WO2006013194A1 - Method for preparing a cold process road surfacing composition - Google Patents

Method for preparing a cold process road surfacing composition Download PDF

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Publication number
WO2006013194A1
WO2006013194A1 PCT/EP2005/053726 EP2005053726W WO2006013194A1 WO 2006013194 A1 WO2006013194 A1 WO 2006013194A1 EP 2005053726 W EP2005053726 W EP 2005053726W WO 2006013194 A1 WO2006013194 A1 WO 2006013194A1
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WIPO (PCT)
Prior art keywords
emulsion
bitumen
bituminous
surfactant
fraction
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Application number
PCT/EP2005/053726
Other languages
French (fr)
Inventor
Sophie Mariotti
Joël HERAULT
Original Assignee
Total France
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Filing date
Publication date
Application filed by Total France filed Critical Total France
Priority to EP05771768A priority Critical patent/EP1781403A1/en
Publication of WO2006013194A1 publication Critical patent/WO2006013194A1/en

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
    • C09K23/56—Glucosides; Mucilage; Saponins
    • 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
    • C08L95/005—Aqueous compositions, e.g. emulsions
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00

Definitions

  • the present invention relates to the preparation and manufacture of cold road coatings, used in particular in the road industry, by implementing an emulsion of bitumen associated with aggregates.
  • the invention also relates to a novel bituminous emulsion comprising at least one nonionic surfactant of alkylpolyglycoside type as well as the bitumen / granulate combination (s), in particular in the form of bituminous mixes, containing said type of emulsion.
  • Bitumen is a heavy product that can come from different origins. It can in particular be obtained from the most viscous fraction produced during the direct distillation of crude oil.
  • the composition of the bitumen is variable and depends on the origin of the crude oil. Bitumens consist essentially of saturated oils, aromatic oils, resins, called maltenes, and asphaltenes. For more information in this regard, it is useful to refer for example to the European patent EP-B-0 246 956.
  • Bitumen is used in many road and / or industrial applications.
  • bituminous mixes are used as materials for the construction and maintenance of pavement bodies and their pavement, as well as for carrying out all road works.
  • Bituminous mixes comprise at least one bituminous binder and aggregates.
  • Bituminous mixes are classified in two categories: hot mixes and cold mixes.
  • bitumen In the case of hot mixes, the bitumen is heated to an elevated temperature of greater than 160 ° C., which makes it possible to reduce its viscosity.
  • these techniques consume a lot of energy (storage, transportation of bitumen). They also cause difficult handling which requires control of the various steps to facilitate the application conditions of hot bitumen, raised to high temperatures.
  • the cold mixes are made by emulsifying a bitumen in aqueous phase, with the aid of a surfactant, by supplying mechanical energy necessary for the dispersion of the binder in droplets in water, then by mixing with the aggregates, at lower temperatures, of the order of 60 ° C.
  • an object of the invention is to provide a novel process for preparing a bitumen / cold aggregate combination using a bituminous emulsion whose application conditions are facilitated over previously known solutions.
  • An additional objective is to propose a new process for the preparation of a bituminous mix, using a bituminous emulsion, for road applications, while retaining the mechanical characteristics, resistance to thermal stress, maneuverability and control. during the application, achieved so far.
  • Another object of the invention is to propose, for the preparation of a bituminous emulsion included in a bitumen / granulate combination, the use of surfactants whose impact on the environment is reduced (in particular not labeled R50 or R53 according to the regulations in force).
  • EB emulsion
  • TA surfactant
  • bituminous emulsion means a composition of at least two liquid phases comprising an aqueous phase -or continuous liquid dispersion phase and at least one liquid phase dispersed in the form of droplets in the dispersion.
  • a bituminous emulsion comprises, for example, an aqueous phase and droplets or globules of bitumen, dispersed in the aqueous phase. It is then an oil-in-water emulsion.
  • a bitumen / cold aggregate association can serve as a basis for the development of various road surfaces: wearing course, tie layer and base course.
  • a wearing course is a superficial road surface covering the structure of the road surface, which is directly affected by traffic and climate aggression.
  • superficial coatings, cold mixes and cold-cast asphalts which result from the implementation of different techniques known to those skilled in the art, are distinguished.
