EP3612617A1 - Bitume solide a temperature ambiante - Google Patents
Bitume solide a temperature ambianteInfo
- Publication number
- EP3612617A1 EP3612617A1 EP18722688.1A EP18722688A EP3612617A1 EP 3612617 A1 EP3612617 A1 EP 3612617A1 EP 18722688 A EP18722688 A EP 18722688A EP 3612617 A1 EP3612617 A1 EP 3612617A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- binder
- granules
- bitumen
- weight
- silicates
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
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- 239000007787 solid Substances 0.000 title description 27
- 239000011230 binding agent Substances 0.000 claims abstract description 217
- 239000000203 mixture Substances 0.000 claims abstract description 154
- 239000008187 granular material Substances 0.000 claims abstract description 153
- 150000001875 compounds Chemical class 0.000 claims abstract description 96
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- 239000011247 coating layer Substances 0.000 claims abstract description 61
- 238000007789 sealing Methods 0.000 claims abstract description 46
- 150000004760 silicates Chemical class 0.000 claims abstract description 43
- 238000004519 manufacturing process Methods 0.000 claims abstract description 41
- 229910052910 alkali metal silicate Inorganic materials 0.000 claims abstract description 17
- 239000003513 alkali Substances 0.000 claims abstract description 16
- 229910052915 alkaline earth metal silicate Inorganic materials 0.000 claims abstract description 13
- 239000000654 additive Substances 0.000 claims description 107
- 239000000126 substance Substances 0.000 claims description 98
- 230000000996 additive effect Effects 0.000 claims description 73
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 69
- -1 alkaline earth metal cation Chemical class 0.000 claims description 40
- 229920000642 polymer Polymers 0.000 claims description 38
- 230000008569 process Effects 0.000 claims description 37
- 238000003860 storage Methods 0.000 claims description 34
- 229920001223 polyethylene glycol Polymers 0.000 claims description 32
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 29
- 239000000377 silicon dioxide Substances 0.000 claims description 29
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- 229910052751 metal Inorganic materials 0.000 claims description 22
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- 150000001768 cations Chemical class 0.000 claims description 17
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- 229920000468 styrene butadiene styrene block copolymer Polymers 0.000 claims description 12
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- 229920000137 polyphosphoric acid Polymers 0.000 claims description 10
- 235000013311 vegetables Nutrition 0.000 claims description 9
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- 239000004115 Sodium Silicate Substances 0.000 claims description 8
- 230000035515 penetration Effects 0.000 claims description 8
- 239000004576 sand Substances 0.000 claims description 8
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 claims description 8
- 239000002023 wood Chemical group 0.000 claims description 8
- 229920001971 elastomer Polymers 0.000 claims description 7
- 230000002209 hydrophobic effect Effects 0.000 claims description 7
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical class O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 7
- 235000019351 sodium silicates Nutrition 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 229920005610 lignin Polymers 0.000 claims description 6
- 239000012188 paraffin wax Substances 0.000 claims description 6
- 230000001698 pyrogenic effect Effects 0.000 claims description 6
- 241001465754 Metazoa Species 0.000 claims description 5
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- 235000011613 Pinus brutia Nutrition 0.000 claims description 5
- 241000018646 Pinus brutia Species 0.000 claims description 5
- FACXGONDLDSNOE-UHFFFAOYSA-N buta-1,3-diene;styrene Chemical compound C=CC=C.C=CC1=CC=CC=C1.C=CC1=CC=CC=C1 FACXGONDLDSNOE-UHFFFAOYSA-N 0.000 claims description 5
- 239000000454 talc Substances 0.000 claims description 5
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- 229920001817 Agar Polymers 0.000 claims description 4
- 108010010803 Gelatin Proteins 0.000 claims description 4
- 241000206672 Gelidium Species 0.000 claims description 4
- 229920002148 Gellan gum Polymers 0.000 claims description 4
- 229920001732 Lignosulfonate Polymers 0.000 claims description 4
- 239000004117 Lignosulphonate Substances 0.000 claims description 4
- 235000010419 agar Nutrition 0.000 claims description 4
- 235000010443 alginic acid Nutrition 0.000 claims description 4
- 229920000615 alginic acid Polymers 0.000 claims description 4
- 239000001913 cellulose Substances 0.000 claims description 4
- 229920002678 cellulose Polymers 0.000 claims description 4
- 235000010980 cellulose Nutrition 0.000 claims description 4
- 229920000159 gelatin Polymers 0.000 claims description 4
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- 235000019322 gelatine Nutrition 0.000 claims description 4
- 235000011852 gelatine desserts Nutrition 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- 238000004898 kneading Methods 0.000 claims description 4
- 235000019357 lignosulphonate Nutrition 0.000 claims description 4
- 239000005060 rubber Substances 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 239000005995 Aluminium silicate Substances 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 3
- 235000002918 Fraxinus excelsior Nutrition 0.000 claims description 3
- 229920000881 Modified starch Polymers 0.000 claims description 3
- 240000007594 Oryza sativa Species 0.000 claims description 3
- 235000007164 Oryza sativa Nutrition 0.000 claims description 3
- 229920002472 Starch Polymers 0.000 claims description 3
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 3
- 235000012211 aluminium silicate Nutrition 0.000 claims description 3
- 239000002956 ash Substances 0.000 claims description 3
- 239000000440 bentonite Substances 0.000 claims description 3
- 229910000278 bentonite Inorganic materials 0.000 claims description 3
- 235000012216 bentonite Nutrition 0.000 claims description 3
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 3
- 239000000920 calcium hydroxide Substances 0.000 claims description 3
- 235000011116 calcium hydroxide Nutrition 0.000 claims description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 239000004568 cement Chemical group 0.000 claims description 3
- 150000004677 hydrates Chemical class 0.000 claims description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000004571 lime Substances 0.000 claims description 3
- 235000019426 modified starch Nutrition 0.000 claims description 3
- 239000011505 plaster Substances 0.000 claims description 3
- 229920003023 plastic Polymers 0.000 claims description 3
- 239000004033 plastic Substances 0.000 claims description 3
- 235000009566 rice Nutrition 0.000 claims description 3
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 3
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 3
- 229910001948 sodium oxide Inorganic materials 0.000 claims description 3
- 235000019698 starch Nutrition 0.000 claims description 3
- 239000010455 vermiculite Substances 0.000 claims description 3
- 229910052902 vermiculite Inorganic materials 0.000 claims description 3
- 235000019354 vermiculite Nutrition 0.000 claims description 3
- 241000255777 Lepidoptera Species 0.000 claims description 2
- 239000006028 limestone Substances 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims 1
- 229920002593 Polyethylene Glycol 800 Polymers 0.000 claims 1
- 239000003921 oil Substances 0.000 description 48
- 235000019198 oils Nutrition 0.000 description 48
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 38
- 239000011295 pitch Substances 0.000 description 38
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 38
- 125000004432 carbon atom Chemical group C* 0.000 description 34
- 229920001577 copolymer Polymers 0.000 description 33
- KAKZBPTYRLMSJV-UHFFFAOYSA-N vinyl-ethylene Natural products C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 30
- 239000000178 monomer Substances 0.000 description 26
- 239000011343 solid material Substances 0.000 description 25
- LYRFLYHAGKPMFH-UHFFFAOYSA-N octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(N)=O LYRFLYHAGKPMFH-UHFFFAOYSA-N 0.000 description 22
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 21
- 239000005977 Ethylene Substances 0.000 description 21
- 239000011347 resin Substances 0.000 description 21
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- 125000003118 aryl group Chemical group 0.000 description 20
- 229960002920 sorbitol Drugs 0.000 description 20
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 18
- 239000004014 plasticizer Substances 0.000 description 18
- 150000002148 esters Chemical class 0.000 description 17
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 16
- 229910052757 nitrogen Inorganic materials 0.000 description 16
- WLJVNTCWHIRURA-UHFFFAOYSA-N pimelic acid Chemical compound OC(=O)CCCCCC(O)=O WLJVNTCWHIRURA-UHFFFAOYSA-N 0.000 description 16
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 description 15
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 15
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- HSEMFIZWXHQJAE-UHFFFAOYSA-N hexadecanamide Chemical compound CCCCCCCCCCCCCCCC(N)=O HSEMFIZWXHQJAE-UHFFFAOYSA-N 0.000 description 12
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 12
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- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- 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
-
- 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
-
- 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
-
- 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
- E01C7/22—Binder incorporated in hot state, e.g. heated bitumen
Definitions
- the present invention relates to granules of a solid material at room temperature, used as a road binder or as a sealing binder, such as a road bitumen, a pitch, a bitumen / polymer composition, a clear binder.
- the present invention also relates to a process for preparing these granules and their use as a road binder, especially for the manufacture of asphalt.
- the present invention also relates to a process for manufacturing mixes from the granules according to the invention as well as a method for transporting and / or storing and / or handling these granules of bitumen at ambient temperature, especially at ambient temperature. high.
- 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 In general, bitumen is stored and transported hot, in bulk, in tanker trucks or by boats at high temperatures in the range of 120 ° C to 160 ° 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. Otherwise, it can become problematic: if the tanker is not sufficiently insulated, the viscosity of the bitumen may increase during a trip too long. Delivery distances for bitumen are therefore limited.
- the maintenance of bitumen at high temperatures in tanks or tank trucks consumes energy. In addition, 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.
- the application WO 2009/153324 describes bitumen granules coated with a polymeric anti-caking compound, in particular polyethylene.
- the disadvantage of this coating is that it modifies the properties of the bitumen during its road application.
- bitumen granules comprising a chemical additive. These bitumen granules allow the transport and / or storage and / or handling of the bitumen at room temperature without it flowing, as well as reducing their adhesion and agglomeration between them.
- the application WO 2016/198782 describes room temperature solid bitumens in the form of granules comprising a core and a coating layer in which:
- the core comprises at least one bitumen base and, the coating layer comprises at least 10% by weight of one or more viscosifying compounds relative to the total mass of the coating layer, and at least one anti-caking compound.
- the anti-caking agents illustrated in WO 2016/198782 are based on lignin, rubber crumb or styrene-butadiene-styrene copolymer crumb. These granules have satisfactory use properties, however, they have the disadvantage of requiring an additional step after embedding the cores by the coating layer to allow formation of a shell around the cores.
- the Applicant has surprisingly discovered a new composition of granules of solid material at room temperature, used as a road binder or as a sealing binder, such as a road bitumen, a pitch, a bitumen composition polymer, a clear binder, to avoid and reduce adhesion and agglomeration during their transport and / or storage and / or handling, at high ambient temperature, over long periods and whose properties are preserved at course of time compared to the granules of the prior art.
- a road binder or as a sealing binder such as a road bitumen, a pitch, a bitumen composition polymer, a clear binder
- US 2004/0209082 discloses a method of coating granules of a tacky and soft polymeric material with a coating composition of a binder and an anti-caking compound. The coating of these granules prevents their agglomeration during storage.
