenolic resin and pulverulent or weighty products of various materials such as micaceous minerals, expanded shales, silicates, magnesium sulphate, alumina, talc, etc. The mixing tank comprises a kneading assembly consisting of a paddle rotor 8 driven in rotation by an electric motor 8a and rotating in front of a finned stator 9, arranged in the bottom part of the tank and whose blades are oriented in the opposite direction to that of the blades of the rotor 8 located opposite. -The bottom of the tank 1 of conical shape opens out through a connection tube 10 onto a screw delivery block 11 whose screw is rotated by an electric motor 12.

The block 11 discharges, via a line 13, via a motorized valve 14 for regulation and cut-off and a flowmeter 15 coupled with a pressure indicator, into the intermediate hopper Upstream of the motorized valve 14, a recirculation line 16 on which is interposed a motorized valve 17 of regulation and cutoff, allows the return or recycling to the tank 1 of all or part of the mixture of resin and filler. A temperature probe 18 is immersed in the mass at the neck of the mixture inside the tank 1 and is electrically coupled, via a regulating member 19, to the motorized valves and 17 and to the flow meter 15.

The hopper 2 is provided with an agitator, not shown, driven by a motor 20 and includes various monitoring probes: a high level probe 21, a low level probe 22 and a temperature probe 23. The hopper 2 delivers to its base, via a motorized valve 24, the mixture of phenolic resin and fillers, maintained at the appropriate viscosity and temperature. The mixture is brought to the inlet connection of the discharge and suction block 3 provided with a solid body capable of withstanding the high discharge pressure and inside which a booster screw 25 rotates. After the connection inlet, the interior space with the booster screw 25, leads to a chamber 26 for suction of the air occluded in the mixture of phenolic resin and fillers. The chamber 26 is connected, via a cut-off valve 27, to a suction line 28 connected to a vacuum pump with low depression, for example of the order of 6 to 7 mbar and not likely to suck the mixture based on phenolic resin. Booster screw 25 is rotated by means of a speed controller 29, so as to allow its speed to be adapted to the discharge flow rate required for the mixture based on phenolic resin and to the viscosity of this mixture. The discharge block 3 discharges under pressure, via a fixed pipe 30 and a flexible connector 31 via a cut-off valve 31a, the mixture based on phenolic resin in the mixing head 4 in the form of a column and which has several (four in the experimented embodiment) rotors provided with cutting blades in the shape of plowshares and driven in rotation by a motor 4a_. Downstream of the entry of the mixture into the body of the mixing head 4, via a cut-off valve 32a opens a supply line 32 of a discharged catalyst by a recovery pump 33, from an intermediate catalyst reservoir 34 equipped with level and temperature detection probes 34a and supplied via a pump 34b with a motorized valve 34c of catalyst taken from a reservoir see main 34d.

The mixing head 4, arranged vertically, ends at its lower part with an injector 35 and is carried by a carriage 36 movable on a rolling track 37. As for the discharge block 3, a complementary vacuum suction pipe 38 sucks in the upper part of the mixing head 4 the gases occluded in the phenolic-based mixture being extruded. The mixing head 4 is integral with the impregnator 6 which includes a small hopper 39 for receiving the extruded mass of resin, fillers and catalyst, available just below the injector 35. The small hopper 39 che on a mixing and propulsion screw 40, upstream of which is introduced by a supply line 41 a homogeneous mixture of expanded products of spheroid form coming from the mixer 42 of the mixer assembly 5. The homogeneous mixture of expanded products or spheroids is brought into the screw mixer 42 from feed hoppers 43, 44, 45 loaded, respectively from downstream to upstream of the mixer: large balls of expanded products, small balls of expanded products, and a refractory cement intended to give cohesion to these expanded products.

L ¹ impregnator 6 is integral with the carriage 36 which rolls in the plane of the figure on the raceway 37, carrying with it the mixing and extrusion head 4. An outlet opening 46 of the impregnator 6 pours the product final composite obtained generally containing less than 20% of phenolic resin coming from head 4 and injector 35 and more than 80% of charges consisting on the one hand of pulverulent products or spheroids coming from the tank and , on the other hand, of expanded products from the mixer assembly 5.