  • a tie layer is a road surface, located in the pavement structure at an intermediate position between a wearing course and a base course.
  • a base layer is a road surface that is a foundation of the roadway.
  • a bonding layer and a base layer may consist for example of a cold mix or a serious-emulsion.
  • cold mix or “cold bituminous mix” is used interchangeably to mean a cold bituminous mix in the strict sense (BBDF), a cold-poured bituminous mix (ECF) and a severe emulsion (which can especially be manufactured at room temperature in a stationary or mobile mixing plant and also spread at room temperature).
  • BBDF strict sense
  • ECF cold-poured bituminous mix
  • severe emulsion which can especially be manufactured at room temperature in a stationary or mobile mixing plant and also spread at room temperature.
  • bitumen emulsion is brought into contact with the aggregates by mixing or mixing.
  • the contact between the bituminous emulsion and the aggregates is carried out by spreading the emulsion and granules and compacting them.
  • the invention also relates to a process for preparing a cold bituminous mix comprising:
  • EB emulsion
  • TA surfactant
  • the alkylpolyglycosides are defined as follows. These are molecules comprising a saccharide fraction of 1 to 10 saccharide units, linked by an ether linkage to a C6 to C20 hydrocarbon fraction. The saccharide fraction has hydrophilic properties, while the hydrocarbon fraction has hydrophobic properties. Alkylpolyglycosides are a family of nonionic surfactants particularly interesting for their properties and because the raw materials used for their manufacture come from biomass. The process for producing alkylpolyglycosides is widely described in the scientific literature.
  • the saccharide units comprise from 3 (triose) to 7 (heptose) carbon atoms, preferably from 5 (pentose) to 6 (hexose) carbon atoms.
  • it is arabinose, xylose, glucose, mannose, galactose and / or fructose, but other pentoses and / or hexoses are also possible.
  • the saccharide units are in hemiacetal (in the case of an aldose) or hemiketal (in the case of ketosis) cyclic form, preferably in the form of furan (5-atom ring) and / or pyran (6-atom ring) ).
  • the saccharide units it is possible to replace an alcohol function -OH with an amino function -NH 2 or with a thiol function -SH.
  • the hydrogen atom (s) of the alcohol and / or amine and / or thiol functions may be replaced by a Cl-C4 alkyl group (s).
  • the saccharide moiety comprises from 1 to 10 units and more preferably 1, 2 or 3 units up to 6 units. It may, for example, be, in addition to the pentoses and hexoses mentioned above, sucrose, maltose, lactose, cellobiose, trehalose, raffinose, cellotriose and / or panose. Saccharide fractions consisting of glucose units are more particularly preferred.
  • the surfactant (TA) is then an alkylpolyglucoside (APG).
  • the hydrocarbon fraction is a saturated or unsaturated, linear or branched aliphatic group comprising from 6 to 20 carbon atoms, and more preferably, 8, 10, 12, 14 or 16 carbon atoms.
  • the hydrocarbon fraction is derived from a saturated linear fatty alcohol, such as caprylyl (C8), caprylic (ClO), lauryl (C12), myristic (C14), palmitic (C16) or stearic (Cl8) alcohol. ).
  • the surfactant is preferably present in the form of a mixture of several variable alkylpolyglycosides at the level of the saccharide fraction and / or at the level of the hydrocarbon fraction.
  • the saccharide fraction has an average degree of polymerization of 1 to 5, preferably 1 to 3, and more preferably close to 1.5.
  • the hydrocarbon fraction preferably comprises linear C8, ClO, Cl 2 and / or C14 alkyl groups.
  • the pH of an aqueous solution of a mixture of alkylpolyglycosides at 10 g / l may in particular be greater than 10 and is preferably from 11 to 13, and more preferably from 11.5 to 12.5. .
  • the pH of the aqueous alkylpolyglycoside solution can be adjusted
  • the surfactant (or the surfactant mixture) is provided, for example, in the form of an aqueous solution comprising at least 25% by weight of alkylpolyglycoside surfactant in the solution.
  • this weight percentage is at least 50% and less than 70% by weight.
