Classifications

• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L95/00—Compositions of bituminous materials, e.g. asphalt, tar, pitch
• • 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
  • C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
  • C04B26/02—Macromolecular compounds
  • C04B26/26—Bituminous materials, e.g. tar, pitch
• • 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
  • C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
  • C04B20/10—Coating or impregnating
  • C04B20/1018—Coating or impregnating with organic materials
  • C04B20/1029—Macromolecular compounds
  • C04B20/1044—Bituminous materials
• • 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
  • C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
  • C04B24/04—Carboxylic acids; Salts, anhydrides or esters thereof
• • 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
  • C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
  • C04B24/12—Nitrogen containing compounds organic derivatives of hydrazine
  • C04B24/124—Amides
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
  • C08K5/00—Use of organic ingredients
  • C08K5/01—Hydrocarbons
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
  • C08K5/00—Use of organic ingredients
  • C08K5/04—Oxygen-containing compounds
  • C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
• • C—CHEMISTRY; METALLURGY
  • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
  • C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
  • C10C3/00—Working-up pitch, asphalt, bitumen
  • C10C3/14—Solidifying, Disintegrating, e.g. granulating
• • E—FIXED CONSTRUCTIONS
  • E01—CONSTRUCTION OF ROADS, RAILWAYS, OR BRIDGES
  • E01C—CONSTRUCTION OF, OR SURFACES FOR, ROADS, SPORTS GROUNDS, OR THE LIKE; MACHINES OR AUXILIARY TOOLS FOR CONSTRUCTION OR REPAIR
  • E01C7/00—Coherent pavings made in situ
  • E01C7/08—Coherent pavings made in situ made of road-metal and binders
  • E01C7/18—Coherent pavings made in situ made of road-metal and binders of road-metal and bituminous binders
  • E01C7/20—Binder incorporated in cold state, e.g. natural asphalt
• • 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
  • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
  • C04B2111/0075—Uses not provided for elsewhere in C04B2111/00 for road construction

Definitions

• the present invention relates to a road bitumen in divided form, solid at room temperature.
• the present invention also relates to a method for preparing road bitumen at ambient temperature and its use as a road binder, especially for the manufacture of asphalt.
• the present invention also relates to a method for manufacturing asphalt from solid bitumen according to the invention and a method for transporting and / or storing solid road asphalt at ambient temperature according to the invention.
• bitumen used in construction, mainly for the manufacture of road pavements or in industry, for example for roofing applications. It is generally in the form of a highly viscous black material, even solid at room temperature, which becomes fluid upon heating.
• bitumen is stored and transported hot, in bulk, in tanker trucks or by boats at high temperatures of the order of 120 ° C to 200 ° C.
• the storage and transport of hot bitumen has certain disadvantages.
• the transport of hot bitumen in liquid form is considered dangerous and it is very framed from a regulatory point of view. This mode of transport presents no particular difficulties when the equipment and the transport infrastructures are in good condition.
• bitumen may increase during a trip too long. Delivery distances for bitumen are therefore limited.
• maintaining the bitumen at elevated temperatures for a long time may affect the properties of the bitumen and thus change the final performance of the bitumen.
• bitumen at room temperature in metal drums As an example of packaging for the cold transport currently used, there may be mentioned the packaging of bitumen at room temperature in metal drums. This means is increasingly questionable from an environmental point of view because the bitumen stored in the barrels must be reheated before use as a road binder. However, this operation is difficult to implement for this type of packaging and the drums are a waste after use. On the other hand, the storage of bitumen at room temperature in drums leads to losses because the bitumen is very viscous and part of the product remains on the walls of the drum when transferring to the tanks of the production units of the mix. As for handling and transporting bituminous products in these drums, they may be difficult and dangerous if specialized drum handling equipment is not available at the carriers or where the bitumen is used.
• bitumen in the form of granules transported and / or stored in bags, often used in places where the ambient temperature is high. These granules have the advantage of being easily manipulated.
• US 3,026,568 discloses bitumen granules coated with a powdery material, such as limestone powder. Nevertheless, this type of granular bitumen does not prevent the flow of bitumen, especially at high ambient temperature.
• WO2009 / 153324 discloses bitumen granules composed of a bitumen core coated with a bitumen layer having a penetration at 25 ° C of less than 5 dmm. Nevertheless, this type of granules does not prevent the flow of the bitumen constituting the core of the granules during the storage and / or transport of the bitumen at high ambient temperature because the hull made of bitumen having a penetration at 25 ° C of less than 5 dmm is not sufficiently resistant to many shocks during storage and / or transport of bitumen.
• US 2011/0290695 discloses a system for transporting bitumen in the form of paving stones, said pavers being covered with a bituminous film comprising natural bitumen and synthetic polymer gum. However, it does not describe solid bitumen at room temperature in the form of granules.
• the Applicant has therefore sought to develop bitumens capable of being subjected to the conditions of transport and / or storage and / or handling at high ambient temperatures without flowing, in particular bitumens in the form of granules whose adhesion and agglomeration during their transport and / or storage and / or manipulation at high ambient temperature are reduced compared to the granules of the prior art.
• bitumen granules comprising at least one chemical additive responding to the problem of transport and / or storage and / or handling of road bitumen at ambient temperatures.
• the bitumen used in FR 3 024 454 is a mono-grade bitumen, that is to say a bitumen of a single type of pre-determined grade and therefore the user can not modulate its properties. to optimize them according to their end use.
• An object of the present invention is to provide a road bitumen transportable and / or storable and / or manipulable at high ambient temperature, and whose properties are preserved over time.
• the object of the present invention is to provide a transportable and / or storable road bitumen for a duration greater than 2 months, preferably 3 months, and at high ambient temperature, especially at a temperature of up to 100 ° C, preferably from 20 ° C to 80 ° C.
• Another object of the invention is to provide an easily manipulable road bitumen, especially at high ambient temperature, in particular at a temperature of up to 100 ° C, preferably from 20 ° C to 80 ° C.
• the object of the present invention is to provide an easily manipulable road bitumen after a transport and / or prolonged storage time at high ambient temperature, in particular during a transport and / or storage period. greater than 2 months, preferably greater than 3 months, and a temperature of up to 100 ° C, preferably between 20 ° C and 80 ° C.
• An object of the present invention is to provide a road bitumen in a form that allows its flow in solid form at room temperature, so that it can be handled without loss of material.
• the proposed bitumen is in divided form and solid at room temperature so that it solves satisfactorily the problems mentioned above.
• Another object of the present invention is to provide a transportable and / or storable and / or manipulable road bitumen at high ambient temperature, the properties of which are conserved over time and the composition of which can be modulated according to its end use. .