- the subject of the invention is granules of material which can be used as road binder or as sealing binder comprising a core and a coating layer, in which:
- the core consists of a first composition comprising at least one material chosen from: a bitumen base, a pitch, a clear binder,
- the coating layer consists of a second composition which comprises:
- At least one viscosifying compound At least one viscosifying compound
- At least one first anti-caking agent chosen from alkali metal and / or alkaline earth metal silicates whose silica SiO 2 : oxide molar ratio: metal M x O is from 1.00 to 4.00, M being the metal cation and x being 1 or 2 depending on the nature of the alkali or alkaline earth metal cation, and • at least one second separate anti-caking agent silicates.
- the invention also relates to a method for producing granules of material which can be used as a road binder or as a sealing binder, composed of a core and a core coating layer, this method comprising:
- a second composition comprising at least one viscosifying compound, at least one first anti-caking agent selected from alkali metal and / or alkaline earth silicates whose molar ratio silica Si0 2 : metal oxide MxO is from 1.00 to 4.00, M representing the metal cation and x being equal to 1 or 2 depending on the nature of the alkali or alkaline earth metal cation and at least one second anti-caking agent distinct from silicates.
- the invention also relates to granules of material that can be used as a road binder or as a sealing binder, that can be obtained by implementing this method.
- the silicates are alkali metal silicates, preferably sodium silicates.
- the mass ratio silica SiO 2 : sodium oxide Na 2 0 silicates is from 1.00 to 4.00, preferably from 1.50 to 3.75 and even more preferably from 2.00 at 3.50.
- the silicate comprises silicic units, preferably consists of silicic units.
- the coating layer comprises: 0 from 25% to 50% of one or more viscosifiers
- 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;
- PEG polyethylene glycols
- PEG-800 polyethylene glycols
- PEG-1000 polyethylene glycols
- PEG-1500 a PEG having a molecular weight of 4000 g. mol-1 (PEG-4000) or PEG having a molecular weight of 6000 gmol-1 (PEG-6000)
- PEG-6000 polyethylene glycols
- the second anti-caking agent is chosen from: talc; fines, also known as "butterflies", generally of diameter less than 125 ⁇ m, such as siliceous fines, with the exception of fine limestones; sand such as fountain sand; cement ; carbon; wood residues such as lignin, lignosulphonate, conifer needle powders, conifer cone powders, especially pine powders; the ashes of rice balls; glass powder; clays such as kaolin, bentonite, vermiculite; alumina such as alumina hydrates; silica; silica derivatives such as silica fumes, functionalized silica fumes, in particular hydrophobic or hydrophilic silica fumes, pyrogenic silicas, especially hydrophobic or hydrophilic pyrogenic silicas, silicon hydroxides and silicon oxides; plastic powder; lime; hydrated lime; the plaster ; rubber crumb; polymer powder, such as styrene-but
- the second anti-caking agent is chosen from fines, preferably from fines with a diameter of less than 125 ⁇ , with the exception of fine limestones.
- the first composition has a needle penetration measured at 25 ° C according to the EN 1426 standard of 5 to 330 1/10 mm, preferably 10 to 220 1/10 mm.
- the first composition further comprises at least one chemical additive chosen from: an organic compound, a paraffin, a polyphosphoric acid, a dope of adhesiveness, and mixtures thereof.
- the granules of material that can be used as a road binder or as a sealing binder exhibit stability during transport and / or storage and / or handling at a temperature of up to 100.degree. 20 ° C to 90 ° C, preferably 20 ° C to 80 ° C, more preferably 40 ° C to 80 ° C, still more preferably 40 ° C to 60 ° C, for a duration greater than or equal to 2 month, preferably greater than or equal to 3 months.
- the second composition is applied to the core of the granules in a fluidized air bed device.
- the invention also relates to the use of the granules defined above as road binder.
- the use relates to the manufacture of asphalt.
- the invention also relates to a process for the manufacture of mixes comprising at least one road binder and aggregates, the road binder being chosen from the granules defined above, this process comprising at least the steps of:
- a tank such as a kneader or a kneading drum
- the asphalt manufacturing process does not include a heating step of the road binder before mixing with the aggregates.
- the invention finally relates to a method for transporting and / or storing and / or handling material that can be used as a road binder or as a sealing binder, material being transported and / or stored and / or handled in the form of granules as defined above.
- compositions of material that can be used as a road binder or as a sealing binder in a divided form, having a core / shell structure, in which the core is based on a first composition and the coating layer gives the overall structure improved properties under extreme conditions of transport and / or storage and / or handling with respect to the granules of material that can be used as a road binder or as a binder. sealing known from the prior art.
- a first subject of the invention relates to granules of material that can be used as a road binder or as a sealing binder comprising a core and a coating layer in which:
- the core consists of a first composition which comprises at least one material chosen from: a bitumen base, a pitch, a clear binder,
- the coating layer consists of a second composition which comprises:
- At least one viscosifying compound At least one viscosifying compound
- At least one first anti-caking agent chosen from alkali metal and / or alkaline earth metal silicates whose molar ratio of silica SiO 2 : metal oxide M ⁇ O is from 1.00 to 4.00, M representing the metal cation and x being 1 or 2 depending on the nature of the alkali or alkaline earth metal cation, and
- High ambient temperature means the temperature resulting from the climatic conditions in which the material used as a road binder or as a sealing binder, in particular road bitumen, is transported and / or stored and / or handled. Specifically, the high ambient temperature is equivalent to the temperature reached during transport and / or storage of the material used as road binder or as a sealing binder, particularly road bitumen, this temperature being less than 100 ° C.
- 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, it being understood that the high ambient temperature implies that no heat input is provided other than that resulting from the climatic conditions.
- the invention relates to materials which can be used as road binder or as sealing binder, in particular bitumens which can be solid when subjected to high ambient temperatures, in particular up to 100 ° C, advantageously 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.
- material usable as a road binder or as a sealing binder is meant in the sense of the present invention any material capable of being used for this purpose, and in particular: bitumen bases, bitumen / polymer compositions, compositions additive bitumen, pitches, bitumen-polymer stock solutions, clear binders, light-polymer bonding stock solutions, mixtures of these materials in all proportions.
- solid material at high ambient temperature is meant a material having a solid appearance at high ambient temperature under conditions of transport and / or storage and / or handling. More specifically, solid material at high ambient temperature is understood to mean a material which retains its solid appearance throughout the transport and / or storage and / or handling at high ambient temperature, that is to say a material which does not flow at a temperature up to 100 ° C, preferably from 20 ° C to 90 ° C, preferably from 20 ° C to 80 ° C, more preferably from 40 ° C to 80 ° C, even more preferably from 40 ° C to 60 ° C, under its own weight and additionally, which does not flow when subjected to a temperature up to 100 ° C, preferably 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, and to pressure forces from transport and / or storage conditions and / or manipulation.
- 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 which retains its solid appearance throughout transport and / or storage at ambient temperature, that is to say a bitumen which does not flow at ambient temperature under its own weight and more, which does not flow when subjected to pressure forces from transport conditions and / or storage.
- Coating layer covering all part of the surface of the core means that the coating layer covers at least 90% of the surface of the core, preferably at least 95% of the surface of the core, more preferably at least 99% of the surface of the heart.
- the expression "between X and Y" includes the terminals. This expression therefore means that the target range includes X, Y values and all values from X to Y.
- composition according to the invention makes it possible to obtain granules of solid material that can be used as a road binder or as a sealing binder, especially bitumen, comprising a coating layer that is resistant to the climatic conditions and to the conditions of transport and / or storage of road binders and / or sealing binders, in particular which is resistant to climatic conditions and conditions of transport and / or storage of solid road asphalt, which breaks easily under a mechanical shear effect, such as for example under the effect of mechanical shear applied in a tank such as a kneader or kneading drum during the manufacture of asphalt.
- the coating layer is resistant to the transport and / or storage of road binders and / or sealing binders, in particular bitumen, at room temperature in "Big Bags" while being brittle under the effect of mechanical shearing. It thus allows the liberation of the bitumen core during the manufacture of asphalt.
- the cores of the granules of material that can be used as a road binder or as a sealing binder are prepared from a first bitumen composition comprising one or more bitumen bases.
- bitumen granules are prepared from a first bitumen composition comprising:
- bitumen bases one or more bitumen bases
- bitumen base and the chemical additive are as described below.
- bitumen granules are prepared from a first bitumen composition comprising:
- bitumen bases one or more bitumen bases
- the cores of the granules are prepared from a first composition comprising:
- bitumen base preferably between 0.1% and 10% by weight, more preferably between 0.5% and 6% by weight of at least one olefinic polymer adjuvant, the percentages being in mass relative to the total mass of bitumen base.
- the cores of the granules are prepared from a first composition comprising:
- the cores of the granules of material that can be used as a road binder or as a sealing binder are prepared from a first composition comprising at least one pitch.
- the cores of the granules consist of a first composition based on pitch.
- the cores of the granules consist of a first composition based on pitch and at least one bitumen base.
- the first composition comprises at least one pitch having a penetrability at 25 ° C. ranging from 0 to 20 1/10 mm, a ball and ring softening temperature (TBA) ranging from 115 ° C. to 175 ° C. ° C, provided that penetrability is measured according to EN 1426 and that TBA is measured according to EN 1427.
- the first composition comprises:
- the granules of material that can be used as road binder or as sealing binder are prepared from a first composition comprising at least one clear binder.
- Colored coatings are increasingly used because they allow, among other things, to improve the safety of road users by clearly identifying specific routes such as pedestrian routes, bike paths, bus lanes. They also make it possible to materialize certain danger zones such as entrances to agglomeration or dangerous turns. Colored coatings promote visibility in low light conditions, for example at night or in particular sites such as tunnels. Finally, they simply improve the aesthetic appearance of urban roads and can be used for public squares, courtyards and schools, sidewalks, pedestrian streets, garden and park paths. , parking and rest areas.
- the first composition comprises at least one clear binder.
- the first composition comprises at least one clear binder base and at least one chemical additive chosen from an organic compound, a paraffin, a polyphosphoric acid and their mixtures.
- the first composition comprises from 0.1% to 5% by weight, preferably from 0.5% to 4% by weight, more preferably from 0.5% to 2.5% by weight. % by weight of said chemical additive relative to the total mass of said additivated clear binder.
- the first composition comprises
- the first composition is called clear concentrated binder.
- the granules are prepared from a first composition comprising:
- the term "cold solid binder” and "split form” means a clear solid binder at room temperature which is packaged in a divided form, that is to say in the form of units which are distinct from one another and which are name granules.
- the clear binder according to the invention is referred to indifferently in the present description as "clear solid binder in cold form and in divided form” or as “clear additivated binder”.
- the clear binder is a composition that can be used as a substitute for bitumen-based binders for the preparation, for example, of colored bituminous mix.
- a clear binder is free of asphaltenes and can therefore keep the natural color of the granulate to which it is mixed or be easily colored with pigments.
- the core or core of the solid bitumen granules according to the invention is prepared from a first composition, which is a road bitumen composition, said first composition being prepared by bringing into contact:
- bitumen bases one or more bitumen bases
- 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 and optionally comprising one or more chemical additives, 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.
- the 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.
- 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.
- 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 bitumen bases may be bitumen bases of hard grade or soft grade.
- production temperatures of between 100 ° C. and 200 ° C., preferably between 140 ° C. and 200 ° C., more preferably between 140 ° C. and 170 ° C, and stirring for a period of at least 10 minutes, preferably between 30 minutes and 10 hours, more preferably between 1 hour and 6 hours.