  • Alkylpolyglycosides and more particularly alkylpolyglucosides, are commercially available products, in particular from Cognis, Akzo
  • a mixture of alkylpolyglucosides of average degree of polymerization substantially equal to 1.5 and whose hydrocarbon fraction is C8 to C10 and / or C8 to C14 is preferably used as surfactant. From the point of view of biodegradability, these surfactants are classified
  • bitumen used is chosen from natural bitumens, distillation bitumens or synthetic bitumens or mixtures thereof. These bitumens can be used pure, fluxed, and / or modified with at least one polymer. In particular, it is possible to distinguish pure bitumens, fluidized bitumens, fluxed bitumens, oxidized bitumens and polymer bitumens.
  • a natural bitumen is a natural blend of bitumen and mineral fines.
  • a distillation bitumen is obtained from the most viscous fraction produced during the direct distillation of crude oil.
  • Other physicochemical techniques such as solvent deasphalting and blowing make it possible to obtain synthetic bitumens.
  • Fluxed bitumens are compositions of bitumen (s) obtained from pure bitumens, the viscosity of which has been lowered by the addition of volatile solvents.
  • fluxed bitumens are obtained by mixing, for example at 150 ° C, on the one hand, bituminous binder, and on the other hand, fluxing.
  • petroleum fluxes and plant fluxes are known.
  • the fluidized bitumens are obtained by mixing bituminous binders with carbochemical or petroleum oils. Fluxed bitumens differ from fluidized bitumens, in particular by the distillation curve of their fluxes, more essentially upwards, but it will be considered in the rest of the description that the terms "fluidized" and
  • the modified bitumens are obtained by mixing with a bitumen composition (s) at least one polymer-type compound, in order to improve its mechanical and thermal performance.
  • a bitumen composition s
  • polymer-type compound in order to improve its mechanical and thermal performance.
  • EPDM ethylene propylene diene monomer
  • EPM ethylene propylene monomer
  • polyisobutylene polybutadiene polyisoprene
  • thermoplastic elastomers such as random or styrene and butadiene random or styrene or block copolymers (SBR, SBS) or styrene and isoprene (SIS) copolymers, optionally crosslinked, polyvinyl chloride,
  • the aggregates used are road aggregates, meeting the relevant standards: NF EN 13043 "Aggregates for hydrocarbon mixtures and for surface coatings used in the construction of pavements, airfields and other traffic areas” in Europe, ASTM C33 “Standard Specification for Concrete Aggregates " to the relevant standards: NF EN 13043 "Aggregates for hydrocarbon mixtures and for surface coatings used in the construction of pavements, airfields and other traffic areas” in Europe, ASTM C33 “Standard Specification for Concrete Aggregates " to the relevant standards: NF EN 13043 "Aggregates for hydrocarbon mixtures and for surface coatings used in the construction of pavements, airfields and other traffic areas” in Europe, ASTM C33 “Standard Specification for Concrete Aggregates " to the relevant standards: NF EN 13043 "Aggregates for hydrocarbon mixtures and for surface coatings used in the construction of pavements, airfields and other traffic areas” in Europe, ASTM C33 “Standard Specification for Concrete Aggregates " to
  • TS very siliceous aggregates With silicate acidic aggregates> 65% SiO 2 ; SiO 2 intermediate silicate aggregates between 52 and 65%; B basic silicate granules SiO 2 between 42 and 52%; UB ultrabasic limestone aggregates SiO 2 ⁇ 42%.
  • an emulsion (EB) of bitumen is initially prepared in an aqueous phase, using a surfactant (TA) to facilitate the emulsification of the bitumen.
  • TA surfactant
  • the result is an oil-in-water emulsion.
  • granules (G) preferably wet and said bituminous emulsion, to obtain the bitumen / granular association sought.
  • the bituminous emulsion and the aggregates can be brought into contact by mixing or mixing, spreading and compacting.
  • bituminous emulsion is prepared in the following manner: at least one surfactant (TA) is dissolved in an aqueous phase, then the bitumen is added to the aqueous phase and the dispersion of the bitumen is effected by means of energy input. mechanical, for example in a colloid mill or a turbine.