• Another objective is to propose an industrial and economical process for making transportable and / or storable and / or manipulable road bitumen at ambient temperature.
• Another object of the invention is to provide an industrial and economical process for manufacturing asphalt from transportable road bitumen and / or storable and / or manipulable at room temperature.
• Another objective of the invention is to propose an ecological and economical process for transporting and / or storing and / or handling the road bitumen at ambient temperature, making it possible to avoid the use of additional means for maintaining the temperature of said bitumen during transport and / or storage and / or handling and to minimize the presence of waste and / or residues.
• the invention relates to a room-temperature solid bitumen in the form of granules comprising a core of a first bituminous material and a coating layer of a second bituminous material, wherein: the first bituminous material comprises at least one bitumen base and,
• the second bituminous material comprises:
• the invention further relates to a method for producing a solid bitumen at room temperature in the form of granules composed of a core of a first bituminous material and a core coating layer of a second bituminous material, which process comprises: i) forming the core from the first bituminous material,
• the second bituminous material comprises:
• TBA ball and ring softening temperature
• At least one chemical additive chosen from: an organic compound, a viscosifying compound, a paraffin, a polyphosphoric acid and their mixtures.
• the first bituminous material comprises at least one chemical additive chosen from: an organic compound, a viscosifying compound, a paraffin, a polyphosphoric acid and mixtures thereof.
• the chemical additive present in the first bituminous material and the additive present in the second bituminous material are identical.
• the chemical additive is an organic compound which has a molar mass of less than or equal to 2000 gmol -1 , preferably a molar mass less than or equal to 1000 gmol -1 .
• the chemical additive is a viscosifying compound which has a dynamic viscosity greater than or equal to 50 mPa ⁇ s -1 , preferably from 50 mPa ⁇ s -1 to 550 mPa ⁇ s -1 , more preferably from 80 mPa.s "1 to 450 mPa.s 1 , the viscosity being a Brookfield viscosity measured at 65 ° C.
• the coating layer has a needle penetration measured at 25 ° C according to EN 1426 greater than 5 1/10 mm.
• the core has a needle penetration measured at 25 ° C according to EN 1426 of between 10 and 850 1/10 mm.
• the invention also relates to a solid bitumen at room temperature that can be obtained by implementing the method defined above.
• the bitumen of the invention has a stability to transport and storage at a temperature ranging from 20 to 80 ° C for a period greater than or equal to 2 months, preferably greater than or equal to 3 months.
• the invention also relates to the use of solid bitumen as defined above as road binder.
• the use relates to the manufacture of asphalt.
• the subject of the invention is also a method for manufacturing mixes comprising at least one road binder and aggregates, the road binder being chosen from the above-described processes, and this method comprises at least the steps of:
• the asphalt manufacturing process does not include a heating step of the road binder before mixing with the aggregates.
• the invention also relates to a method for transporting and / or storing road bitumen, said road bitumen being transported and / or stored as solid bitumen at room temperature as described above.
• bitumen compositions in a divided form, having a core / shell structure, in which the core is based on bitumen and the coating layer based on bitumen confers on the overall structure improved properties with respect to the known bitumen granules of the prior art.
• a first object of the invention relates to a solid bitumen at ambient temperature in the form of granules comprising a core made of a first bituminous material and a coating layer made of a second bituminous material, in which:
• the first material comprises at least one bitumen base and,
• the second bituminous material comprises:
• Ambient temperature means the temperature resulting from the climatic conditions in which the road bitumen is transported and / or stored and / or handled. More precisely, the ambient temperature is equivalent to the temperature reached during the transport and / or the storage of the road bitumen, it being understood that the ambient temperature implies that no heat input is made other than that resulting from the climatic conditions.
• the invention relates to bitumens capable of being subjected to a high ambient temperature, in particular a temperature of up to 100 ° C, preferably from 20 ° C to 80 ° C.
• solid bitumen at ambient temperature is meant a bitumen having a solid appearance at ambient temperature regardless of the transport and / or storage conditions. More specifically, solid bitumen at ambient temperature is understood to mean a bitumen that retains its solid appearance throughout transport and / or storage and / or manipulation at ambient temperature, ie a bitumen that does not flow. not at room temperature under its own weight and more, which does not flow when subjected to pressure forces from transport conditions and / or storage and / or handling.
• Bitumen core means a core that is formed of at least one bituminous material designated "first bituminous material".
• the first bituminous material comprises:
• bitumen bases one or more bitumen bases
• one or more chemical additives selected from: an organic compound, a viscosifying compound, a paraffin, a polyphosphoric acid and mixtures thereof.
• Coating layer means a homogeneous layer covering all part of the surface of the heart. More specifically, it is meant that the coating layer covers at least 90% of the surface of the heart, preferably at least 95% of the surface of the heart, more preferably at least 99% of the core area.
• 'Bituminous coating layer' means a coating layer which is formed from at least one bituminous material designated 'second bituminous material'.
• the second bituminous material comprises:
• TBA ball and ring softening temperature
• bitumen and “road bitumen” are used, in an equivalent manner and independently of one another.
• Bitumen or “road bitumen” means any bituminous compositions consisting of one or more bitumen bases, said compositions being intended for road application.
• bitumen bases that may be used according to the invention, mention may first be made of bitumens of natural origin, those contained in deposits of natural bitumen, natural asphalt or bituminous sands and bitumens originating from the refining of crude oil.
• the bitumen bases according to the invention are advantageously chosen from bitumen bases originating from the refining of crude oil.
• the bitumen bases may be chosen from bitumen bases or bitumen base mixtures derived from the refining of crude oil, in particular bitumen bases containing asphaltenes or pitches.
• bitumen bases can be obtained by conventional processes for the manufacture of bitumen bases in a refinery, in particular by direct distillation and / or vacuum distillation of the oil. These bitumen bases may optionally be visbroken and / or deasphalted and / or rectified in air. Vacuum distillation of atmospheric residues from atmospheric distillation of crude oil is common. This manufacturing process therefore corresponds to the succession of an atmospheric distillation and a distillation under vacuum, the feed supplying the vacuum distillation corresponding to the atmospheric residues. These vacuum residues from the vacuum distillation tower can also be used as bitumens. It is also common to inject air into a charge usually composed of distillates and heavy products from the vacuum distillation of atmospheric residues from the distillation of petroleum.
• This method provides a base blown, or semi-blown or oxidized or rectified in air or rectified partially in air.
• the various bitumen bases obtained by the refining processes can be combined with each other to obtain the best technical compromise.
• the bitumen base can also be a bitumen base for recycling.
• the blown bitumens can be manufactured in a blowing unit, by passing a stream of air and / or oxygen through a starting bituminous base.
• This operation can be carried out in the presence of an oxidation catalyst, for example phosphoric acid.