- manufactured temperature means the heating temperature of the bitumen base (s) before mixing as well as the temperature of the mixed. The temperature and the duration of the heating vary according to the quantity of bitumen used and are defined by the standard NF EN 12594.
- 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 bitumen base used to manufacture the granules of the invention has a needle penetration measured at 25 ° C according to the EN 1426 standard of 5 to 330 1/10 mm, preferably 20 to 220 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 of bitumen, after a time of 5 seconds, of a needle whose weight with its support is 100 g.
- the NF EN 1426 standard replaces the homologated NF T 66-004 standard of December 1986 with effect from December 20, 1999 (decision of the Chief Executive Officer of AFNOR dated November 20, 1999).
- clear binder base compositions comprising a plasticizer, for example an oil of petroleum or plant origin, a structuring agent, for example a hydrocarbon resin, and a polymer.
- a plasticizer for example an oil of petroleum or plant origin
- a structuring agent for example a hydrocarbon resin
- the composition of the clear binder bases determines certain essential properties of these binders, in particular the plasticity index, the viscosity of the binder, or the color which must be as clear as possible.
- the clear binder base comprises:
- plasticizing agent for example a natural or synthetic oil, free of asphaltenes
- a structuring agent for example a hydrocarbon or vegetable resin
- Clear binder compositions are described in the following applications and patents and these clear binder compositions can be used as a clear binder base in the present invention.
- a clear binder comprising hydrogenated white oils comprising at least 60% paraffmic carbons (according to the ASTM D2140 method) and a hydrocarbon resin, optionally mixed with ethylene-acetate copolymers, may be used as clear binder base.
- a clear binder comprising an oil with a naphthenic content between 35% and 80% and a hydrocarbon resin as described in EP 1783174 can be used as clear binder base.
- a clear binder base a clear binder comprising a synthetic oil, a resin and an SBS or SIS type polymer can be used, as described in EP 1473327.
- a clear binder base a clear binder may be used comprising:
- At least one oil of petroleum origin preferably an aromatic oil comprising aromatic extracts of petroleum residues, obtained by extraction or dearomatization of residues of distillations of petroleum fractions,
- At least one resin of plant origin preferably chosen from rosin esters, esters of glycerol and rosins, esters of pentaerythritol and rosins, taken alone or as a mixture, and
- a clear binder base a clear synthetic binder can be used comprising:
- At least one oil of vegetable origin preferably chosen from rapeseed, sunflower, soya, flax, olive, palm, castor oil, wood, corn, squash, grape seed oil , jojoba, sesame, walnut, hazelnut, almond, shea, macadamia, cotton, alfalfa, rye, safflower, peanut, coconut and copra, and mixtures thereof
- at least one resin of petroleum origin preferably chosen from resins of petroleum hydrocarbon origin resulting from the copolymerization of aromatic, aliphatic, cyclopentadienic petroleum fractions taken alone or as a mixture and
- At least one polymer preferably chosen from styrene and butadiene copolymers, styrene and isoprene copolymers, ethylene / propene / diene terpolymers, polychloroprenes, copolymers of ethylene and vinyl acetate, copolymers of ethylene and methyl acrylate, copolymers of ethylene and butyl acrylate, ethylene / methyl acrylate / glycidyl methacrylate terpolymers, ethylene / butyl acrylate / maleic anhydride terpolymers, atactic polypropylenes , taken alone or in mixtures,
- the clear binder base comprises:
- a plasticizer consisting of an oil containing a total content of paraffmic compounds, measured according to ASTM D2140 method, of at least 50%, preferably at least 60% by weight, more preferably between 50%> and 90%>, preferably between 60% and 80%, and
- the oil is a synthetic oil derived from deasphalting unit cuts (or "DAO oil").
- DAO oil synthetic oil derived from deasphalting unit cuts
- the oil contains a total content of paraffmic compounds greater than or equal to 50%, preferably greater than or equal to 60% by weight, and a total naphthenic compounds content of less than or equal to 25% by weight, measured. according to ASTM Method D2140.
- the oil contains a total content of paraffmic compounds greater than or equal to 50%, preferably greater than or equal to 60% by weight, a total naphthenic compounds content of less than or equal to 25% by weight, and total content of aromatic compounds of less than or equal to 25% by weight, measured according to the ASTM D2140 method.
- the oil contains a total content of paraffmic compounds, measured according to the ASTM D2140 method, of between 50% and 90%, preferably between 60% and 80% by weight, and a total naphthenic compounds content of between 5% and 5%. and 25% by weight, and a total content of aromatic compounds of between 5% and 25% by weight.
- the oil has an aniline point, measured according to the standard IS02977: 1997, greater than or equal to 80 ° C, preferably greater than or equal to 90 ° C, for example greater than 100 ° C.
- the clear binder base preferably comprises (i) from 40 to 80% by weight of plasticizer, (ii) from 18 to 50% by weight of resin, (iii) from 1 to 7% by weight of copolymer; and, (iv) optionally from 0.05% to 0.5% by weight of tackifier, for example amine, based on the basis weight of clear binder.
- the clear binder base preferably comprises (i) from 40 to 80% by weight of plasticizer, (ii) from 18 to 50% by weight of resin, (iii) from 1 to 7% by weight of copolymer ; and, (iv) from 0.05% to 0.5% by weight of tackifier, for example amine, based on the weight of clear binder base.
- the clear binder base also comprises (i) from 45% to 70% by weight of plasticizer, (ii) from 25 to 50% by weight of resin, (iii) from 1% to 7% by weight of copolymer; and, (iv) optionally 0.1% and 0.3% by weight of tackifier, based on the total weight of clear binder base.
- the clear binder base consists essentially of (i) from 40 to 80% by weight of plasticizer, (ii) from 20 to 50% by weight of resin, (iii) from 1 to 7% by weight of copolymer, based on the total weight of clear binder base.
- the clear binder base consists essentially of (i) from 40 to 80% by weight of plasticizer, (ii) from 20 to 50% by weight of resin, (iii) from 1 to 7% by weight of copolymer and (iv) from 0.05% to 0.5% by weight of tackifier, based on the total weight of clear binder base.
- the clear binder base essentially also consists of (i) from 45% to 70% by weight of plasticizer, (ii) from 25% to 50% by weight of resin (iii) from 1% to 7% by weight. weight copolymer; and, (iv) 0.1% and 0.3% by weight of tackifier, based on the total weight of clear binder base.
- the copolymer is a copolymer based on styrene and butadiene units which comprises a weight content of butadiene 1-2 ranging from 5 to 70%.
- the copolymer is advantageously a copolymer based on styrene and butadiene units which comprises a weight content of butadiene 1-2 ranging from 5 to 70% and a weight content of 1,2-vinyl group of between 10 and 40%.
- said copolymer based on styrene and butadiene units has a weight average molecular weight of between 10,000 and 500,000, preferably between 50,000 and 200,000, and more preferably between 50,000 and 150,000 daltons.
- a styrene / butadiene block copolymer or styrene / butadiene / styrene block copolymer will be used.
- the clear binders according to the invention are advantageously characterized in that they have a color index of less than or equal to 4, preferably less than or equal to 3, as determined according to the ASTM DH4 scale. In addition, they can advantageously have a softening temperature
- Ball-Ring temperature determined according to standard NF EN1427 between 55 ° C and 90 ° C.
- the clear binder used according to the invention has a penetrability at 25 ° C., measured according to standard NF EN 1426, of between 10 and 220 1/10 mm, preferably between 30 and 100 1/10 mm, more preferably between 40 and 80 1/10 mm.
- Those skilled in the art can modulate the penetrability of the clear binder used in the invention, in particular by judiciously choosing the weight ratio [structuring agent / plasticizer] in the composition of the clear binder base. Indeed, it is known that an increase in this ratio makes it possible to reduce the penetrability at 25 ° C.
- the clear binder bases used in the invention may be prepared for example according to the following process comprising the steps of:
- steps (i) to (iv) can be changed.
- the cores of the light binder granules further comprise at least one coloring agent as described above, such as for example a pigment.
- the anti-caking agent and / or the coloring agent will be selected by those skilled in the art depending on the color of the desired clear binder.
- pitch is a residue from the distillation of petroleum tars, oil, coal, wood or other organic molecules.
- the invention relates here to the residues of petroleum distillation, also known as "petroleum pitch”.
- pitch For the purposes of the invention, the terms “pitch”, “petroleum pitch” and “deasphalting pitch” will be used independently of one another.
- 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 production of a gaseous phase, various distillates and an atmospheric distillate residue.
- the residue of the atmospheric distillation is subjected itself to a distillation under reduced pressure, called vacuum distillation, which makes it possible to separate a heavy gas oil, various distillais cuts and a residue of vacuum distillation.
- This vacuum distillation residue contains "petroleum pitch" in varying concentration.
- the vacuum distillation residue is subjected to a desalting operation by adding a suitable solvent, such as propane, which thus makes it possible to precipitate the pitch and to separate it from light fractions such as the unphased oil.
- a suitable solvent such as propane
- the vacuum distillation residue is subjected to a solvent extraction, and more precisely to furfural.
- This heterocyclic aldehyde has the particularity of selectively solubilizing aromatic and polycyclic compounds. This process thus makes it possible to eliminate the aromatic extracts and to recover the "oil pitch".
- the pitch is an oxidized pitch.
- the oxidized pitch according to the invention is obtained by oxidation of a mixture comprising pitch and a diluent, such as a light gasoline, also called “fluxing" subjected to an oxidation operation in a blowing tower. presence of a catalyst, at a fixed temperature and at a given pressure.
- a diluent such as a light gasoline
- oxidized pitches may be manufactured in a blowing unit, passing a stream of air and / or oxygen through a starting pitch.
- This operation can be carried out in the presence of an oxidation catalyst, for example phosphoric acid.
- the oxidation 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 oxidation temperature are adjusted according to the properties targeted for the oxidized pitch and according to the quality of the starting pitch.
- the mechanical properties of 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.
- the pitch exhibits needle penetration at 25 ° C. of 0 to 1/10 mm, preferably 0 to 1/10 mm, more preferably 0 to 10 1. / 10 mm, it being understood that the penetrability is measured according to the standard EN 1426.
- the pitch has a softening point of between 115 ° C. and 175 ° C.
- pitches used in the invention there are pitches respectively having a softening point between 115 ° C and 125 ° C, between 135 and 145 ° C or between 165 and 175 ° C.
- plasticizing agent is intended to mean a chemical constituent that makes it possible to thin and reduce the viscosity and the modulus of the binder obtained.
- the plasticizing agent is chosen from oils of petroleum origin, oils of vegetable origin and their mixtures.
- the oils of plant origin are chosen from rapeseed, sunflower, soybean, flax, olive, palm, castor oil, wood, corn, squash, grape seed, jojoba, sesame, walnut, hazelnut, almond, shea, macadamia, cotton, alfalfa, rye, safflower, peanut, coconut and copra, and their mixtures.
- oils of vegetable origin are chosen from rapeseed, sunflower, linseed, coconut and soybean oils, and mixtures thereof.
- oils of petroleum origin are chosen from aromatic oils or oils of synthetic origin.