  • TA surfactant
  • the aqueous phase Prior to the incorporation of bitumen, and especially during the dissolution of the surfactant in the aqueous phase, the aqueous phase is heated to a temperature between 20 and 120 ° C, preferably between 40 and 80 ° C and better still between 55 and 65 °.
  • the temperature is chosen substantially equal to 60 ° C.
  • the bituminous emulsion (EB) comprises from 20 to 50 parts by weight of water per 100 parts by weight of bituminous emulsion.
  • the surfactant (TA) is used in an amount of 0.1 to 2.0% by weight based on the amount of emulsion, preferably in an amount of 1.0 to 1.5% by weight.
  • a bituminous emulsion (EB) preferably has the following composition:
  • At least one bitumen from 50 to 80% by weight of emulsion, preferably from 50 to 65% by weight, at least one surfactant (TA) of general formula (I), from 0.1 to 2% by weight; weight of the emulsion, preferably from 1.0 to 1.5% by weight,
  • TA surfactant
  • adjuvants polymer (s), surfactant, fluxing agent, from 0 to 10% by weight of the emulsion,
  • the bitumen intended to be incorporated in the aqueous phase is brought to a temperature of between 80 and 200 ° C., preferably of between 100 and 150 ° C. and more preferably of between 135 and 145 ° C. According to one particular implementation, the temperature is selected close to 140 ° C.
  • bituminous emulsion that is stable over time is thus obtained, as can be measured according to the NF EN 12850 standard. Its bitumen content is between 50 and 65% by weight, preferably between 57 and 62%. in weight.
  • bituminous emulsion can be prepared in a coating plant, at the time of preparation of the bituminous mix, or be prepared and stored before use and then transported, for example by tanker truck, as needed.
  • the bitumen / granulate combination can be prepared in various ways. To prepare a superficial coating, a layer of granulate is then applied and a bituminous emulsion layer, and the assembly is compacted. Those skilled in the art may prepare other types of surface coatings, for example by multiplying the number of layers, by modifying the spreading order of the aggregates and bituminous emulsion layers, according to techniques known elsewhere.
  • Cold bituminous mixes are prepared by mixing (or mixing) previously moistened aggregates and the bituminous emulsion with a suitable mixer. This method of preparation covers cold-cast asphalts and cold mixes.
  • the bitumen / granulate combination for example a bituminous mix, comprises, before breaking, 4 to 20 parts by weight of bituminous emulsion per 100 parts by weight of aggregates.
  • the treatment of the aggregates can advantageously be carried out by a surface treatment agent capable of forming in particular a lipophilic film on the surface of the aggregates.
  • the surface treatment agent is adsorbed on the aggregates and preferably forms a monolayer, which makes it possible in particular to overcome the chemical nature of the aggregates during the preparation of the mix. The characteristics of rupture of the emulsion and cohesion of the asphalt can thus be better controlled.
  • the surface treatment agent is used in the liquid phase, preferably aqueous, during the wetting of aggregates.
  • amino acid compounds polyalkylamphopolycarboxyglycinate, especially tallow-amphopolycarboxyglycinates
  • alkylamines alkylsulfpropylenepolyamine
  • macromolecular surfactant compounds polyoxyethylenepolyalkyletherphosphate, such as polyoxyethyleneolephosphate.
  • the addition in the emulsion of a coalescing agent iavorise the rupture of the emulsion which causes the agglomeration of globules of bitumen in clusters on the aggregates.
  • the coalescing agent is introduced into the bituminous emulsion in the aqueous phase. It is composed, for example, of C 12 to C 14 ethoxylated and propyloxylated amines, of C 8 to C 12 ethoxylated and propyloxylated alcohols, of sodium polyacrylate, of glycol compounds or of antifoaming compounds such as C mineral oils. 20 to 30 with ethoxylated silicone sites or mixtures of silicone oils and silica.
  • the coalescing agent is introduced at a level of at least 0.03% by weight with respect to the aggregates, immediately before mixing them with the emulsion.
  • This coalescence agent is introduced into the bituminous emulsion, preferably in the aqueous phase.
  • adjuvants may also be provided, depending on the properties desired for the bituminous mix.
  • Such adjuvants are known to those skilled in the art. It is for example additional surfactants, pigments, dyes, breaking agents, fluxing agents, polymers, salts, etc.