• the blowing is carried out at high temperatures, of the order of 200 to 300 ° C, for relatively long periods of time typically between 30 minutes and 2 hours, continuously or in batches. The duration and the blowing temperature are adjusted according to the properties targeted for the blown bitumen and according to the quality of the starting bitumen.
• the chemical additive is chosen from: an organic compound, a viscosifying compound, a paraffin, a polyphosphoric acid and their mixtures.
• the chemical additive is an organic compound.
• the organic compound has a molar mass less than or equal to 2000 gmol -1 , preferably a molar mass less than or equal to 1000 gmol -1 .
• the organic compound is a compound of general formula (I):
• Ar 1 and Ar 2 represent, independently of one another, a benzene ring or a fused aromatic ring system of 6 to 20 carbon atoms, substituted by at least one hydroxyl group, and
• R represents an optionally substituted divalent radical, the main chain of which comprises from 6 to 20 carbon atoms and at least one group chosen from amide, ester, hydrazide, urea, carbamate and anhydride functions.
• Ar 1 and / or Ar 2 are preferably substituted with at least one alkyl group of 1 to 10 carbon atoms, advantageously at one or more ortho positions with respect to the hydroxyl group (s), more preferably Ar 1 and Ar2 are 3,5-dialkyl-4-hydroxyphenyl groups, advantageously 3,5-di-ter-butyl-4-hydroxyphenyl groups.
• R is in the para position with respect to a hydroxyl group of Arl and / or
• the compound of formula (I) is 2 ', 3-bis [(3- [3, 5-di-tert-butyl-4-hydroxyphenyl] propionyl]] propionohydrazide.
• the organic compound is a compound of general formula (II):
• the groups R and R ' which may be identical or different, contain a saturated or unsaturated, linear, branched or cyclic hydrocarbon-based chain comprising from 1 to 22 carbon atoms, which may be optionally substituted, and optionally comprising hetero atoms, rings and / or heterocycles;
• the X group contains a hydrocarbon chain, saturated or unsaturated, linear, cyclic or branched, comprising from 1 to 22 carbon atoms, optionally substituted, and optionally comprising hetero atoms, rings and / or heterocycles; n and m are integers having a value of 0 or 1 independently of one another.
• the groups R- (NH) n CONH and NHCO (NH) n -R ' are covalently linked by a CONH-NHCO hydrazide bond.
• the group R, or the group R ' then comprises at least one group chosen from: a hydrocarbon chain of at least 4 carbon atoms, an aliphatic ring of 3 to 8 atoms, an aliphatic condensed polycyclic system, partially aromatic or entirely aromatic, each ring comprising 5 or 6 atoms.
• the group R, the group R 'and / or the group X comprises at least one group chosen from: a hydrocarbon chain of at least 4 carbon atoms an aliphatic ring of 3 to 8 atoms, an aliphatic condensed polycyclic ring system, partially aromatic or wholly aromatic, each ring comprising 5 or 6 atoms.
• the group R and / or R ' comprises an aliphatic hydrocarbon chain of 4 to 22 carbon atoms, in particular selected from the C4H groups 9, C5H11, C 9 H1 9, C11H2 3, C12H25, C 17 H 3 5 C1 8 H 3 7, 3 C21H4, C22H45.
• the group X represents a saturated linear hydrocarbon chain comprising from 1 to 22 carbon atoms.
• the group X is selected from C2H4 groups, C 3 H 6.
• the group X may also be a cyclohexyl group or a phenyl group, the radicals R- (NH) n CONH- and NHCO (NH) n -R'- may then be in the ortho, meta or para position. Moreover, the radicals R- (NH) n CONH- and NHCO (NH) n -R'- may be in the cis or trans position with respect to each other. In addition, when the radical X is cyclic, this ring may be substituted by groups other than the two main groups R- (NH) n CONH- and -NHCO (NH) n -R '.
• the X group comprises two 6-carbon rings connected by a CH 2 group, these rings being aliphatic or aromatic.
• the group X is a group comprising two aliphatic rings connected by an optionally substituted CH 2 group, for example:
• the organic compound is a compound of general formula (II) chosen from hydrazide derivatives such as the compounds C 5 H 11 CONH-NHCO-C 5 H 11, C 9 H 19 -CONH-NHCO-C 9 H 19 , C 11 H 23 CONH-NHCO -C11H23, C17H35-CONH-NHCO-C17H35, or C21H43-CONH-NHCO-C21H43; diamides such as ⁇ , ⁇ '-ethylenedi (stearamide) of the formula C 17 H 35 CONH-CH 2 -CH 2 -NHCO-C 17 H 35; and derivatives ureides such as 4,4'-bis (dodécylaminocarbonylamino) diphénylmetriane of formula C12H25- NHCONH-C 6 H4-CH 2 -C 6 H 4 -NHCONH 2 C 1 H 25.
• hydrazide derivatives such as the compounds C 5 H 11 CONH-NHCO-C 5 H 11, C
• the organic compound is a compound of formula (III):
• R and R ' which may be identical or different, contain a linear, branched or cyclic saturated or unsaturated hydrocarbon-based chain containing from 1 to 22 carbon atoms, which may be optionally substituted, and optionally comprising hetero atoms, rings and / or heterocycles,
• Z represents a tri-functionalized group chosen from the following groups:
• the compound of formula (III) is N 2, N 4, N 6 -tridecylmelamine having the following formula with R 'representing the group C 9 H 19 :
• HN A preferred compounds corresponding to formula (III) are such that x is equal to 0, Z represents Z 2 and R 'represents a linear saturated hydrocarbon-based chain of 1 to 22 carbon atoms, preferably 2 to 18 carbon atoms, preferably 5 to 12 carbon atoms.
• R selected from the following groups, taken alone or in mixtures:
• the organic compound is a product of the reaction of at least one C3-C12 polyol and at least one C2-C12 aldehyde.
• the polyols that may be used, mention may be made of sorbitol, xylitol, mannitol and / or ribitol.
• the polyol is sorbitol.
• the organic compound is a compound which comprises at least one function of general formula (IV):
• x is an integer, x can be equal to 0,
• R is chosen from an alkyl, alkenyl, aryl or aralkyl radical C1-C1, optionally substituted with one or more halogen atoms, one or more C1-C6 alkoxy groups.
• the organic compound is advantageously a derivative of sorbitol.
• sorbitol derivative is meant any reaction product, obtained from sorbitol.
• any reaction product obtained by reacting an aldehyde with D-sorbitol. This condensation reaction produces sorbitol acetals, which are derivatives of sorbitol.