The operation of the installation which has just been described is explained below. Mixing tank 1 is supplied with phenolic resin and the aforementioned pulverulent products such as micaceous ores, expanded shales of silicates, magnesium sulphate, alumina, tal in predetermined proportions for which the percentage of phenolic resin is significantly lower than that powdery products. The kneading assembly 8, 9 in the lower part of the tank ensures good impregnation of powdered products with phenolic resin and these impregnated powdered products are poured into the bottom of the tank at the inlet of the screw delivery block 11 which conveys via line 13 to the inlet of the intermediate hopper 2 where the pulverulent products impregnated with phenolic resin are brought to and maintained at a suitable viscosity and temperature ^* -. At the start of the installation, the still insufficiently impregnated pulverulent products are brought back by the recirculation line 16 to the mixing tank 1 to perfect their impregnation. Likewise, in the event of a sudden reduction in the flow rate of impregnated pulverulent products flowing through line 13, the motorized regulating valve 17 opens to allow recycling to the tank 1 of impregnated powdery products which are discharged at flow rate. almost cons¬ by the screw delivery block 11 operating in volumetric pump. The intermediate hopper 2 delivers at its base a controlled flow of impregnated pulverulent products which enters the high-pressure delivery block 3 where the air and the occluded gases are sucked by the suction line 28. The impregnated pulverulent products discharged by the loading screw 25 of the delivery block 3 are brought to the appropriate viscosity, by means of any thermal source, via flexible connector 31 at the upper part of the mixing head 4 in which the rotors have blades plowshares. Line 32 leads into the mixing head 4, downstream of the arrival of the pulverulent products impregnated with phenolic resin, a catalyst discharged by the recovery pump 33. The mixture of impregnated pulverulent products and catalyst is discharged by the injector 35 provided at the base from column 4, in the form of an extrusion, into the small hopper 39 which introduces it inside the screw 40.

The mixer for expanded products or spheroid assembly introduces, via the supply line 41, the homogeneous mixture of the expanded products made coherent by a refractory cement, at the inlet of the screw 40 where it meets the mixture of pulverulent products impregnated with phenolic resin and added with catalyst. The screw 40 ensures the mixing of impregnated powder products and expanded or spheroid products and pours through the outlet opening 46 the final composite product obtained.

The final product obtained having a relatively pasty and sticky structure, the outlet opening 46 in the form of a sleeve moves alternately in the plane of the figure and pours this pasty and sticky final product into a mold pan 47 which moves perpendicularly in the plane of the figure, the length of a pass by any appropriate means such as rollers or slides after each pass for discharging this opening 46. In this way, there is obtained in the tank 47 the juxtaposition of several adjacent "strips" of final product pasty, the outer surface of which becomes substantially flat at rest to give a rectangular or square slab shape to the final product which hardens after polymerization of the phenolic resin. There are shown in 47a and 47b other molding tanks intended for molding slabs of composite product respectively thinner or thicker. The hardening of the slabs or other forms of molding filled by regular distribution of the pasty final product in a mold, can be obtained in a few minutes by polycondensation of the phenolic resin after the triggering of the exothermic physico-chemical phenomenon causing the solidification

Note in the figure that the mixing head 4 is connected to its lower part via a cut-off valve 48a pa a flexible pipe 48 and a pump 49 to a rinsing tank equipped with level and temperature probes 50a and supplied with products rinsing by a pump 51 from a reser¬ see 52 of rinsing products. Before stopping the installation, it is thus possible after stopping the injection of catalyst at valve 32a to gradually replace, in mixing head 4, the mixture based on phenolic resin coming from flexible connector 31 and of catalyst supplied by line 32 with a rinsing product capable of cleaning the injector 35 and avoid blocking of the mixing head 4 and of the injector due to the subsequent polymerization of phenolic resin during the shutdown of the installation. The mixture of phenolic resin and fillers present in the delivery block 3 remains liquid on the other hand during the shutdown of the installation due to the absence of catalyst and only requires reheating at the time of restarting the installation when the rinsing products are discharged from the mixing head 4, followed by the reopening of the respective motorized valves 31a, 32a, of the connector 31 and of the pipe 32 and of the closing of the motorized valve 4 controlling the flow of rinse aid.

FIG. 2 shows a different embodiment of the final mixer of the expanded or spherical products and of the pulverulent products impregnated with phenolic resin. The elements identical to those in FIG. 2 retain the same reference numbers. A hopper 60 for supplying expanded mineral spherules is connected via a solenoid valve with adjustable opening 61 to a propulsion screw 62 driven in rotation by a motor with adjustable speed 63. The hopper 60 which can replace the three hoppers 43 44, 45 represented in FIG. 1 receives a mixture of expanded mineral products or spheroids and of a refractory cement giving cohesion to these mineral products.