  • bituminous emulsion After contacting the bituminous emulsion and the aggregates, or simultaneously, it is arranged that the breakage of the bituminous emulsion takes place, so that globules or droplets of bitumen adhere to the aggregates.
  • the rupture takes place during the compaction of the road surface that is being prepared.
  • the breakage of the bituminous emulsion takes place during spreading.
  • the invention relates to the use of at least one nonionic surfactant (TA) of the alkylpolyglycoside type for the preparation of a bituminous emulsion.
  • the invention furthermore relates to the use, as surface coating or bituminous mix, for a cold application of a bitumen / granulate combination, as defined above as such and as a product obtained for the implementation of the preparation process according to the invention.
  • the invention furthermore relates to a bitumen / granulate combination, comprising a bituminous emulsion (EB) prepared using nonionic surfactant (TA) of the alkylpolyglycoside type.
  • Said bitumen / granulate association is eg a surface coating or a bituminous cold mix.
  • the invention also relates to a road surface comprising at least one layer based on a combination bitumen / aggregate defined above, in particular a surface coating, a cold bituminous mix, a cold-poured bituminous mix or a severe -emulsion.
  • bituminous emulsion comprising water as dispersion phase, at least one bitumen, for example as dispersed phase, and at least one nonionic surfactant (TA) of alkylpolyglycoside type.
  • said surfactant comprises a saccharide fraction of 1 to 10 saccharide units, linked by an ether linkage to a C 6 to C 20 aliphatic hydrocarbon fraction, as previously described. It can be a mixture of several types of alkylpolyglucosides, the mixture being provided in the form of an aqueous solution.
  • said surfactant is of the alkylpolyglucoside type and comprises a saccharide fraction of 1 to 6 glucose units, connected to a C8 to C6 linear aliphatic hydrocarbon fraction.
  • said surfactant is in the form of a mixture of alkylpolyglucosides, the saccharide fraction of which has an average degree of polymerization of from 1 to 5, preferably from 1 to 3, and wherein the hydrocarbon fraction comprises linear C8, ClO, Cl 2 and / or C 14 alkyl groups.
  • the surfactants are the agents TA1 and TA2, identified in Table 2 below.
  • the bitumen used is TOTAL 50/70 ED type.
  • the aggregates are of silico-calcareous type Meilleraie (porphyry diorite of siliceous nature, which can be assimilated to a mixture SiO 2 ZCaO 60/40% by weight), of particle size 0/10. It is a G3 type granulate (see Table 2).
  • Surface treatment agents especially hydrophobants, used are a styrene-maleimide copolymer (H).
  • the coalescing agent used is a mixture of fatty amines and amidoamines (STABIRAM ® CM 506, CECA) (Cl) or a solution of calcium chloride (C2).
  • % MA % by weight of active material in the aqueous solution.
  • the water content is equal to the complement of 100% (5)
  • DP Average degree of polymerization of the oligosaccharide fraction
  • Bituminous emulsions are prepared comprising 60% by weight of bitumen relative to the emulsion (ie 600 kg of bitumen per ton of emulsion) and the surfactant dissolved in water, according to the doses indicated in Table 3.
  • the surfactant solution is brought to 60 ° C. before introducing the heated bitumen at a temperature close to 140 ° C.
  • the emulsification is carried out in a colloid mill.
  • bituminous emulsions are measured and reported in Table 4: - sieve deposit of 630 ⁇ m, measured according to the standard NFT 66 016. To do this, a certain quantity of emulsion is passed over a sieve of 630 ⁇ m and collected particles that do not pass through the sieve. This gives an indication of the quality of the emulsion: the lower the particle content, the thinner the emulsion; - bitumen content of the emulsion; - Stability of the emulsion, measured according to standard NF EN 12847 "Storage stability of bitumen emulsions at 7 days".
  • the purpose of this measure is to know the bitumen content at the top and bottom of a specimen containing a bituminous emulsion, after 7 days of storage, in order to evaluate the phenomena of sedimentation and creaming.
  • After preparing the bituminous emulsion it is stored for 7 days in a test tube equipped with two valves, one at the top of the test tube, the other at the bottom.