• 1,3: 2,4-Di-O-benzylidene-D-sorbitol is obtained by reacting 1 mole of D-sorbitol and 2 moles of benzaldehyde and has the formula:
• sorbitol derivatives may thus be all the condensation products of aldehydes, especially aromatic aldehydes with sorbitol. Sorbitol derivatives of general formula will then be obtained:
• Ari and Ar 2 are optionally substituted aromatic rings.
• sorbitol other than 1,3: 2,4-Di-O-benzylidene-D-sorbitol
• 1,3: 2,4-Di-O-benzylidene-D-sorbitol there can be found, for example, 1,3,3,4,5,6-tri-O-benzylidene.
• the organic compound is a compound of general formula (V):
• the group R " is preferably a saturated linear chain of formula C w H 2w with w an integer ranging from 4 to 22, preferably from 4 to 12.
• the diacids may also be diacid dimers of unsaturated fatty acid (s), that is to say dimers formed from at least one unsaturated fatty acid, for example from a single fatty acid. unsaturated or from two different unsaturated fatty acids.
• the diacid dimers of unsaturated fatty acid (s) are conventionally obtained by intermolecular dimerization reaction of at least one unsaturated fatty acid (reaction of Diels Aid for example).
• Preferably, only one type of unsaturated fatty acid is dimerized. They derive, in particular, from the dimerization of an unsaturated fatty acid, especially of C 1 to C 34, in particular of C 12 to C 22 , in particular of C 16 to C 20, and more particularly to C 18 .
• a preferred fatty acid dimer is obtained by dimerization of linoleic acid, which can then be partially or fully hydrogenated.
• Another preferred fatty acid dimer is obtained by dimerization of methyl linoleate. In the same way, it is possible to find triacids of fatty acids and tetracides of fatty acids, obtained respectively by trimerization and tetramerization of at least one fatty acid.
• the organic compound is a compound of general formula (VI):
• the groups Y and Y ' represent, independently of one another, an atom or a group chosen from: H, - (CH 2 ) q -CH 3 , - (CH 2 ) q -NH 2 , - (CH 2 ) q-OH, - (CH 2 ) q-
• the organic compound of general formula (VI) is:
• the organic compound is a compound of general formula (VII):
• R-NH-CO-CO-NH-R '(VII) in which R and R', which may be identical or different, represent a saturated or unsaturated, linear, branched or cyclic hydrocarbon-based chain comprising from 1 to 22 carbon atoms, preferably 8 to 12 carbon atoms, optionally substituted, and optionally comprising hetero atoms, rings and / or heterocycles.
• R and R' which may be identical or different, represent a saturated or unsaturated, linear, branched or cyclic hydrocarbon-based chain comprising from 1 to 22 carbon atoms, preferably 8 to 12 carbon atoms, optionally substituted, and optionally comprising hetero atoms, rings and / or heterocycles.
• the chemical additive is chosen from organic compounds, it is preferably chosen from compounds of formula (I) and compounds of formula (V).
• the chemical additive is preferably 2 ', 3-bis [(3- [3, 5-di-tert-butyl-4-hydroxyphenyl] propionyl]] propionohydrazide.
• the chemical additive is preferably sebacic acid or 1,10-decanedioic acid.
• the chemical additive is a paraffin.
• Paraffins have chain lengths of 30 to 120 carbon atoms (C 30 to C 120).
• the paraffins are advantageously chosen from polyalkylenes.
• polymethylene paraffins and polyethylene paraffins will be used according to the invention. These paraffins may be of petroleum origin or come from the chemical industry.
• the paraffins used are synthetic paraffins resulting from the conversion of biomass and / or natural gas.
• these paraffins contain a large proportion of so-called "normal" paraffins, that is straight-chain, unbranched linear paraffins (saturated hydrocarbons).
• the paraffins may comprise from 50 to 100% of normal paraffins and from 0 to 50% of isoparaffins and / or branched paraffins. More preferably, the paraffins comprise from 85 to 95% of normal paraffins and from 5 to 15% of isoparaffins and / or branched paraffins.
• the paraffins comprise from 50 to 100% of normal paraffins and from 0 to 50% of isoparaffins. Even more advantageously, the paraffins comprise from 85 to 95% of normal paraffins and from 5 to 15% of isoparaffins.
• the paraffins are polymethylene paraffins. More particularly, paraffins are synthetic paraffins of polymethylene, for example paraffins resulting from the conversion of synthesis gas by the Fischer-Tropsch process. In the Fischer-Tropsch process, paraffins are obtained by reaction of hydrogen with carbon monoxide on a metal catalyst. Fischer-Tropsch synthesis methods are described for example in the publications EP 1 432 778, EP 1 328 607 or EP 0 199 475.
• the chemical additive is a polyphosphoric acid.
• the polyphosphoric acids (PPA) that can be used in the invention are described in WO 97/14753.
• said polyphosphoric acids may be linear compounds of formula P q H ( q + 2 ) O (3q + 1) corresponding to the structural formula:
• All these polyphosphoric acids can be considered as polycondensation products by heating aqueous metaphosphoric acid.
• the chemical additive is a viscosifying compound.
• the viscosifying compound is a compound which has the property of reducing the fluidity of a liquid or of a composition and thus of increasing its viscosity.
• viscosifier and “viscosifying compound” are used in the sense of the invention, in an equivalent manner and independently of one another.
• the viscosifying compound is a material which has a dynamic viscosity greater than or equal to 50 mPa ⁇ s -1 , preferably from 50 mPa ⁇ s -1 to 550 mPa ⁇ s -1 , more preferably 80 mPa ⁇ s 1 to 450 mPa ⁇ s -1 , the viscosity being a Brookfield viscosity measured at 65 ° C.
• the viscosity of a viscosifier according to the invention is measured at 65 ° C. using a Brookfield CAP 2000+ viscometer. and at a speed of rotation of 750 rpm The reading of the measurement is carried out after 30 seconds for each temperature.
• the viscosifying compound is chosen from: gelling compounds preferably of vegetable or animal origin, such as: gelatin, agar-agar, alginates, cellulose derivatives, starches, modified starches, or gellan gums;
• gelling compounds preferably of vegetable or animal origin, such as: gelatin, agar-agar, alginates, cellulose derivatives, starches, modified starches, or gellan gums;
• PEG polyethylene glycols
• PEG- 1 polyethylene glycols
• 800 a PEG having a molecular weight of 800 gmol -1
• 800 a PEG having a molecular weight of 1000 gmol -1
• PEG-1500 a PEG having a molecular weight of 4000 g Molar 1 (PEG-4000) or PEG having a molecular weight of 6000 gmol -1 (PEG-6000);
• the chemical additive is chosen from an organic compound, a viscosifying compound, a paraffin and mixtures thereof.
• the chemical additive is chosen from an organic compound, a viscosifying compound, a polyphosphoric acid and mixtures thereof.