The propulsion and mixing screw 62 is surrounded by a cylindrical casing or casing 64 open at its upper part on the outlet of a funnel 65 for receiving impregnated pulverulent products delivered by the injector 35 the mixing head 4. The mixture , kneaded by the screw 62, of expanded or spheroid products, of refractory cement and of impregnated pulverulent products is poured through an outlet nozzle 66 of the impregnator 6 contained in the casing 64.

An orifice 67 for injecting cut threads or filamen opens laterally into the wall of the outlet nozzle 66 11

to inject, if necessary, cut son or cut filament into the kneaded mixture ready to harden after its étale¬ ment in viscous parallel strips in a receiving and molding tank 47. To prepare the cut son, it is possible to use, as shown in FIG. 2, coils 68 e 69 of different threads, for example textiles but more generally non-combustible, the threads 70 and 71 of which are brought "by unwinding in a device 72 for cutting and injecting threads comprising for example, rotary knives and a blowing injection fan as wires or filaments for reinforcing the final product 67 hardened into plates in the molding trays 47. Various shades and varieties of textile or other yarns or fibers can be used. preferably non-combustible or flame retardant, such as fire-retardant treated threads, but also carbon, glass, high-resistance synthetic fibers and also for certain applications. Ations of metallic wires of very small diameter, for example wires cut from .... high resistance rope of the kind of metallic wires used for the tread ply, pneumatic tires for rolling vehicles (commonly called pneumatic tires) . Examples 1 to 8

Eight samples of the composite material according to the invention were prepared and which substantially present the following compositions, expressed in volume parts. Example 1

Resin 100

Silicate Mg 30

Aluminum silicate 30 τi0 ₂ 15

Perlite 100

Vermiculite 75

Expanded clay spherules 850 Example 2 Resin 100

Silicate Mg 35

TiO. 5

Phosphogypsum 40 Perlite 100

Vermiculite 150

Expanded clay spherules 950 Example 3 Resin 100

Silicate Mg 35

Aluminum silicate 20

^Ti0 2 ⁵

Phosphogypsum 30 Mica 20

Perlite 100

Vermiculite 100

Expanded clay spherules 950 Example 4 Resin 100

Silicate Mg 30

Aluminum silicate ...... 15

^Ti0 2 ⁵

Perlite 100 Vermiculite 100

Expanded clay spherules 850 Example 5

Resin 100

Silicate Mg 30 Aluminum silicate 25

Ti0 ₂ 15

Perlite 80

Vermiculite 50

Expanded clay spherules 800 Example 6

Resin 100

Silicate Mg 30

Aluminum silicate 25

Ti0 ₂ 15 Mica 30

Vermiculite 100

Expanded clay spherules 850 13

Example 7

Resin 100

Silicate Mg 35

Aluminum silicate 15 Ti0 ₂ 10

Vermiculite 50

Phosphogypsum 80

Expanded clay spherules 900 Example 8 Resin 100

Silicate Mg 25

Aluminum silicate 15

Ti0 ₂ 10

Perlite 50 Vermiculite 50

Expanded clay spherules 800

73 x 73 x 80 mm test pieces with a surface area of 53.3 cm ^{2 are formed} by cutting from molded blocks of the aforementioned samples and the compressive strength measurements are carried out. The results obtained are recorded in Table I.

TABLE I Measurement of compressive strength

Examples 9 to 12

On test pieces similar to those used in Examples 1 to 8, but having the following composition:

- example 9a to 9c Ja) _ lesin 100

Mg 30 silicate

Silicate alumini um ^* powder. . . 15

Ti0 ₂ 5 Perlite 100

Vermiculite 100

Globular aluminum silicate .... -

Expanded clay spherules 850

Expanded glass spherules 8/12 ... - Expanded glass spherules 16/25 ... -

- example 10a to 10c

Resin 100

Mg 30 silicate

Powdered aluminum silicate ... 20 Ti0 ₂ 10

Perlite 80

Vermiculite 60

Globular aluminum silicate.

Expanded clay spherules 800 Expanded glass spherules 8/12 ...

Expanded glass spherules 16/25 ...