- the aromatic oils comprise aromatic extracts of petroleum residues, obtained by extraction or dearomatization of residues of distillations of petroleum fractions.
- the aromatic oils have an aromatic compound content of between 30 and 95% by weight, advantageously between 50 and 90% by weight, more advantageously between 60 and 85% by weight (SARA method: Saturated / Aromatic / Resins / Asphaltenes).
- the aromatic oils have a content of saturated compounds of between 1 and 20% by weight, advantageously between 3 and 15% by weight, more advantageously between 5 and 10% by weight (SARA method: Saturated / Aromatic / Resins / Asphaltenes).
- the aromatic oils have a content of resin compounds of between 1 and 10% by weight, advantageously between 3 and 5% by weight, (SARA method: Saturated / Aromatic / Resins / Asphaltenes).
- SARA method Saturated / Aromatic / Resins / Asphaltenes
- the oils of synthetic origin come from distillation deasphalting cuts under reduced pressure (vacuum residue, RSV) of crude oil (hereinafter referred to as "DAO oil").
- the plasticizer consists solely of a DAO oil.
- the contents of paraffinic, naphthenic and aromatic compounds mentioned in the present application are determined according to the ASTM D2140 standard, in% by weight relative to the weight of the oil.
- the plasticizer is an oil, for example a DAO oil, containing a total content of paraffinic compounds of at least 50% by weight, preferably at least 60% by weight, by weight. example between 50%> and 90%>, preferably between 60% and 90%, more preferably between 50% and 80% and in particular between 55% and 70%) or in particular between 60%> and 75% .
- the plasticizer is an oil, for example a DAO oil, also containing a total content of naphthenic compounds which does not exceed 25% o, for example between 5% and 25%, and in particular between 10% and 25%.
- the plasticizer is an oil, for example a DAO oil, further containing a total aromatic content of not more than 25%, for example between 5% and 25%, and between 8% and 18%.
- the plasticizer is an oil, for example a DAO oil, comprising the respective contents:
- the plasticizing agent is an oil, for example a DAO oil, comprising the respective contents:
- Oils meeting the above characteristics and usable for the preparation of the clear binder according to the invention are obtained by vacuum residue deasphalting processes (RSV) from petroleum refining, for example by deasphalting with the aid of a C 3 to C 6 solvent, preferably propane.
- RSV vacuum residue deasphalting processes
- C 3 to C 6 solvent for example propane
- DAO oil deasphalted oil
- paraffin has a very low asphaltene content
- evaporation temperature of between 440 ° C. and 750 ° C.
- API gravity much higher than that vacuum residues.
- paraffinic, naphthenic and aromatic compounds depend to some extent on the nature of the crude oil at the origin of the DAO oil and the refining process used.
- Those skilled in the art know how to determine the respective contents of paraffinic, naphthenic and aromatic compounds of a DAO oil, for example using the SARA fractionation method also described in Lee et al 2014, Fuel Processing. Technology 119: 204-210 and thus select the appropriate DAO oil for the preparation of the clear binder according to the invention.
- the amount of plasticizer used in the process for preparing the clear binder base is 40% to 80%, preferably 45% to 70% by weight based on the total weight of clear binder base.
- the structuring agent The structuring agent
- structural agent any chemical component imparting mechanical properties and satisfactory cohesiveness to said binder.
- the structuring agent used in the context of the invention is a resin, preferably chosen from resins of petroleum hydrocarbon origin, for example derived from the copolymerization of aromatic, aliphatic, cyclopentadienic petroleum fractions, taken alone or as a mixture, preferably from aromatic petroleum cuts.
- resins of petroleum hydrocarbon origin for example derived from the copolymerization of aromatic, aliphatic, cyclopentadienic petroleum fractions, taken alone or as a mixture, preferably from aromatic petroleum cuts.
- it may be a polycycloaliphatic thermoplastic resin, for example of the low molecular weight hydrogenated cyclopentadiene homopolymer type.
- the hydrocarbon resin of the cyclopentane type has a softening point (or ball-ring temperature, TBA, according to standard NF T 66-008) greater than 125 ° C., and a Gardner color index (according to the NF standard). T 20-030) equal to the maximum of 1.
- resins that can be used as structuring agents include, but are not limited to, resins of vegetable origin obtained from plants and / or plants. They can be called harvest, that is to say harvested from the living plant. They can be used as they are, we speak then of natural resins or be transformed chemically, one speaks then of modified natural resins.
- the enhanced resins there are the enhanced resins, dammar, natural rosins, modified rosins, rosin esters and metal resinates. These can be taken alone or mixed.
- Natural rosins include gem and wood rosin, especially pine, and / or tall oil or tall oil. These natural rosins can be taken alone or as a mixture.
- Modified rosins include hydrogenated rosins, disproportionated rosins, polymerized rosins and / or maleic rosins. These rosins modified natural forms can be taken alone or in mixture, and undergo one or more disproportionation, polymerization and / or maleization treatments.
- rosin esters mention may be made of the natural rosin methyl esters, the hydrogenated rosin methyl esters, the natural glycerol and rosin esters, the hydrogenated glycerol and rosin esters and the disubstituted glycerol and rosin esters, esters of glycerol and of polymerized rosins, esters of glycerol and of maleated rosin, esters of pentaerythritol and natural rosins and esters of pentaerythritol and hydrogenated rosins.
- These rosin esters can be taken alone or in mixture and come from rosins having undergone one or more disproportionation, polymerization and / or maleization treatments.
- Esters of pentaerythritol and natural rosins and esters of pentaerythritol and hydrogenated rosins are the preferred rosin esters.
- metal resinates there may be mentioned metal carboxylates, for example of Ca, Zn, Mg, Ba, Pb, Co, obtained from natural rosins or modified rosins.
- metal carboxylates for example of Ca, Zn, Mg, Ba, Pb, Co, obtained from natural rosins or modified rosins.
- the weight ratio between the structuring agent and the plasticizer used for the preparation of the clear binder is generally from 0.3 to 1.5, for example from 0.5 to 1.
- the amount of structuring agent used in the process for preparing the clear binder base is 25 to 50% by weight relative to the total weight of clear binder base.
- the polymer used in the first composition is a copolymer based on conjugated diene units and monovinyl aromatic hydrocarbon units.
- the conjugated diene is preferably chosen from those comprising from 4 to 8 carbon atoms per monomer, for example butadiene, 2-methyl-1,3-butadiene (isoprene), 2,3-dimethyl-1,3- butadiene, 1,3-pentadiene and 1,2-hexadiene, chloroprene, carboxylated butadiene, carboxylated isoprene, especially butadiene and isoprene, and mixtures thereof.
- the monovinyl aromatic hydrocarbon is preferably selected from styrene, o-methyl styrene, p-methyl styrene, p-tert-butylstyrene, 2,3-dimethylstyrene, vinyl naphthalene, vinyl toluene, vinyl xylene, and the like or mixtures thereof, in particular styrene.
- the polymer consists of one or more copolymers chosen from block copolymers of styrene and butadiene, styrene and isoprene, styrene and chloroprene, styrene and carboxylated butadiene or else styrene and isoprene. carboxyl.
- a preferred copolymer is a copolymer based on butadiene units and styrene units such as SB styrene / butadiene block copolymer or SB SB styrene / butadiene / styrene block copolymer.
- the styrene-conjugated diene copolymer in particular the styrene-butadiene copolymer, advantageously has a weight content of styrene ranging from 5 to 50%, preferably from 20 to 50%.
- the copolymer of styrene and conjugated diene, in particular the styrene-butadiene copolymer advantageously has a weight content of butadiene (1-2 and 1-4) ranging from 50 to 95%.
- the copolymer of styrene and conjugated diene in particular the styrene-butadiene copolymer, advantageously has a weight content of butadiene 1-2 ranging from 5 to 70%, preferably from 5 to 50%.
- the butadiene units 1-2 are the units which result from the polymerization via the 1-2 addition of the butadiene units.
- the weight average molecular weight of the copolymer of styrene and of conjugated diene, and in particular that of the styrene-butadiene copolymer may be, for example, between 10,000 and 500,000, preferably between 50,000 and 200,000 and more. preferably from 50,000 to 150,000 daltons.
- the total amount of polymer used in the process of the invention is from 0.5 to 20% by weight, preferably from 1 to 10%, preferably from 1 to 7% by weight. o, for example from 2% to 5% relative to the total weight of bitumen base, or clear binder.
- the total quantity of polymer used in the process of the invention is 20% to 50% by weight, relative to the total weight of bitumen base, or with respect to total mass of clear binder base.
- the first composition is said mother solution of bitumen / polymer composition or parent solution of clear binder / polymer composition. It is intended to be transported and stored in concentrated form, then diluted with the appropriate amount of bitumen base or clear binder base just prior to its use as a road binder or as a binder. coating. According to the invention, it is possible to form granules of mother liquor of bitumen or clear binder, so as to facilitate their transport and storage as well as their handling at high ambient temperature.
- the polymer is chosen from micronized polymers.
- the polymer has particles of diameter ranging from 250 to 1000 ⁇ , preferably with a diameter ranging from 400 to 600 ⁇ .
- the compatibilizing agent is chosen from waxes, for example animal waxes, vegetable waxes, mineral waxes and their mixtures.
- Animal and vegetable waxes are mainly composed of mixtures of fatty acid derivatives (fatty acid esters) while mineral waxes are paraffinic derivatives.
- adhesiveness dopes may also be used in the first composition, mixed with the other components, in particular the clear binder, or the bitumen base or the pitch.
- these are, for example, nitrogen-containing surfactant compounds derived from fatty acids (amines, polyamines, alkylpolymers, etc.).
- the adhesiveness dopes When added to the first composition, the adhesiveness dopes generally represent between 0.05% and 0.5% by weight relative to the weight of light binder or bitumen base or pitch. For example, in a specific embodiment, from about 0.05% to about 0.5% amine, preferably from about 0.1% to about 0.3% amine, will be added to the mass. total base of clear binder or base bitumen or pitch.
- the clear synthetic binder may also include one or more coloring agents, such as inorganic pigments or organic dyes.
- the pigments are selected according to the color, the desired color for the coating. For example, metal oxides such as iron oxides, chromium oxides, cobalt oxides, titanium oxides will be used to obtain the colors red, yellow, gray, blue green or white.
- the pigments can be added, either in the clear binder or in the mix (mixed with the aggregates for example) or in an emulsion of the clear binder.
- the chemical additive can be added, either in the clear binder or in the mix (mixed with the aggregates for example) or in an emulsion of the clear binder.
- the bitumen base, the pitch or the light binder may further comprise at least one chemical additive selected from: an organic compound, a paraffin, a polyphosphoric acid and mixtures thereof.
- the solid material comprises at least one chemical additive
- it is in an amount adapted so that its penetrability is preferably from 5 to 50 1/10 mm and / or the ball and ring softening temperature (TBA) is preferably greater than or equal to 60 ° C, it being understood that the penetrability is measured at 25 ° C according to EN 1426 and the TBA according to EN 1427.