• the chemical additive is chosen from an organic compound, a viscosifying compound and mixtures thereof.
• the chemical additive is chosen from viscosifiers.
• the bitumen base comprises from 0.1% to 20% by weight, preferably from 0.5% to 15% by weight, more preferably from 0.5% to 10% by weight. mass of chemical additive with respect to the total mass of said bitumen base.
• the bitumen base comprising the additive has a ball and ring softening temperature (TBA) of between 80 ° C. and 130 ° C., more preferably between 90 ° C. and 130 ° C., it being understood that the TBA is measured according to the EN 1427 standard.
• TBA ball and ring softening temperature
• the core or core of the solid bitumen granules according to the invention is prepared from at least one first bituminous material, said first bituminous material being prepared by putting in contact :
• bitumen bases one or more bitumen bases
• one or more chemical additives chosen from: an organic compound, a viscosifying compound, a paraffin, a polyphosphoric acid and mixtures thereof.
• the chemical additive is as defined above.
• the core or core of the solid bitumen granules according to the invention is prepared from at least one first bituminous material, said first bituminous material being prepared by bringing into contact:
• bitumen bases one or more bitumen bases
• At least one chemical additive selected from: an organic compound, a viscosifying compound, a paraffin, a polyphosphoric acid and mixtures thereof.
• compositions comprising at least one bitumen base and optionally one or more chemical additives constitute the first bituminous material.
• the first bituminous material, used to manufacture the core of the granules of the invention has a needle penetration measured at 25 ° C according to EN 1426 from 10 to 850 1/10 mm, preferably from 20 to 600 1/10 mm, more preferably 20 to 330 1/10 mm.
• the so-called "needle penetration” measurement is carried out by means of a standardized test NF EN 1426 at 25 ° C. (P25). This characteristic of penetrability is expressed in tenths of a millimeter (dmm or 1/10 mm).
• the needle penetration, measured at 25 ° C, according to the standardized test NF EN 1426 represents the measurement of the penetration into a sample bitumen, after a time of 5 seconds, a needle whose weight with its support is 100 g.
• the first bituminous material, used to manufacture the core of the granules of the invention advantageously has a dynamic viscosity of between 50 and 200 mPa.s, preferably between 70 and 150 mPa.s, the viscosity being a Brookfield viscosity measured at 135 ° C.
• the bitumen base forming the core of the granules according to the invention may also comprise at least one known bitumen elastomer such as copolymers SB (block copolymer of styrene and butadiene), SBS ( styrene-butadiene-styrene block copolymer), SIS (styrene-isoprene-styrene), SBS * (styrene-butadiene-styrene star block copolymer), SBR (styrene-b-butadiene rubber), EPDM (ethylene propylene diene) amended).
• copolymers SB block copolymer of styrene and butadiene
• SBS styrene-butadiene-styrene block copolymer
• SIS styrene-isoprene-styrene
• SBS * styrene-butadiene-
• the first bituminous material advantageously comprises from 1 to 10% by weight, preferably from 2 to 8% by weight, more preferably from 3 to 6% by weight of elastomer relative to the total weight of said first material. bituminous material.
• the first bituminous material may further comprise at least one olefinic polymer builder.
• the olefinic polymer adjuvant is preferably selected from the group consisting of (a) ethylene / glycidyl (meth) acrylate copolymers; (b) ethylene / monomer A / monomer B terpolymers and (c) copolymers resulting from the grafting of a monomer B onto a polymer substrate.
• the ethylene / glycidyl (meth) acrylate copolymers are advantageously chosen from random or block copolymers, preferably random copolymers of ethylene and a monomer chosen from glycidyl acrylate and glycidyl methacrylate, comprising from 50% to 99.7% by weight, preferably from 60% to 95% by weight, more preferably 60% to 90% by weight of ethylene.
• the terpolymers are advantageously chosen from random or sequential terpolymers, preferably random, of ethylene, a monomer A and a monomer B.
• the A monomer is selected from vinyl acetate and alkyl acrylates or methacrylates to C 6.
• Monomer B is selected from glycidyl acrylate and glycidyl methacrylate.
• the ethylene / monomer A / monomer B terpolymers comprise from 0.5% to 40% by weight, preferably from 5% to 35% by weight, more preferably from 10% to 30% by weight of units derived from monomer A, and from 0.5% to 15% by weight, preferably from 2.5% to 15% by weight of units derived from monomer B, the remainder being formed from units derived from ethylene.
• the copolymers result from the grafting of a B monomer selected from glycidyl acrylate and glycidyl methacrylate onto a polymeric substrate.
• the polymer substrate consists of a polymer chosen from polyethylenes, in particular low density polyethylenes, polypropylenes, statistical or sequential copolymers, preferably random copolymers of ethylene and vinyl acetate, and statistical or block copolymers, preferably statistical copolymers.
• polyethylenes in particular low density polyethylenes, polypropylenes, statistical or sequential copolymers, preferably random copolymers of ethylene and vinyl acetate, and statistical or block copolymers, preferably statistical copolymers.
• ethylene and C 1 -C 6 alkyl acrylate or methacrylate comprising from 40% to 99.7% by weight, preferably from 50% to 99% by weight of ethylene.
• Said graft copolymers comprise from 0.5% to 15% by weight, preferably from 2.5% to 15% by weight of grafted units derived from monomer B.
• the olefinic polymer adjuvant is chosen from among the random terpolymers of ethylene (b), a monomer A chosen from C1-C6 alkyl acrylates or methacrylates and a monomer B chosen from acrylate.
• a monomer A chosen from C1-C6 alkyl acrylates or methacrylates
• a monomer B chosen from acrylate.
• glycidyl and glycidyl methacrylate comprising from 0.5% to 40% by weight, preferably from 5% to 35% by weight, more preferably from 10% to 30% by weight of units derived from monomer A, and from 0, From 5% to 15% by weight, preferably from 2.5% to 15% by weight of units derived from monomer B, the remainder being formed from units derived from ethylene.
• the first bituminous material of which the core of the granules is composed comprises from 0.05% to 15% by weight, preferably from 0.1% to 10% by weight, more preferably from 0.5% to 6% by weight of the olefinic polymer adjuvant relative to the total mass of said first bituminous material.
• the core may further comprise at least one anti-caking agent, preferably of mineral or organic origin.
• the anti-caking agent is chosen from talc; the fines generally of diameter less than 125 ⁇ with the exception of fine limestones, such as siliceous fines; sand such as fountain sand; cement ; carbon; wood residues such as lignin, lignosulphonate, conifer needle powders, conifer cone powders, especially pine powders; glass powder; clays such as kaolin, bentonite, vermiculite; alumina such as alumina hydrates; silica; silica derivatives such as silicates, silicon hydroxides and silicon oxides; plastic powder; lime; the plaster ; rubber powder; polymer powder such as styrene-butadiene copolymers (SB), styrene-butadiene-styrene copolymers (SBS); and their mixtures.