- example lia à lie

Resin 100

Mg silicate 30 Powdered aluminum silicate ... 20

Ti0 ₂ 10

Perlite 80

Vermiculite 60

Globular aluminum silicate .... - Expanded clay spherules 850

Expanded glass spherules 8/12 -

Expanded glass spherules 16/25 -

15

(a) (b) (c)

- example 12a to 12c

Resin 100 100 100

Mg silicate 50 30 15 Powdered aluminum silicate ... 50

Ti0 ₂ 20 10 5

Perlite 100 - 100

Vermiculite 100 60 100

Phosphogypsum 30 Alumina globular silicate .... - 100 80

Expanded clay spherules 950

Expanded glass spherules 8/12. . . - 850 300

Expanded glass spherules 16/25. . . - - 650

The flexural strength (in daN / cm ² ) is measured using a mobile punch moving at 10 mm / m nute.

TABLE II Measurement of the flexural strength (in daN / cm ² )

Examples 13 and 14

On test pieces similar to those used in Examples 1 to 8, but having the following composition (in volume parts): - Example 13

100 parts resin

Mg 50 silicate

Powdered aluminum silicate 45 Ti0 ₂ 5

Perlite 200

Expanded clay spherules 950

- example 14 Resin 100

Mg 45 silicate

Ti0 ₂ 5

Perlite 200

Expanded clay spherules .... 900 TABLE III

Measurement of the tensile strength determined on 6 test pieces having a section of 5 cm x 5 cm and a height of 8 cm or 10 cm, cut from plates molded from the composite product according to the invention of Examples 13 and 14.

Tensile strength no. (In N / πm Plate thickness 8 cm 1 0.58

2 0.74

3 0.68 average 0.67

Plate thickness 10 cm 4 0.70

5 0.71

6 1.01 average 0.77 Examples 15 and 16

On test pieces similar to the test pieces used in Examples 1 to 8, but having the following composition (expressed in volume parts):

- example 15 Resin 100

Mg 20 silicate

Powdered aluminum silicate 10 Aluminum sulfate 65

^Ti0 2 ⁵ Vermiculite 150

Perlite 150

Expanded glass spherules 8/12 300 Expanded glass spherules 16/25 600 17

- example 16

Resin 100

Mg 20 silicate

Powdered aluminum silicate 65

Aluminum sulfate 10

Ti0 ₂ 5

Vermiculite 150

Expanded glass spherules 8/12 300 Expanded glass spherules 16/25 600

TABLE IV

Measurement of the thermal properties of two panels molded in composite product according to the invention, presenting the composition of samples no. 15 and 16

W is a heat flux expressed in watts. K ° expresses Kelvin or centigrade degrees The thermal resistance and thermal conductivity measurements were carried out for an average temperature of around 20 ° C.

EXAMPLES 17 Pipes are prepared having the following composition (expressed in volume parts): a) pipes: resin 100, roving wire 3 thicknesses, powdery minerals 22, for each pipe; b) insulation between pipes: resin 100, powdery minerals 40, ceramic fibers 5.

Example n ° 17 / for pipes (Fenotubes) Fenotubes:

100 parts resin

Roving wire 3 passages

(.at). Silicate Mg 10)

Powdered aluminum silicate 10 (__ Mica 1)

Carbon powder 1 (

Insulation between Fenotubes: Resin -. 100

Silicate Mg 20)

... Powdered aluminum silicate 10 (._ Mica 5)

Carbon powder 5 (Ceramic fibers 5

TABLE V Water absorption tests They are carried out on 3 test pieces in the form of an insulating pipe with an internal diameter of 80 mm and a thickness of 36 mm, showing the composition of Example 17.

The absorption of water takes place immersion after drying at a temperature of 40 ° C until a constant weight is obtained.

Water absorption Test tube no. (In volumetric%) 1 33.90

2 37.89

3 27.65 average 33.15 Example 18

Samples having an identical composition to Examples 13 and 14 are prepared (in volume parts).

TABLE VI Frost resistance tests

Testing the gel were carried out on 4 specimens obtained from the sample saturated with water under a vacuum ^"part with a residual pressure of 51 kPa, the feel your were initially subjected to 10 freeze and thaw cycles -10 ° C / + 10 ° C in the mass and then at 15 freeze-thaw cycles of -3 ° C / + 10 ° C in the mass; after the test, the 4 specimens were intact.

8 cm thick plate

Thickness plate 10 c

Water permeability tests The tests were carried out on 2 test pieces with a 30 cm water colon for 24 hours.

Height of the water column after 24 hours

Plate thickness 8 cm 29 cm

Thickness plate 10 cm 23 cm

As follows from the above tables, the composite product according to the invention prepared with the aid of the installation described above has, in cut test pieces, a mechanical resistance close to that of common molded concretes, excellent cold behavior and good thermal insulation properties.