- TSA ball and ring softening temperature
- 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 -R-Ar 2 (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-tert-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, represent a saturated or unsaturated, linear, branched or cyclic hydrocarbon-based chain comprising from 1 to 22 carbon atoms, and optionally comprising heteroatoms such as N, O, S, C5-C24 hydrocarbon rings and / or C4-C24 hydrocarbon heterocycles comprising one or more heteroatoms such as N, O, S, and R "may be H;
- the group X represents a hydrocarbon chain, saturated or unsaturated, linear, cyclic or branched, comprising from 1 to 22 carbon atoms, optionally substituted, and optionally comprising heteroatoms, such as N, O, S, C5 hydrocarbon-based rings; -C24 and / or C4-C24 hydrocarbon heterocycles comprising one or more heteroatoms such as N, O, S;
- n, m and p 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 linked so that 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, a aliphatic condensed polycyclic system, partially aromatic or wholly aromatic, each ring comprising 5 or 6 atoms.
- 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 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 chosen from the groups C 4 H 9, C 5 H 11, C 9 H 19, C 11 H 23, C 12 H 25, C 17 H 35, C 18 H 37, C 21 H 43, C 22 H 45.
- the group X represents a saturated, linear hydrocarbon-based chain comprising from 1 to 22 carbon atoms, advantageously X represents a linear, saturated hydrocarbon-based chain comprising from 1 to 12 carbon atoms, more preferably from 1 to 4 carbon atoms.
- the group X is chosen from C2H4 groups,
- the group X can also be a cyclohexyl group or a phenyl group, the radicals R- (NH) n CONH- and NHCO (NH) n -R'- can then be in 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 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-C 11 H 23, CIVHBS-CONH-NHCO-CIVHBS, or
- diamides such as N, N'-ethylenedi (laurylamide) of formula C n H 2 3 CONH-CH 2 -CH 2 -NHCO-C 11 H 31 , N, N-ethylenedi (myristylamide) of formula C 13 H 27 -CONH-CH 2 -CH 2 -NHCO-C 13 H 27 , N, N'-ethylenedi (palmitamide) of formula Ci 5 H 3 i-CONH-CH 2 -CH 2 -NHCO-C 15 H 31 , N N, N-ethylenedi (stearamide) of the formula CONH-C11-C10-NHCO-C13;
- the compound of general formula (II) is chosen from those which satisfy the condition: the sum of the numbers of the carbon atoms of R ', X and R "is greater than or equal to 10, advantageously greater than or equal to 14 preferably greater than or equal to 18.
- the compound of general formula (II) is chosen from those which satisfy the condition: the number of carbon atoms of at least one of R 'and R "is greater than or equal to 10, advantageously greater than or equal to at 12, preferably greater than or equal to 14.
- the compound of general formula (II) is chosen from those of formula (IIA):
- R ', R ", m and X have the same definition as above.
- the group X represents a saturated linear hydrocarbon-based chain containing from 1 to 22 carbon atoms, advantageously X represents a linear hydrocarbon-based saturated chain comprising from 1 to 12 carbon atoms more preferably from 1 to 4 carbon atoms.
- the group X is chosen from C 2 H 4 and C 3 H 6 groups.
- the compound of general formula (IIA) is chosen from those which satisfy the condition: the sum of the numbers of the carbon atoms of R ', X and R "is greater than or equal to 10, advantageously greater than or equal to 14 preferably greater than or equal to 18.
- the compound of general formula (IIA) is chosen from those which satisfy the condition: the number of carbon atoms of at least one of R 'and R "is greater than or equal to 10, advantageously greater or equal to 12, preferably greater than or equal to 14.
- the compound of general formula (IIA) is chosen from hydrazide derivatives such as compounds C5H11-CONH-NHCO-C5H11, C9H19-CONH-NHCO-C9H19, C11H23-CONH-NHCO-C11H23, CIVHBS -CONH-NHCO-CIVHBS, or C 2 H 4 3-CONH-NHCO-C 2 H 4 3; diamines such as N, N'-ethylenedi (laurylamide) of the formula C 11 H 23 -CO-CH 2 -CH 2 -NHCO-C 11 H 31, N, N -ethylenedi (myristylamide) of the formula C 13 H 27 CONH-CH 2 -CH 2 -NHCO- C13H27, N, N * -éthylènedi (palmitamide) of the formula Ci H3I 5-CONH-CH 2 CH 2 -NHCO-Ci 5 H3I, N, N * -éth
- the compound of general formula (IIA) is ⁇ , ⁇ '-ethylenedi (stearamide) of formula Ci 7 H 35 -CONH-CH 2 -CH 2 -NHCO-C 7 H 35 .
- the compound of general formula (II) is chosen from those of formula (IIB):
- R 'and R have the same definition as above.
- the sum of the numbers of the carbon atoms of R 'and R " is greater than or equal to 10, advantageously greater than or equal to 14, preferably greater than or equal to 18.
- the compound of general formula (II) is chosen from hydrazide derivatives such as compounds C 5 H "-CONH-NHCO-C 5 H 1, C 9 H 19 -C CONH-NHCO-C 9 H 19, C 11 H 23 CONH-NHCO-C 11 H 23, CIVHBS-CONH-NHCO-CIVHBS, or C21H43-CONH-NHCO-C21H43; diamides such as N, N'-ethylenedi (laurylamide) of formula C 1 1 H 23 -CONH-CH 2 -CH 2 -NHCO-C 1 1 H 31 , N, N * -ethylenedi (myristylamide) of formula C 13 H 27 -CONH-CH 2 -CH 2 -NHCO-C 13 H 27 , N, N'-ethylenedi (palmitamide) of formula C 5 H 3 i-CONH-CH 2 -CH 2 -NHCO-C 5 H 3 i, N, N '-ethylenedi (stearamide)
- the compound of general formula (II) is ⁇ , ⁇ '-ethylenedi (stearamide) of formula C 7 H 35 -CONH-CH 2 -CH 2 -NHCO-C 17 H 35 .
- the chemical additive when the chemical additive is chosen from the organic compounds of formula (II), it is used in combination with at least one other chemical additive chosen from the organic compounds of formula (I), (III), (V) , (VI) and (VII) and / or the reaction products of at least one C 3 -C 12 polyol and at least one C 2 -C 12 aldehyde, in particular those comprising a group of formula (IV ).
- 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 :
- R selected from the following groups, taken alone or in mixtures
- the organic compound is a reaction product of at least one polyol C3-C 12 and at least one aldehyde C 2 -C 12.
- 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):
- R is chosen from an alkyl, alkenyl, aryl or C 1 -C aralkyl radical, optionally substituted by one or more halogen atoms, or one or more C 1 -C 6 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- D-sorbitol, 2,4-mono-O-benzylidene-D-sorbitol, 1,3,2,4-bis (p-methylbenzylidene) sorbitol, 1,3,2,4-bis (3,4-bis), dimethylbenzylidene) sorbitol, 1,3,2,4-bis (p-ethylbenzylidene) sorbitol, 1,3,2,4-bis (p-propylbenzylidene) sorbitol, 1,3,2,4-bis (p-butylbenzylidene) sorbitol, 1,3,2,4-bis (p-ethoxylbenzylidene) sorbitol,
- the organic compound is a compound of general formula (V):
- R represents a linear or branched, saturated or unsaturated chain comprising from 4 to 68 carbon atoms, preferably from 4 to 54 carbon atoms, more preferably from 4 to 36 carbon atoms, and z is an integer ranging from 2 to at 4.
- 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 diacid is sebacic acid.
- 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, in particular C 8 to C 34, especially C 12 to C 22 , in particular C 16 to C 20, and more particularly 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 -COOH or
- the organic compound of general formula (VI) is:
- the organic compound is a compound of general formula (VII):
- 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 from 8 to 12 carbon atoms, which may be substituted, and comprising optionally heteroatoms, rings and / or heterocycles.
- the chemical additive is a paraffin. Paraffins have chain lengths of 30 to 120 carbon atoms (C30 to C20 ).
- the paraffins are advantageously chosen from polyalkylenes. Preferably, 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 85 to 95% of normal paraffins and 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 preferably, the paraffins comprise 85 to 95% normal paraffins and 5 to 15% 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. These are compounds of empirical formula P q H r O s wherein q, r and s are positive numbers such that:
- q> 2 and in particular q is from 3 to 20 or more and that 5q + r-2s 0.
- said polyphosphoric acids may be linear compounds of formula P q H (q + 2) O (3q + 1) corresponding to the structural formula: Where qa the definition given above. They can still be products of two-dimensional or three-dimensional structure.
- All these polyphosphoric acids can be considered as polycondensation products by heating aqueous metaphosphoric acid.
- a chemical additive when used in the material which can be used as a road binder or as a sealing binder, it is chosen from compounds of formula (I), compounds of formula (II), compounds of formula (V) and mixtures of these compounds.
- a chemical additive when used in the material that can be used as a road binder or as a sealing binder, it is chosen from:
- hydrazide derivatives such as: C 5 H 5 -CONH-NHCO-C 5 H 1, C 9 H 19 -CONH-NHCO-C 9 H 19 , C 11 H 23 -C CONH-NHCO-C 11 H 23, CIVHBS-CONH-NHCO-CIVHBS, or C 21 H 43 -CONH-
- diamides such as N, N'-ethylenedi (laurylamide) of formula C n H 2 3 CONH-CH 2 -CH 2 -NHCO-C 11 H 31 , N, N-ethylenedi (myristylamide) of formula C 13 H 27 -CONH-CH 2 -CH 2 -NHCO-C 13 H 27 , N, N'-ethylenedi (palmitamide) of formula Ci 5 H 3 i-CONH-CH 2 -CH 2 -NHCO-C 15 H 31 , N N, N-ethylenedi (stearamide) of the formula CONH-C11-C10-NHCO-C13;
- a chemical additive when used in the material that can be used as a road binder or as a sealing binder, it is chosen from:
- a chemical additive when used in the material that can be used as a road binder or as a sealing binder, it is chosen from:
- the first composition comprising, for example, a bitumen base, of which the core of the granules is composed comprises from 0.1% to 10% by weight, preferably from 0.5% to 5% by weight, more preferably from 0.5% to 2.5% by weight of chemical additive relative to the total mass of the first composition.
- the first composition comprises at least two chemical additives.
- the first composition comprises at least one first chemical additive of formula (V) and at least one second chemical additive chosen from: chemical additives of formula (I); chemical additives of formula (II); chemical additives of formula (III); chemical additives of formula (V); chemical additives of formula (VI); chemical additives of formula (VII) and the reaction products of at least one polyol C 3 -C 2 and at least one aldehyde C 2 -C 12, in particular those comprising a group of formula (IV), the second chemical additive being distinct from the first chemical additive.
- second chemical additive chosen from: chemical additives of formula (I); chemical additives of formula (II); chemical additives of formula (III); chemical additives of formula (V); chemical additives of formula (VI); chemical additives of formula (VII) and the reaction products of at least one polyol C 3 -C 2 and at least one aldehyde C 2 -C 12, in particular those comprising a group of formula (IV), the second chemical additive being distinct from the first chemical additive.
- the first composition comprises at least one first chemical additive of formula (V) and at least one second chemical additive of formula (II).
- the first composition comprises at least one first additive of formula (V) and at least one second chemical additive of formula (IIA).