• fine limestones such as siliceous fines
• sand such as fountain sand
• cement carbon
• wood residues such as lign
• anti-caking agent is chosen from talc; the fines generally of diameter less than 125 ⁇ with the exception of fine limestones, such as siliceous fines; wood residues such as lignin, lignosulphonate, conifer needle powders, conifer cone powders, especially pine powders; glass powder; sand such as fountain sand; and their mixtures.
• the first bituminous material further comprises between 0.5% and 20% by weight, preferably between 2% and 20% by weight, more preferably between 2% and 15% by weight of ⁇ anti-caking agent with respect to the total mass of the first bituminous material.
• the coating layer of bituminous material is the coating layer of bituminous material
• the coating layer is made of a second bituminous material comprising: at least one bitumen base and at least one chemical additive selected from: an organic compound, a viscosifying compound, a paraffin, a polyphosphoric acid and mixtures thereof; or
• TBA ball and ring softening temperature
• the second bituminous material is solid at room temperature, including at elevated ambient temperature.
• the chemical additive is as defined above.
• the coating layer of bituminous material comprises at least one bitumen base, or at least one pitch having a ball and ring softening temperature (TBA) of greater than or equal to 80 ° C., it being understood that TBA is measured according to standard EN 1427, or a mixture of these materials and a chemical additive selected from: an organic compound, a viscosifying compound, a paraffin, a polyphosphoric acid and mixtures thereof.
• TBA ball and ring softening temperature
• pitch is a residue of distillation of petroleum tars, coal tar, wood or other organic molecules.
• the pitch used in the present invention is advantageously chosen from the distillation residues of petroleum tars.
• Petroleum pitch is mainly composed of a mixture of aromatic hydrocarbons and aromatic hydrocarbons substituted with alkyl groups.
• “Petroleum pitch” is in solid form at room temperature.
• the pitches can be obtained by conventional refinery manufacturing processes.
• the manufacturing process corresponds to the succession of atmospheric distillation and vacuum distillation.
• the crude oil is subjected to distillation at atmospheric pressure, which leads to the obtaining of a phase gas, various distillates and an atmospheric distillate residue.
• the residue of the atmospheric distillation is itself subjected to distillation under reduced pressure, called vacuum distillation, which makes it possible to separate a heavy gas oil, various sections of distillate and a distillation residue under vacuum.
• This vacuum distillation residue contains "petroleum pitch" in varying concentration.
• the vacuum distillation residue is subjected to a desalting operation by addition of a suitable solvent, such as an alkane type solvent comprising from 3 to 6 carbon atoms, for example n-propane, which thus makes it possible to precipitate the pitch and separate it from the unpaved oil.
• a suitable solvent such as an alkane type solvent comprising from 3 to 6 carbon atoms, for example n-propane, which thus makes it possible to precipitate the pitch and separate it from the unpaved oil.
• pitches are generally appreciated by determining a series of mechanical characteristics by standardized tests, the most used of which are needle penetration expressed in 1/10 mm and the softening point determined by the ball and ring test. , also called ball and ring softening temperature (TBA).
• TSA ball and ring softening temperature
• the pitch has a ball and ring softening temperature (TBA) of between 80 ° C. and 180 ° C., more preferably between 80 ° C. and 170 ° C., it being understood that the TBA is measured according to the EN 1427 standard.
• TBA ball and ring softening temperature
• pitches according to the invention it is possible to use a pitch having a ball and ring softening temperature (TBA) of between 130 ° C. and 160 ° C., it being understood that the TBA is measured according to the EN 1427 standard.
• TBA ball and ring softening temperature
• a pitch also having a dynamic viscosity ranging from 1500 to 2500 mPa.s, preferably from 1800 to 2200 mPa.s, more preferably from 2000 to 2100 mPa.s. the viscosity being a Brookfield viscosity measured at 200 ° C.
• the pitch used according to the invention has a ball and ring softening temperature (TBA) of from 130 ° C. to 160 ° C., it being understood that the TBA is measured according to EN 1427 and a dynamic viscosity of 1800 to 2200 mPa.s, the viscosity being a Brookfield viscosity measured at 200 ° C.
• TBA ball and ring softening temperature
• the second bituminous material has a needle penetration measured at 25 ° C according to EN 1426 greater than 5 1/10 mm, preferably ranging from 5 to 40 1/10 mm with the value 5 excluded, more preferably ranging from 6 to 40 1/10 mm.
• the coating layer of second bituminous material may optionally comprise at least one olefinic polymer builder as defined above.
• the second bituminous material comprises from 0.05% to 15% by weight, preferably from 0.1% to 10% by weight, more preferably from 0.5% to 6% by weight. > in mass of the olefinic polymer adjuvant relative to the total mass of the second bituminous material.
• the second bituminous material may optionally comprise at least one bitumen elastomer as defined above.
• the coating layer comprises from 1 to 10% by weight, preferably from 2 to 8% by weight, more preferably from 3 to 6% by weight of elastomer relative to the total mass of the second material. bituminous.
• the second bituminous material may optionally comprise at least one anti-caking agent as defined above.
• the second bituminous material further comprises between 0.5% and 30% by weight, preferably between 2% and 25% by weight, more preferably between 2% and 20% by weight. anti-caking P with respect to the total mass of the second bituminous material.
• the solid bitumen at room temperature may further comprise a second coating layer.
• second coating layer means a homogeneous coating layer covering in part the surface of the first coating layer surrounding the core, and directly in contact with the core, also called “first coating layer”. More specifically, it is meant that the second coating layer covers at least 90% of the surface of the first coating layer, preferably at least 95% of the surface of the first coating layer, more preferably at least 99% of the surface of the first coating layer. In this particular embodiment, the second coating layer may cover at least a portion of the surface of the first coating layer with an anti-caking agent as defined above.
• the second coating layer may be obtained by applying a composition comprising at least one viscosifying compound as defined above and at least one anti-caking compound as defined above. on all or part of the surface of the first coating layer.
• the second coating layer is solid at room temperature, including at elevated ambient temperature.
• the composition comprising the second coating layer comprising at least one viscosifying compound and at least one anti-caking compound, has a viscosity greater than or equal to 200 mPa.s -1 , preferably between 200 mPa. s “1 and 700 mPa.s " 1 , the viscosity being Brookfield viscosity.
• the second coating layer comprises at least 10% by weight of a viscosifying compound relative to the total mass of the second coating layer, preferably from 10 to 90% by weight, more preferably from 10 to 85% by weight. mass.