The fire behavior of the composite material according to the invention intended in particular to constitute a sound insulator and to the flame was tested on samples of the material according to the invention composed of micaceous minerals, expanded wart, expanded shales with phenolic binder, silicates , sulphates of magnesia and alumina having, for a thickness of 70 mm, a total surface mass of approximately 5000 g / m ² .

These samples were subjected to: - radiation tests which did not show flammable gas emissions; - tests for fusible materials which have not ^** revealed the trace of the slightest fusible or combustible material; ; - flame propagation tests with the edge sample: no propagation could be detected. The composite material according to the invention turns out to be an excellent material for protection against flames accidental heating both by its qualities of resistance to flame and to thermal shock as by its qualities of thermal insulation.

The composite material according to the invention obtained in the installation which has just been described is thus formed from a thermosetting organic resin charged with incombustible powdery mineral products, mainly of micaceous type and at high melting temperature. The resin thus obtained from a mixture of liquid and solid constituents in substantially equal amounts, has a very high viscosity and serves as a binder to a saturated agglomerate of spherical aggregates of clay or of expanded glass or other products, even organic .

The volume of the aggregates, therefore of the pulverulent fillers and of the expanded or spheroid products, thus incorporated into the final molded composite product can reach 80 to 90% of the total volume of the product, while the specific specific weights of these aggregates vary between 15 and 1 700 g / dm ³ . The specific mass of the molded composite product varies between 350 and 740 kg / m ³ depending on the proportions of the various aggregates used. The thickness of the slabs obtained by molding the composite material according to the invention varies between 80 and 800 and it has already been possible to mold slabs reaching 3 per side. The blocks molded in ^“ composite product according to the invention have a texture allowing them to be machined by cutting tools under conditions close to those of hard boils, that is to say preferably using tungsten carbide tools or similar.

Some of the mechanical characteristics of the raw composite materials according to the invention formed by molding have been specified in the preceding tables. These mechanical characteristics can be improved on molded products by adding to these products internal reinforcements of various structures and textures, made from resistant materials and inserted into these products during molding.

The materials according to the invention have been found to be practically insensitive to the aggression of all alkaline or acid bases. Their behavior in cold or fire is remarkable and they remain inert and without apparent disorder after being subjected to the greatest thermal shocks while being considered as non-freezing. Their natural color, after exposure to the solar spectrum, and close to dark mahogany. All coatings and paints can be applied without precaution on the raw surface of these materials, the behavior and duration of which have not revealed any failure so far.

Of course, the present invention is not limited to the embodiments described and shown and it is capable of numerous variants accessible to those skilled in the art without departing from the spirit of the invention.

Claims

22

CLAIMS 1.- Process for obtaining a composite product containing less than 20% of phenolic resin or other organic or mineral binders and more than 80% of charges consisting of 5 pulverulent products and of expanded or spheroid products, characterized in that 'It comprises the steps consisting in: a.- mixing the phenolic resin and the pulverulent fillers by controlling the viscosity of the mixture obtained so as to obtain a mass of constant viscosity; B.- discharge, under pressure by sucking in the occluded air, the mass of phenolic resin and of powdery fillers resulting from step a.-; c- introducing the mass obtained and the polymerization catalyst into a mixing and extrusion head; D.- extruding the mass resulting from step c- and adding it to the mixture of expanded products or spheroids in an impregnator in which a homogeneous mixture of the mass is formed and from the mixture of expanded products or spheroids of the abovementioned; 20 e.- send, by means of mobile distribution means, the mixture resulting from the aforementioned step d.- to a forming and setting zone.

2.- Method according to claim 1, characterized in that the pulverulent fillers are chosen from the group 25 comprising magnesium silicate, aluminum silicate TiO 2, talc, mica, phosphogypsum, aluminum sulphate nium, alumina, silica, shales, magnesia and magnesium sulfate.

3. A method according to claim 1 or 2, characterized in that the expanded products or spheroids are chosen from the group comprising spheres of expanded clay, perlite, vermiculite, spherules of expanded glass or ceramic fibers.

4.- Method according to claim 1, characterized in c 35 that the fillers can consist of son or fiber filaments chosen from the group comprising glass fibers, carbon fibers, metal son, igni¬ fugged son, etc. 23

5.- Method according to any one of claims 1 4, characterized in that the total volume of the aggregates, therefore of the pulverulent fillers and of the expanded or spherical products incorporated in the composite product forms from 80 to 90% 5 total volume of the said product.

6.- Method according to any one of claims 1 4, characterized in that the polymerization catalyst ^' consists of methanol and sulfuric acid or hydrochloride.