- the first composition comprises at least one first chemical additive of formula (II) and at least one second chemical additive chosen from: chemical additives of formula (I); chemical additives of formula (II); chemical additives of formula (III); chemical additives of formula (V); chemical additives of formula (VI); the chemical additives of formula (VII) and the reaction products of at least one C 3 -C 12 polyol and at least one C 2 -C 12 aldehyde, in particular those comprising a group of formula (IV), the second chemical additive being distinct from the first chemical additive.
- second chemical additive chosen from: chemical additives of formula (I); chemical additives of formula (II); chemical additives of formula (III); chemical additives of formula (V); chemical additives of formula (VI); the chemical additives of formula (VII) and the reaction products of at least one C 3 -C 12 polyol and at least one C 2 -C 12 aldehyde, in particular those comprising a group of formula (IV), the second chemical additive being distinct from the first chemical additive.
- the first chemical additive of formula (II) is chosen from chemical additives of formula (II A).
- the first composition comprises at least one first chemical additive of formula (IIA) and at least one second chemical additive chosen from: chemical additives of formula (I); chemical additives of formula (IIB); chemical additives of formula (III); chemical additives of formula (V); chemical additives of formula (VI); the chemical additives of formula (VII) and the reaction products of at least one C 3 -C 12 polyol and at least one C 2 -C 12 aldehyde, in particular those comprising a group of formula (IV), the second chemical additive being distinct from the first chemical additive.
- second chemical additive chosen from: chemical additives of formula (I); chemical additives of formula (IIB); chemical additives of formula (III); chemical additives of formula (V); chemical additives of formula (VI); the chemical additives of formula (VII) and the reaction products of at least one C 3 -C 12 polyol and at least one C 2 -C 12 aldehyde, in particular those comprising a group of formula (IV), the second chemical additive being distinct from the first chemical additive
- the first composition comprises at least one first additive of formula (IIA) and at least one second chemical additive of formula (V).
- (II) is N, N'-ethylenedi (stearamide).
- the first composition comprises at least sebacic acid or 1,10-decanedioic acid and at least ⁇ , ⁇ '-ethylenedi (stearamide).
- the first composition comprises at least one first additive of formula (I) and at least one second chemical additive chosen from: chemical additives of formula (I); chemical additives of formula (II); chemical additives of formula (III); chemical additives of formula (V); chemical additives of formula (VI); chemical additives of formula (VII) and the reaction products of at least one polyol C3-C 12 and at least one aldehyde C 2 -C 12, in particular those comprising a group of formula (IV), the second chemical additive being distinct from the first chemical additive.
- second chemical additive chosen from: chemical additives of formula (I); chemical additives of formula (II); chemical additives of formula (III); chemical additives of formula (V); chemical additives of formula (VI); chemical additives of formula (VII) and the reaction products of at least one polyol C3-C 12 and at least one aldehyde C 2 -C 12, in particular those comprising a group of formula (IV), the second chemical additive being distinct from the first chemical additive.
- the second chemical additive is chosen from the chemical additives of formula (II) and the chemical additives of formula (V).
- the second chemical additive of formula (II) is chosen from the chemical additives of formula (II A).
- the second chemical additive of formula (II) is N, N'-ethylenedi (stearamide).
- the second chemical additive of formula (V) is sebacic acid or 1,10-decanedioic acid.
- the first chemical additive of formula (I) is 2 ', 3-bis [(3- [3, 5-di-tert-butyl-4-hydroxyphenyl] propionyl]] propionohydrazide.
- the mass ratio of the first chemical additive with respect to the second chemical additive is from 1: 99 to 99: 1, preferably from 1: 9 to 9: 1, even more preferably from 1: 5 to 5: 1.
- the first composition may further comprise at least one olefinic polymer adjuvant.
- the olefin 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 from 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 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 random or block copolymers of Any statistics, ethylene and alkyl acrylate or methacrylate to C 6, comprising from 40% to 99.7% o by weight, preferably 50%> 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 additive polymer is selected from olefinic random terpolymers of ethylene (b), of a monomer A chosen from acrylates or methacrylates of alkyl to C 6 and a monomer B selected from acrylate of 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% to 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 composition comprising for example a bitumen base, which is composed of the core of the granules, comprises from 0.05% to 15% by weight, preferably from 0.1% to 10% by weight. % by weight, more preferably from 0.5% to 6% by weight of the olefinic polymer adjuvant, relative to the total weight of the first composition.
- the first composition may also comprise other known additives or other known bitumen elastomers such as SB copolymers (block copolymer of styrene and butadiene), SB S (copolymer with styrene-butadiene-styrene blocks), SIS (styrene-isoprene-styrene), SBS * (star styrene-butadiene-styrene block copolymer), SBR (styrene-b-butadiene rubber), EPDM (modified ethylene propylene diene) .
- SB copolymers block copolymer of styrene and butadiene
- SB S copolymer with styrene-butadiene-styrene blocks
- SIS styrene-isoprene-styrene
- SBS * star styrene-butadiene-styrene block cop
- the first composition comprises a combination of the chemical additive of formula (II) and the olefinic polymer adjuvant described above.
- the coating layer / second composition :
- the coating layer is obtained by applying all or part of the surface of the bitumen core of a composition comprising:
- At least one viscosifying compound At least one viscosifying compound
- At least one first anti-caking agent chosen from alkali metal and / or alkaline earth metal silicates whose SiO 2 silica: metal oxide M ⁇ O molar ratio is from 1.00 to 4.00, M representing the metal cation and x being 1 or 2 depending on the nature of the alkali or alkaline earth metal cation, and
- the precursor composition of the coating layer may comprise at least one solvent to facilitate its application.
- the coating layer is solid at elevated ambient temperature, especially at a temperature above 60 ° C.
- the average thickness of the coating layer is preferably greater than or equal to 20 ⁇ , more preferably between 20 and 200 ⁇ , and still more preferably from 40 to 150 ⁇ , and still more preferably from 50 to 100 ⁇ .
- the coating layer must be thick enough for it to be continuous.
- the coating layer may optionally comprise one or more compounds chosen from: the chemical additives which have been described above, the polymers, the plasticizers, the surfactants. ..
- the coating layer consists essentially of:
- silicates of alkali metals and / or of alkaline earth metals whose molar ratio of silica SiO 2 : metal oxide M ⁇ O is from 1.00 to 4.00, M representing the metal cation and x being equal to 1 or 2 depending on the nature of the alkali or alkaline earth metal cation
- One or more anti-caking agents distinct from the silicates are distinct from the silicates.
- the coating layer comprises, or better consists essentially of:
- the coating layer comprises, or better consists essentially of:
- alkali metal and / or alkaline earth metal silicates whose SiO 2 silica: metal oxide M ⁇ O molar ratio is from 1.00 to 4.00, M representing the metal cation and x being 1 or 2 depending on the nature of the alkali or alkaline earth metal cation, and
- the coating layer comprises, or better consists essentially of:
- the second composition is in the form of a solution or a dispersion in a solvent.
- the solvent is advantageously chosen from water and mixtures of water and organic solvents miscible with water such as alcohols, for example ethanol, methanol, glycerol.
- the concentration of material other than the solvent in said solutions and / or dispersions is from 50 g / l to 500 g / l, preferably from 75 g / l to 300 g / l and even more preferentially from 100 g / l. at 250 g / L.
- viscosifier and “viscosifying compound” are used in the sense of the invention, in an equivalent manner and independently of one another.
- viscosifier or “viscosifying compound” is meant a compound which has the property of decreasing the fluidity of a liquid or a composition and thus increasing its viscosity.
- the viscosifier within the meaning of the invention 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 at 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. by means of a Brookfield CAP 2000+ viscometer and at a rotation speed of 750 rpm. The measurement is read 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;
- PEG polyethylene glycols
- PEG-800 polyethylene glycols
- PEG-1000 polyethylene glycols
- PEG-1500 a PEG having a molecular weight of 4000 g. mol-1 (PEG-4000) or PEG having a molecular weight of 6000 gmol-1 (PEG-6000)
- PEG-6000 polyethylene glycols
- the viscosifying compound is chosen from:
- gelling compounds preferably of vegetable or animal origin, such as: gelatin, agar-agar, alginates, cellulose derivatives or gellan gums;
- PEG polyethylene glycols
- PEG-800 polyethylene glycols
- PEG-1000 polyethylene glycols
- PEG-1500 polyethylene glycols
- the coating composition comprises at least 25% by weight of at least one viscosifying compound relative to the total mass of the composition, preferably from 25 to 50% by weight, more preferably from 30 to 47% by weight, and preferably from 35% to 44% by weight.
- the composition is solid at room temperature, including at elevated ambient temperature.
- the granules may further comprise one or more other coating layers, based on anti-caking agent covering all or part of the composition comprising at least one anti-caking agent and at least one viscosifying.
- anti-caking compounds are of mineral or organic origin.
- anti-caking agent or “anti-caking compound” is meant any compound which limits, reduces, inhibits, delays, the agglomeration and / or the adhesion of the granules together during their transport and / or their storage. at room temperature and which ensures their fluidity during handling.
- the coating layer of the granules according to the invention comprises at least one first anti-caking agent chosen from silicates.
- Silicates are salts of a negatively charged backbone and essentially formed of silicon atoms and oxygen atoms, and one or more metal cations.
- salt means an ionic compound comprising at least one cation and at least one anion and whose overall electrical charge is zero.
- the silicates are silicates of alkali metals and / or alkaline earth metals.
- the silicates are alkali metal silicates.
- the silicates are chosen from lithium silicates, sodium silicates, potassium silicates, rubidium silicates, cesium silicates, francium silicates and mixtures thereof.
- the silicates are selected from sodium silicates, potassium silicates and mixtures thereof.
- the silicates are sodium silicates.
- the anionic backbone of the alkali metal and / or alkaline earth metal silicates is formed of one or more silicic units bonded together by pooling at least one oxygen atom.
- silicic unit is meant in the sense of the invention the conjugate bases of silicic acids.
- Silicic acids are chemical compounds comprising one or two silicon atoms bonded to one or more oxo groups and / or one or more hydroxyl groups.
- silicic acids there may be mentioned orthosilicic acid H 4 SiO 4 , pyrosilicic acid H 6 Si 2 O 7, metasilicic acid H 2 SiO 3 or disilicic acid of formula H 2 Si 2 O 5 .
- the silicates comprise units derived from orthosilicic acid. Even more preferentially, the silicates are composed essentially of units derived from orthosilicic acid.
- the silicates are selected from the sodium salts of orthosilicic acid.
- the backbone comprises a single silicic unit.
- the backbone is composed of several silicic units bonded together by the pooling of one or more oxygen atoms.
- skeletons are similar to polymeric chains whose monomers are silicic acids.
- the silicic acids bind to one another by pooling one or more oxygen atoms and form chains essentially composed of silicon atoms and oxygen atoms.
- These skeletons can be linear, branched or can form a three-dimensional network.
- the silica SiO 2 : metal oxide M ⁇ O molar ratio of the silicates is from 1.00 to 4.00, preferably ranging from 1.5 to 4 and even more preferentially ranging from 2 to 3.75, M representing the metal cation and x being 1 or 2 depending on the nature of the alkali or alkaline earth metal cation.