• the second coating layer comprises from 10 to 90% by weight of viscosifying compound relative to the total mass of the second coating layer, preferably from 15 to 85%, even better from 15 to 60%.
• the second coating layer comprises from 10 to 90% by weight of anti-caking compound relative to the total mass of the second coating layer, preferably from 15 to 85%, even better from 40 to 85%.
• the second layer of coating comprises from 10 to 90% by weight of viscosifying compound with respect to the total mass of the second coating layer, preferably from 40 to 90%, more preferably from 60 to 90%.
• the second coating layer comprises from 10 to 90% by weight of anti-aging compound. agglomerating with respect to the total mass of the second coating layer, preferably from 10 to 60%, more preferably from 10 to 40%.
• the second coating layer comprises at least 10% by weight of an anti-caking compound relative to the total mass of the second coating layer, preferably from 10 to 90% by weight, more preferably from 15 to 90% by weight.
• the viscosifying compound and the anti-caking compound represent at least 90% by weight relative to the total mass of the second coating layer, more preferably at least 95% by weight and preferably at least 98% by weight.
• the second coating layer consists essentially of the viscosifying compound and the anti-caking compound.
• the solid bitumen at room temperature is packaged in a divided form, that is to say in the form of small units, which are called granules or particles, comprising a core based on bitumen and a shell or shell or coating or coating layer.
• the granules of solid bitumen according to the invention may have within the same population of granules, one or more forms chosen from a cylindrical, spherical or ovoid shape.
• the size of the bitumen granules is such that the longest average dimension is preferably less than or equal to 30 mm, more preferably 5 to 30 mm, even more preferably 5 to 20 mm.
• the size and shape of the bitumen granules may vary depending on the manufacturing process employed. For example, the use of a die makes it possible to control the manufacture of granules of a chosen size. Sieving allows the selection of granules according to their size.
• the bitumen granules according to the invention have a weight ranging from 1 mg to 5 g, preferably from 10 mg to 4 g, more preferably from 50 mg to 2 g.
• the coating layer of the second bituminous material according to the invention makes it possible to obtain a coating layer:
• the coating layer (s) resists (s) transport and / or storage and / or handling of the bitumen at room temperature in "Big Bags” while being suitable (s) for the manufacture of asphalt. It (s) allow) the liberation of the core first bituminous material during the manufacture of asphalt under the effect of mechanical shearing and / or liquefying in contact with hot aggregates.
• the solid bitumen has: a core made of a first bituminous material, comprising at least one bitumen base and,
• a coating layer of a second bituminous material comprising:
• the solid bitumen has: a core made of a first bituminous material, comprising at least one bitumen base and,
• a coating layer of a second bituminous material comprising:
• At least one chemical additive chosen from an organic compound, a viscosifying compound, a paraffin, a polyphosphoric acid and their mixtures, and
• TBA ball and ring softening temperature
• the additive present in the first bituminous material and the additive present in the second bituminous material are identical.
• the solid bitumen consists essentially of: a core made of a bituminous material consisting of a bitumen base and a coating layer of a second bituminous material comprising:
• Another subject of the invention relates to a process for manufacturing a solid bitumen at room temperature in the form of granules composed of a core in a first bituminous material and a coating layer of a second bituminous material, which process comprises:
• the shaping step ii) is done by dipping, spraying, coextruding, etc.
• the method further comprises the step iii) of shaping the second coating layer on all or part of the surface of the first coating layer obtained in step ii).
• the shaping of the core of the granules according to the invention from a first bituminous material comprising at least one bitumen base optionally additive with at least one chemical additive may be carried out according to any known process, for example according to the manufacturing method described. in US 3,026,568, WO 2009/153324 or WO 2012/168380. According to a particular embodiment, the shaping of the solid bitumen core can be carried out by dripping, in particular by means of a drum.
• the core particles of solid bitumen have a longest average dimension ranging from from 1 to 20 mm, advantageously from 4 to 12 mm.
• Another object of the invention is a solid bitumen at room temperature in the form of granules obtainable by the implementation of the method according to the invention as described above.
• Such solid bitumen in the form of granules advantageously has the properties described above.
• Another object of the invention also relates to the use of solid bitumen granules at ambient temperature according to the invention as described above as road binder.
• the road binder can be used to manufacture mixes, in combination with aggregates according to any known method.
• the solid bitumen at ambient temperature is used for the manufacture of bituminous mixes.
• Bituminous mixes are used as materials for the construction and maintenance of pavement bodies and their pavement, as well as for the realization of all road works. For example, superficial coatings, hot mixes, cold mixes, cold mixes, low emulsions, base layers, binding, hooking and rolling, and other combinations of a bituminous binder and road aggregate having particular properties, such as anti-rutting layers, draining asphalts, or asphalts (mixture between an asphalt binder and sand-like aggregates).
• an asphalt mix comprises:
• aggregates means mineral fillers such as fines, sand or chippings, but also synthetic fillers.
• the mineral fillers consist of fines or filaments (particles smaller than 0.063 mm in size), sand (particles with dimensions of between 0.063 mm and 2 mm), and possibly chippings (particles larger than 2 mm in size, preferably between 2 mm and 4 mm).
• Fine or sand, sands and chippings are aggregates preferably meeting the specifications of NF EN 13043.
• a granulate can be natural, artificial or recycled.
• the natural granulate is a granulate of mineral origin that has not undergone any transformation other than mechanical.
• Artificial granulate is a granulate of mineral origin resulting from an industrial process including thermal or other transformations.
• Aggregates are generally referred to in terms of lower (d) and upper (D) sieve sizes, expressed as "d / D" corresponding to the granular class. This designation allows that grains can be retained on the upper sieve (refusal on D) and that others can pass through the lower sieve (passing to d).
• Aggregates are grains of dimensions between 0 and 125mm.
• the fines like the fiirers are a granular fraction of a granulate which passes through a sieve of 0.063 mm.
• Filler is a granulate most grains pass through a 0.063 mm sieve and can be added to building materials to give them certain properties.
• the sands are 0/2 aggregates according to standard NF EN 13043 for bituminous mixtures.
• Chippings are aggregates for which d> 2 mm and D ⁇ 45 mm according to standard NF EN 13043 for bituminous mixtures and coatings.
• the fines are of any mineral nature. They are preferably chosen from calcareous type fi lers.
• the granulometry of the fines according to the invention is preferably less than 63 ⁇ m.
• the sands are preferably chosen from semi-crushed or rolled sands.
• the granulometry of the sands according to the invention is preferably between 63 ⁇ and 2 mm.
• the chippings are chosen from chippings of any geological nature with a density greater than 1.5.
• the granulometry of the chippings according to the invention is between 2mm and 14mm.