10 7.- Installation for obtaining a building material comprising a mixing tank and a delivery block of products mixed in the tank to a mold formed of the building material, characterized in that the mixing tank ( 1) receives and mixes doses of

15 phenolic resin and powder or weight products of various materials such as micas, shales, talc, etc., which at a screw delivery block (11) delivers the kneaded products to an intermediate hopper (2) for stabilizing temperature supplying a discharge block (3) which discharges into

20 a mixing and extrusion head (4) into which also leads a pipe (32) for discharging a hardening catalyst and in that said installation comprises a set (5) of mixer of expanded charges or spheroids q pours these charges in a screw impregnator (6) connected to

25 injector (35) of the mixing head (4) capable of extruding the mixture of phenolic resin, pulverulent products and catalyst prepared in this head, the outlet (46) of the impregnator (6) being disposed at the - over molding trays (47, 47a, 47b) receiving the product before it hardens

30 pasty and sticky final consisting of expanded fillers or spheroids impregnated with said mixture.

8.- Installation according to claim 7, characterized in that the mixing tank (1) has at its base the screw delivery block (12) connected to the intermediate hopper (2) vi

35 a motorized cut-off valve (14) and to a recirculation line (16) via a motorized cut-off valve (17), these motorized valves (14 and 17) being coupled via a regulating organ (19) to a temperature probe (18) of the tank ( 24

and to a sensor (15) for pressure and / or discharge flow from the tank.

9.- Installation according to claim 7 or 8, characterized in that the intermediate hopper comprises at least one level probe (21, 22) and a temperature probe (23) and delivers, via a motorized valve (14) , the mixture of phenolic resin and fillers maintained at suitable viscosity and temperature, at its base at the discharge block (3) which is connected to an air and gas suction chamber (26)

10 occluded and in which rotates at speed adjust a booster screw (25).

10.- Installation according to one of claims 7 to 9, characterized in that the mixing and extrusion head (4) is connected from upstream to downstream in the direction of its injection.

15 tor (35): to a suction line (38) of air and gases occluded at the delivery block (3) of the kneaded and conditioned mixture of phenolic resin and of pulverulent products then to the line (32) of delivery of a curing catalyst and finally to a possible supply line (48)

20 of a liquid for rinsing the injector (35) after stopping the injection of catalyst.

11.- Installation according to one of claims 7 to 10 characterized in that the charge mixer assembly (5) e consisting of a screw mixer (42) connected from downstream to amon

25 respectively to a hopper (43) for supplying large balls of expanded products or spheroids, to a hopper (44) for supplying small balls of expanded products or spheroids and finally to a hopper (45) for supplying crowns refractory intended to give cohesion to these products

30 expanded.

12.- Installation according to one of claims 7 to 11 characterized in that the screw impregnator (6) and the injection head are made integral and are carried by a carriage (36) movable on a rolling track ( 37) in order to

35 allow the spreading of the final product leaving the impré¬ gnateur in a mold (47, 47a, 47b).

13.- Installation according to one of claims 7 to 12 characterized in that the outlet nozzle (66) of the impregnate 25

screw (6) is connected to an orifice (67) for injecting cut wire or filaments (70, 71) made of a material having good mechanical and heat resistance.

14.- Construction material based on phenoliq resin, characterized in that it contains 80 to 90% of its total volume of pulverulent fillers, of expanded products, of refractory cement, and possibly of son or filaments of fibers.

15.- Material according to claim 14, characterized in that for 100 volumes of resin, it contains from 25 to 125 v lumes of mineral fillers and from 900 to 1,275 volumes of powdered products.

16.- Material according to claim 14 or 15, caracté¬ ized in that the pulverulent fillers are chosen from a group comprising magnesium silicate, silicate of al minium, Ti0 ₂ , talc, mica, phosphogypsum, aluminum sulfate, alumina, silica, shales, magnesia and magnesium sulfate.

17.- Material according to any one of claims 1 to 16, characterized in that the expanded or spherical products are chosen from the group comprising spheres of expanded clay, perlite, vermiculite, spherules of expanded glass or fibers ceramic.

18.- Material according to any one of claims 1 to 17, characterized in that the son or filaments of fibers are chosen from the group comprising glass fibers, carbon fibers, metallic son, igni¬ fugged son, etc. .

19.- Building material according to any one of claims 14 to 18, characterized in that it is in the form of flat plates or boards capable of being sawn and machined by tools intended for sawing wood.