- the silicates are chosen from sodium silicates.
- the silica Si0 2 : sodium oxide: Na 2 0 mass ratio of sodium silicates is from 1.00 to 4.00, preferably ranging from 1.5 to 3.75 and even more preferentially. ranging from 2 to 3.50.
- the silicates are in hydrated form.
- the silicates correspond to the following formula (VIII):
- M represents the metal cation
- x is 1 or 2 depending on the nature of the metal cation
- y is a number ranging from 1.00 to 4.00, preferably from 1.5 to 4, still more preferably ranging from 2 to 3.75, and
- z is a number ranging from 0.00 to 10.00, preferably from 5.00 to 10.00.
- the silicates correspond to the following formula (IX):
- y is a number ranging from 1.00 to 4.00, preferably from 1.5 to 4, still more preferably ranging from 2 to 3.75, and
- z is a number ranging from 0.00 to 10.00, preferably from 5.00 to 10.00.
- the silicates are in the form of sols or gels in an aqueous medium.
- silicate sol is intended to mean a colloidal solution in which the silicates are dispersed in a continuous medium, preferably an aqueous medium.
- the coating composition comprises from 1% to 50% by weight of at least one first anti-caking agent chosen from silicates relative to the total mass of the coating composition, from preferably from 5 to 40% by weight, more preferably from 10 to 30% by weight.
- the coating layer of the granules according to the invention also comprises at least one second anti-caking agent distinct from the silicates.
- the second anti-caking agent is chosen from: talc; the fines, also called “fibers", generally of diameter less than 125 ⁇ , such as siliceous fines, with the exception of fine limestones; sand such as fountain sand; cement ; carbon; wood residues such as lignin, lignosulphonate, conifer needle powders, conifer cone powders, especially pine powders; the ashes of rice balls; glass powder; clays such as kaolin, bentonite, vermiculite; alumina such as alumina hydrates; silica; silica derivatives such as silica fumes, functionalized silica fumes, in particular hydrophobic or hydrophilic silica fumes, pyrogenic silicas, especially hydrophobic or hydrophilic pyrogenic silicas, silicon hydroxides and silicon oxides; plastic powder; lime; hydrated lime; the plaster ; rubber crumb; polymer powder, such as styrene-butadiene
- the second 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; silica fumes, especially hydrophobic or hydrophilic silica fumes; and their mixtures.
- the second anti-caking agent is chosen from the fines, preferably chosen from fines with a diameter of less than 125 ⁇ , with the exception of fine limestones.
- the second anti-caking agent is selected from siliceous fines.
- the coating composition comprises at least 25% by weight of at least one second anti-caking agent with respect to the total weight of the coating composition, preferably from 25 to 49%. by weight, more preferably from 30 to 48% by weight and even more preferably from 35 to 46% by weight.
- the term "granules of material that can be used as a road binder or as a sealing binder” can also be defined as a material that can be used as a road binder or as a solid sealing binder at room temperature in a divided form. , that is to say in the form of small units called granules or particles, comprising a core made of material usable as a road binder or as a sealing binder and a shell or shell or coating or coating layer or coating.
- the coating layer covering the granules of material that can be used as a road binder or as a sealing binder according to the invention is continuous.
- the coating layer is applied so that at least 90% of the core area of said granules is covered with the coating layer, preferably at least 95%, more preferably at least 99%.
- the coating layer covering at least a portion of the core surface of the granules represents from 0.2% to 20% by weight, preferably from 0.5% to 15% by weight. mass, more preferably from 1% to 10%> relative to the total mass of the heart of the granules.
- the granules of material that can be used as a road binder or as a sealing binder, advantageously bitumen, according to the invention can have, within the same population of granules, one or more forms chosen from a cylindrical, spherical shape. or semi-spherical or ovoid, preferably in a semi-spherical form.
- the size of the granules is such that the longest average dimension is preferably less than or equal to 50 mm, more preferably from 2 to 30 mm, even more preferably from 3 to 20 mm.
- the size and shape of the 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 granules of material that can be used as road binder or as sealing binder, advantageously the bitumen granules, according to the invention have a weight of between 0.1 g and 50 g, preferably between 0.2 g and 10 g. g, more preferably between 0.2 g and 5 g.
- an anti-caking agent selected from alkali metal silicates and / or alkaline earth metal silicones whose SiO 2 silica molar ratio metal oxide ⁇ is from 1.00 to 4.00, M representing the metal cation and x being 1 or 2 depending on the
- M representing the metal cation and x being 1 or 2 depending on the
- the coating layer is resistant to the transport and / or storage of the material that can be used as a road binder or as a sealing binder, in particular bitumen, at high ambient temperature, especially at a temperature greater than 60 ° C., in " Big Bags "while being brittle under the effect of mechanical shear. It allows the liberation of the heart during the manufacture of asphalt.
- the bitumen granules may further comprise one or more other coating layers covering all or part of the coating layer of the solid material that can be used as a road binder or as a sealing binder, in particular bitumen, according to the invention. - Production process of the granules:
- Another subject of the invention relates to a method for producing granules of solid material that can be used as a road binder or as a sealing binder, in particular bitumen, composed of a core and a coating layer of the core, this process comprising :
- Step ii) shaping the core from at least one first composition, and ii) embedding the core on all or part of its surface with at least a second composition comprising at least one viscosifiable compound, at least a first anti-caking agent chosen from alkali metal and / or alkaline-earth metal silicates whose molar ratio of SiO 2 silica: MxO metal oxide is from 1.00 to 4.00, M representing the metal cation and x being equal to 1 or 2 depending on the nature of the alkali or alkaline earth metal cation and at least one second anti-caking agent distinct from the silicates.
- Step ii) may be carried out by dipping, spraying, coextrusion, etc.
- step ii) is carried out by a method employing a fluidized air bed device.
- the shaping of the core of the granules from a solid material that can be used as a road binder or as a sealing binder, in particular bitumen can be carried out according to any known method, for example according to the manufacturing method described in the US document. 3,026,568, WO 2009/153324 or WO 2012/168380. According to a particular embodiment, the shaping of the core of solid material can be carried out by dripping, in particular using a drum.
- the coating of granules of solid material that can be used as a road binder or as a sealing binder, in particular bitumen may be made by any known technique, in particular by applying the second material in a fluidized air bed process, as described by US Pat. example in US-5,236,503 or in EP 1,407,814.
- the method according to the invention may comprise an additional step of drying the granules obtained in step ii), this drying step being carried out at a temperature ranging from 20 to 60 ° C. and during a duration ranging from 5 minutes to 5 hours, preferably from 5 minutes to 2 hours.
- the core particles of solid material have a longest average dimension ranging from 1 to 30 mm, preferably from 2 to 20 mm, even more preferably from 2 to 10 mm.
- the ratio by weight of the coating layer to the mass of the core, optionally additive is from 0.05 to 1, advantageously from 0.1 to 0.9, even more advantageously from 0.1 to 0.5.
- Another subject of the invention consists of granules of solid material which can be used as road binder or as sealing binder, in particular bitumen, which can be obtained by implementing the method according to the invention as described hereinabove. above.
- Such granules advantageously have the properties described above. - Uses of the granules:
- Another object of the invention also relates to the use of the granules according to the invention as a road binder.
- the road binder can be used to manufacture mixes, in combination with aggregates according to any known method.
- the granules of solid material that can be used as a road binder or as a sealing binder, in particular bitumen, according to the invention are used for the manufacture of mixes.
- Bituminous or non-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 or non-bituminous binder and road aggregate having particular properties, such as anti-rutting layers, draining asphalts, or asphalts (a mixture of bituminous binder and sand-like aggregates).
- Another subject of the invention relates to a process for the manufacture of mixes comprising at least one road binder and aggregates, the road binder being chosen from the granules of solid material according to the invention, this process comprising at least the steps of:
- 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 a prior step of heating the granules of solid material.
- the process for manufacturing mixes according to the invention does not require a step of heating the granules before mixing with the aggregates because in contact with the hot aggregates, the granules melt.
- the granules of solid material that can be used as road binder or as sealing binder, especially bitumen, according to the invention as described above have the advantage of being able to be added directly to hot aggregates, without having to be melted beforehand. mixing with hot aggregates.
- the step of mixing the aggregates and the road binder is carried out with stirring, then the stirring is maintained for not more than 5 minutes, preferably not more than 2 minutes to allow to obtain a homogeneous mixture.
- the granules according to the present invention are remarkable in that they allow the transport and / or the storage and / or the handling of road bitumen at high ambient temperature under extreme conditions, in particular without agglomeration and / or adhesion of granules of solid material during their transport and / or storage and / or handling.
- the coating layer of the granules breaks under the effect of contact with hot aggregates and shear and releases the composition forming the core.
- the presence of the coating layer in the road binder and aggregate mixture does not degrade the properties of said road bitumen for road application, as compared to an uncoated core composition.
- the granules obtained by the process of the invention can be transported and / or stored and / or handled in the form of granules of solid material, in particular bitumen, which are solid at ambient temperature.
- the solid material especially road bitumen, can be 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 .
- the granules of solid material, in particular bitumen, obtained by the process according to the invention have the advantage of keeping 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 this packaging to equipment, as a construction equipment (tank, mixer etc ).
- the granules of solid material, especially bitumen 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 made of hot-melt material. They may also be transported and / or stored in bulk in cartons of 5 kg to 30 kg or in drums of 100 kg to 200 kg.
- the various embodiments, variants, preferences and advantages described above for each of the objects of the invention apply to all the objects of the invention and can be taken separately or in combination. Figures:
- Figure 1 Sectional view of the fluidized bed installation
- Figure 1 shows a sectional view of a fluidized air bed granulator.
- the fluidized air bed installation (10) (also known as a granulator) comprises a fluidised air bed process chamber (11) in which the cores in one bituminous material (14) are placed and in which an air stream (16) is fed from below to the fluidized bed (12) and through a perforated grid (13) to maintain the fluidized bed and to dry and / or cooling the cores of bituminous material (14).
- a precursor composition of the coating layer (18) is then fed to the fluidized bed via a spray nozzle (20) emerging from below into the fluidized bed (12).
- the fluidized-bed process chamber (12) also comprises an insert (22) located above the spray nozzle (20) and in the form of a cylindrical installation piece adjustable in height and diameter. and whose lower edges (15) are adjustably spaced from the perforated grid (13) of the bottom of the fluidized bed (12).
- the filtration chamber (IV) comprises several filters (24) for recycling the fine particles emitted during the implementation of the process.
- the air stream (16) fed to the fluidized bed (12) is guided by an incoming air box (I) comprising an inlet air chamber (26).
- the granulator (10) with fluidized air bed (12) thus comprises 4 distinct zones: (I) the incoming air casing, (II) the process chamber, (III) the expansion chamber and (IV) the filtration chamber.
- the zone of the fluidized bed formed by the inlet air chamber (26) has a zone (28) with a higher flow velocity of the air stream (16) applied to the cores of bituminous material (14).
- the precursor composition of the coating layer (18) is fed into the zone (28) operating at a higher flow rate.