• the chippings are preferably selected from the particle sizes 2/6, 4/6, 6/10, and 10/14.
• Another subject of the invention relates to a process for manufacturing asphalt mixes comprising at least one road binder and aggregates, the road binder being chosen from among the bitumens according to the invention, this process comprising at least the steps of: aggregates at a temperature of from 100 ° C to 180 ° C, preferably from
• a tank such as a kneader or a kneading drum
• the method of the invention has the advantage of being able to be implemented without any prior step of heating the solid bitumen granules.
• the method for manufacturing mixes according to the invention does not require a step of heating the granules of solid bitumen before mixing with the aggregates because in contact with the hot aggregates, the solid bitumen at ambient temperature melts.
• the solid bitumen at ambient temperature according to the invention as described above has the advantage of being able to be added directly to the hot aggregates, without having to be melted before mixing with the hot aggregates.
• the step of mixing the aggregates and road binder is carried out with stirring, then the stirring is maintained for at most 5 minutes, preferably at most 1 minute to allow to obtain a homogeneous mixture.
• the solid bitumen in the form of granules according to the present invention is remarkable in that it allows the transport and / or the storage of road bitumen at ambient temperature under optimum conditions, in particular without there being agglomeration and / or adhesion solid bitumen during transport and / or storage, even when the ambient temperature is high. Furthermore, the coating layer (s) of the granules break (s) under the effect of contact with hot aggregates and shear and releases (s) the bitumen base. Finally, the presence of the coating layer (s) in the road binder and aggregate mixture does not degrade the properties of said road bitumen for road application, compared to an uncoated bitumen base.
• Another object of the invention also relates to a method for transporting and / or storing and / or handling road bitumen, said road bitumen being transported and / or stored and or handled in the form of solid bitumen granules at room temperature.
• the road bitumen is transported and / or stored at a high ambient temperature for a period greater than or equal to 2 months, preferably 3 months.
• the high ambient temperature is from 20 ° C to 90 ° C, preferably from 20 ° C to 80 ° C, more preferably from 40 ° C to 80 ° C, still more preferably from 40 ° C to 60 ° C .
• bitumen granules according to the invention have the advantage of maintaining their divided form, and therefore of being able to be handled, after storage and / or transport at a high ambient temperature. They have in particular the ability to flow under their own weight without flowing, which allows their storage in a packaging bags, drums or containers of all shapes and volumes and their transfer from there conditioning to equipment, such as construction equipment (tank, mixer, etc.).
• bitumen granules are preferably transported and / or stored in bulk in bags of 1 kg to 100 kg or 500 kg to 1000 kg commonly known in the field of road bitumens of "Big Bag", said bags being preferably in hot melt material. They may also be transported and / or stored loose in cartons of 5 kg to 30 kg or in drums of 100 kg to 200 kg.
• the variation of the ball and ring softening temperature is measured according to standard NF EN 1427 between the sample extracted from the upper part of the sample tube and the sample extracted from the lower part of the sample tube.
• Bitumens B 3 and B 4 are prepared from:
• the non-additive bitumen base is introduced into a reactor and is maintained at 160 ° C. with stirring at 300 rpm for two hours.
• the additive is then introduced into the reactor and the whole is maintained at 160 ° C. with stirring at 300 rpm for 1 hour.
• the core of the granules consists of bitumen B 3 and the coating layer consists of bitumen B 4 .
• the additive bitumen base B 4 is heated at 160 ° C. for two hours in an oven.
• the additive bitumen base B 4 previously heated, is then cast in silicone molds having different spherical holes and then impressions are applied directly to the molds filled with bitumen so as to obtain bitumen coating layers in the form of hollow half-spheres.
• the surplus is leveled with a heated blade Bunsen burner.
• the coating layer formed is demolded.
• the bitumen coating layer is then allowed to cool to room temperature for 10 to 15 minutes.
• Each of the solid bitumen coating layers obtained in the form of a hollow half-sphere is then filled at room temperature with the additive bituminous material B3.
• the half-spheres thus filled are then sealed in pairs by means of a spatula previously heated so as to obtain a solid bitumen at room temperature in the form of granules according to the invention comprising a bitumen core and a coating layer. bitumen.
• the granules of solid bitumen Gi according to the invention were prepared according to the general method 1.1 described above.
• the compositions of these granules are described in Table 2.
• the granules of solid bitumen Gi according to the invention have a size of between 4 and 10 mm.
• the purpose of this test is to simulate the crushing strength of granules contained in an 800 kg big bag placed on a pallet of 1.21 m 2 .
• a mass of 208 g is applied to a surface of a 2 cm diameter piston.
• the laboratory assembly consists of a syringe containing the granules on which is installed a box filled with aggregates for a mass of 208 g. The whole is placed in an oven set at 40 ° C for 24 hours. After each test, the piston is removed and the compressive strength of the granules is evaluated visually, in particular their appearance and their ability to agglomerate. The observations are listed in Table 3 below. Table 3
• the granules retain their original form and do not adhere to each other.
• the granules do not adhere to each other but no longer have their rounded shape.
• Gi granules according to the invention have a very good resistance at an ambient temperature of 40 ° C insofar as they do not adhere to each other and retain their original shape. Thus, handling and transport / storage of said granules Gi will be easy to the extent that the granules do not melt and do not agglomerate with each other at high ambient temperature.
• This test is carried out in order to evaluate the load resistance of Gi granules at a temperature of 40 ° C. under a compressive force. Indeed, this test makes it possible to simulate the temperature and compression conditions of the granules on each other to which they are subjected during transport and / or storage in bulk in bags of 10 to 30 kg or in Big Bags of 500 to 1000 kg or in drums of 200 kg and to evaluate their resistance under these conditions.
• the load resistance test is carried out using a texture analyzer sold under the name LF Plus® by the company LLOYD Instruments and equipped with a thermal enclosure. To do this, a 25 mm diameter metal container containing a mass of 10 g of bitumen granules is placed inside the thermal enclosure set at a temperature of 40 ° C for 3 hours.
• the piston of the texture analyzer is a cylinder with a diameter of 20 mm and a height of 60 mm.
• the cylindrical piston is initially placed in contact with the upper layer of the granules. Then, it moves vertically downwards, at a constant speed of 0.5 mm / min over a calibrated distance of 5 mm so as to exert a compressive force on all the granules placed in the container. After removal of the piston, it is visually assessed the compressive strength of the granules, including their appearance and ability to agglomerate. The observations are listed in Table 4 below.
• the granules retain their original form and do not adhere to each other.
• the granules do not adhere to each other but no longer have their rounded shape.
• Gi granules according to the invention have a very good resistance to charging at 40 ° C insofar as they do not adhere to each other and remain separate.

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