- the cores of bituminous material (14) from the higher flow rate zone (28) are returned to the fluidized bed (12). Part of the cores of bituminous material (14) present in the fluidized bed (12) is returned to the zone (28) at a higher flow rate, so that a circulation of cores made of bituminous material appears (14) between the fluidized bed (12) and the zone (28) at a higher flow rate.
- bituminous material cores used as raw material in the examples below are composed of:
- bitumen base grade 50/70, rated Bi having a penetrability P 25 of 58 1/10 mm and a TBA of 49.6 ° C and commercially available from the TOTAL group under the trademark AZALT ®
- Table 1 Composition of the bituminous binder constituting the heart of the granules
- the amounts are expressed as a percentage by mass of additive compound relative to the total mass of the composition.
- the coating composition used for coating the cores of the granules is prepared from the following compounds:
- VI viscosifying agent pregelatinized maize starch introduced in the form of Lycatab® C commercially available from Roquette Anti-caking agent:
- AGI anti-caking agent sodium silicate introduced in the form of Betol® 39 T sold by the company Woellner,
- Anti-agglomerating agent AG2 talc introduced in the form of GPR RECTAPUR® commercially available from VWR (CAS 14807-96-6), and
- AG3 anti-caking agent mineral fillers with a diameter less than or equal to 0.063 mm.
- the bitumen base (Bi) is introduced into a reactor maintained at 160 ° C. with stirring at 300 rpm for two hours.
- the additives are then introduced into the reactor.
- the contents of the reactor are maintained at 160 ° C. with stirring at 300 rpm for 1 hour.
- the core composition is heated at 160 ° C for two hours in an oven before being cast in a silicone mold having different spherical holes so as to form the solid binder cores. After observing the solidification of the binder in the mold, the surplus is leveled with a heated blade Bunsen burner. After 30 minutes, the solid binder in the form of uncoated granules is demolded and stored in a tray coated with silicone paper. The cores are then allowed to cool by binding at room temperature for 10 to 15 minutes.
- Bitumen granules can also be obtained from the bituminous composition according to the invention poured into the tank of such a device and maintained at a temperature between 130 and 160 ° C.
- a nozzle or several injection nozzles allow the transfer of the bitumen composition according to the invention into the interior of the double drum with a rotating outer drum, the two drums being equipped with slots, nozzles and orifices. allowing the pastiUation of bitumen drops through the first fixed drum and orifices having a diameter of between 2 and 8 mm from the rotating outer drum. The drops of bitumen are deposited on the upper face of a tread, horizontal, driven by rollers.
- Bitumen granules were obtained from the bituminous composition C1 poured into the tank of such a device and maintained at a temperature between 130 and 160 ° C.
- a nozzle or several injection nozzles allow the transfer of the bituminous composition C1 into the interior of the double drum with a rotating outer drum, the two drums being equipped with slots, nozzles and orifices for the treatment of drops of bitumen through the first fixed drum and orifices having a diameter of between 2 and 8 mm from the rotating outer drum.
- the drops of bitumen are deposited on the upper face of a tread, horizontal, driven by rollers.
- the precursor composition of the coating layer is an aqueous composition comprising at least:
- bitumen cores previously obtained in I- are stitched onto a needle before being immersed in the coating composition.
- the coated bitumen granules are deposited on a silicone plate
- the coated solid bitumen granules thus obtained may be coated with an additional layer with the lignin powder.
- the solid bitumen granules thus obtained are left in the open air for at least 2 hours and at ambient temperature to solidify the coating layer.
- bitumen cores obtained in I- are poured into the coating composition. They are then stirred manually in the solution for a few minutes then they are removed to be on a plate and allowed to dry at room temperature (about 30 ° C).
- the cores made of bituminous material are loaded into the process chamber, the airflow being in operation.
- the cores made of bituminous material are thus fluidized by the flow of air injected into the process chamber.
- the precursor composition of the coating layer is sprayed into the process chamber through the spray nozzle.
- the sticky appearance of the granules is evaluated by a manipulator directly to the touch directly after the step of coating the cores (without a drying step).
- the manipulator takes a dozen granules and evaluates the stickiness of each of them by placing them first between two fingers and then trying to move the fingers of the surface of the granule.
- This test is carried out in order to evaluate the resistance to the load of the granules at a temperature of 25 ° 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 100 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 according to the following protocol: 5 mL of granules are placed in a 20 mL syringe and the piston is placed on the granules and mass of 208g, representing a force applied as in a Big Bag. The whole is placed in an oven at 25 ° C for at least 24 hours.
- the binder cores are dip-coated in the coating composition according to the method described in II-2.a), second variant.
- bitumen granules in Examples 1, 2 and 3 above are then evaluated according to two criteria:
- the granules are agglomerated.
- Example 2 The granules prepared in Example 2 are advantageous in that they do not stick. The latter can then be bagged and stored directly after the coating step without the need for an additional drying step.
- the granules prepared in Examples 1 and 3 are tacky. It is therefore necessary for these granules to proceed with an additional step of drying the coating layer before being able to be bagged.
- the granules prepared in Example 2 are advantageous in that they retain their original shape and exhibit no adhesion.
- Example 2 Therefore, the handling and transport / storage of said granules formed in Example 2 are easy and do not cause alteration of the granules.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Structural Engineering (AREA)
- Civil Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Architecture (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Sealing Material Composition (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR1753475A FR3065465B1 (fr) | 2017-04-21 | 2017-04-21 | Bitume solide a temperature ambiante |
PCT/FR2018/050974 WO2018193211A1 (fr) | 2017-04-21 | 2018-04-18 | Bitume solide a temperature ambiante |
Publications (1)
Publication Number | Publication Date |
---|---|
EP3612617A1 true EP3612617A1 (fr) | 2020-02-26 |
Family
ID=59521016
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP18722688.1A Withdrawn EP3612617A1 (fr) | 2017-04-21 | 2018-04-18 | Bitume solide a temperature ambiante |
Country Status (4)
Country | Link |
---|---|
US (1) | US11447636B2 (fr) |
EP (1) | EP3612617A1 (fr) |
FR (1) | FR3065465B1 (fr) |
WO (1) | WO2018193211A1 (fr) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR3065464B1 (fr) * | 2017-04-21 | 2019-06-28 | Total Marketing Services | Bitume solide a temperature ambiante |
CA3121628A1 (fr) | 2018-12-10 | 2020-06-18 | Total Marketing Services | Composition bitumineuse solide a temperature ambiante |
WO2020120314A1 (fr) * | 2018-12-10 | 2020-06-18 | Total Marketing Services | Composition bitumineuse solide à température ambiante |
Family Cites Families (24)
Publication number | Priority date | Publication date | Assignee | Title |
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US3026568A (en) | 1958-11-14 | 1962-03-27 | Schuller Services Ltd | Method for producing coated bitumen pellets |
US3235483A (en) * | 1963-04-24 | 1966-02-15 | Texaco Inc | Method of granulating asphaltic materials |
EP0012192B1 (fr) | 1978-12-08 | 1983-01-12 | Santrade Ltd. | Dispositif pour extruder des masses fluides d'un récipient |
GB8508613D0 (en) | 1985-04-02 | 1985-05-09 | British Petroleum Co Plc | Chemical process |
US5236503A (en) | 1991-10-28 | 1993-08-17 | Glatt Air Techniques, Inc. | Fluidized bed with spray nozzle shielding |
FR2739863B1 (fr) | 1995-10-16 | 1997-11-21 | Elf Antar France | Procede de preparation de compositions bitume/polymere a caractere multigrade renforce et application des compositions obtenues a la production de liants bitume/polymere pour revetements |
FR2804125B1 (fr) | 2000-01-24 | 2002-10-25 | Total Raffinage Distribution | Liant bitumineux, compositions coloree obtenue a partir de ce liant et leurs applications |
AU9397801A (en) | 2000-10-13 | 2002-04-22 | Bp Exploration Operating | Fischer-tropsch synthesis process |
PE20030220A1 (es) | 2001-07-27 | 2003-04-30 | Sasol Tech Pty Ltd | Produccion de cera obtenida mediante sintesis fischer-tropsch |
EP1407814B1 (fr) | 2002-09-28 | 2014-05-07 | Glatt Ingenieurtechnik GmbH | Procédé et appareillage mettant en oeuvre un lit fluidisé pour fabriquer des granules |
US20040209082A1 (en) * | 2003-04-17 | 2004-10-21 | Lee Willy W. | Process of Coating Tacky and Soft Polymer Pellets |
EP1473327A1 (fr) | 2003-05-01 | 2004-11-03 | KRATON Polymers Research B.V. | Composition colorable |
ATE548425T1 (de) | 2005-11-04 | 2012-03-15 | Latexfalt Bv | Bindemittelzusammensetzung enthaltend ein naphthenisches öl mit niedriger viskosität für gefärbte asphalt-heissmischgut-anwendungen |
EP2589624B1 (fr) | 2005-11-14 | 2015-04-01 | Kraton Polymers US LLC | Composition polymère pour la préparation d'une composition à liant bitumineux |
US7622519B2 (en) | 2007-05-01 | 2009-11-24 | Kraton Polymers U.S. Llc | Bituminous binder composition and process for preparing the same |
US8491985B2 (en) * | 2008-03-31 | 2013-07-23 | Certainteed Corporation | Coating compositions for roofing granules, dark colored roofing granules with increased solar heat reflectance, solar heat-reflective shingles, and process for producing the same |
FR2932487B1 (fr) | 2008-06-12 | 2010-08-27 | Total France | Emulsion de liant synthetique clair. |
US20110115116A1 (en) | 2008-06-20 | 2011-05-19 | De Amorim Novais Da Costa Nobrega Joao Miguel | Method for preparing coated binder units |
US20110233105A1 (en) * | 2008-08-29 | 2011-09-29 | Billian I.P. Limited | Asphalt pellets |
FR2938547B1 (fr) | 2008-11-14 | 2012-11-16 | Total Raffinage Marketing | Liant synthetique clair |
FR2948677B1 (fr) | 2009-07-29 | 2011-09-16 | Total Raffinage Marketing | Procede de preparation de compositions bitume/polymere reticulees sans agent reticulant |
EP2718375B1 (fr) | 2011-06-07 | 2015-03-18 | Shell Internationale Research Maatschappij B.V. | Procédé de préparation d'unités à base de liant revêtu |
FR3024456B1 (fr) | 2014-08-01 | 2016-08-19 | Total Marketing Services | Granules de bitume routier |
FR3037337B1 (fr) | 2015-06-09 | 2019-06-14 | Total Marketing Services | Bitume solide a temperature ambiante |
-
2017
- 2017-04-21 FR FR1753475A patent/FR3065465B1/fr not_active Expired - Fee Related
-
2018
- 2018-04-18 WO PCT/FR2018/050974 patent/WO2018193211A1/fr active Application Filing
- 2018-04-18 EP EP18722688.1A patent/EP3612617A1/fr not_active Withdrawn
- 2018-04-18 US US16/606,827 patent/US11447636B2/en active Active
Also Published As
Publication number | Publication date |
---|---|
FR3065465B1 (fr) | 2019-06-28 |
WO2018193211A1 (fr) | 2018-10-25 |
FR3065465A1 (fr) | 2018-10-26 |
US11447636B2 (en) | 2022-09-20 |
US20200040187A1 (en) | 2020-02-06 |
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