  • a volume of emulsion (about 300 mL) is taken from the top and bottom of the test tube and the bitumen content of each aliquot is measured. The difference between these levels gives an indication of the stability of the emulsion. The smaller the difference, the more stable the emulsion.
  • bituminous emulsions obtained thus have good characteristics. Indeed, the sieve deposit is particularly low and the stability is quite satisfactory. This means, in particular, that the bitumen is dispersed as fines droplets in the aqueous phase, and that these droplets have little tendency to cluster over time.
  • bituminous mixes A to G were prepared for cold application, according to the proportions indicated in Table 5.
  • the aggregates are Meilleraie type.
  • the bituminous mix is prepared with 6.4 parts by weight of bituminous emulsion per 100 parts by weight of granulate.
  • the mixes A, C and F comprise a coalescing agent; the mixes E and F comprise a surface treatment agent.
  • the mixes B and D do not include a coalescing agent or a surface treatment agent.
  • the mix After mixing the bituminous emulsion and the aggregates, the mix is spread and then compacted, which causes the breaking of the emulsion and the adhesion of the bitumen droplets to the aggregates. The water of rupture is taken for analysis.
  • the compressive strength under different conditions measured according to the DURIEZ test described in standard NF P 98-251-4.
  • the purpose of this DURIEZ test is to determine, for a given temperature and compaction, the water resistance of a hydrocarbon mixture, based on the I / C ratio of the compressive strengths with and without immersion of the asphalt specimens. . This is to evaluate the resistance of the bituminous mix to the stripping.
  • a cylindrical test specimen of 1 kg of asphalt is prepared and packaged according to the indications below.
  • the conditioning begins with 1 day corresponding to the demolding of the test piece, then continues with the maturation under pre-defined conditions of temperature and relative humidity or immersion: Condition 1: After 1 day at room temperature (ie around 20 ° C) plus 6 hours at
  • the compressive strength test is performed under axial compression of the test piece, at a speed of 1 mm / s, until the test piece is broken.
  • the asphalt mixes thus obtained have a good cohesion increase, compatible with rapid re-circulation.
  • the compressive strengths increase rapidly depending on the ripening time. This indicates satisfactory behavior of the asphalt.

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Abstract

The invention concerns a method for preparing a cold process granular material/bitumen combination which consists in: using at least one bitumen emulsion (EB) in aqueous phase, said emulsion further comprising at least one nonionic surfactant (TA) of alkylpolyglycoside type. Said granular material/bitumen combination can lead to various road surfacing compositions, including cold process surface coatings or bituminous mixes broadly speaking. The invention also concerns the use of such a surfactant for preparing a bituminous emulsion. The invention further concerns a bituminous emulsion.

Description

PROCEDE DE PREPARATION D'UN REVETEMENT ROUTIER A FROID PROCESS FOR PREPARING A COLD ROAD COATING
La présente invention concerne la préparation et la fabrication de revêtements routiers à froid, utilisables notamment dans l'industrie routière, par mise en œuvre d'une émulsion de bitume associée à des granulats. L'invention concerne également une nouvelle émulsion bitumineuse comprenant au moins un agent tensioactif non-ionique de type alkylpolyglycoside ainsi que l'association bitume/granulat(s), sous la forme notamment d'enrobés bitumineux, contenant ledit type d'émulsion.The present invention relates to the preparation and manufacture of cold road coatings, used in particular in the road industry, by implementing an emulsion of bitumen associated with aggregates. The invention also relates to a novel bituminous emulsion comprising at least one nonionic surfactant of alkylpolyglycoside type as well as the bitumen / granulate combination (s), in particular in the form of bituminous mixes, containing said type of emulsion.
Le bitume est un produit lourd pouvant provenir de différentes origines. Il peut notamment être obtenu à partir de la fraction la plus visqueuse produite lors de la distillation directe de pétrole brut. La composition du bitume est variable et dépend de l'origine du pétrole brut. Les bitumes comprennent essentiellement des huiles saturées, des huiles aromatiques, des résines, appelées maltènes, et des asphaltènes. Pour plus d'informations à cet égard, on peut utilement se reporter par exemple au brevet européen EP-B-O 246 956.Bitumen is a heavy product that can come from different origins. It can in particular be obtained from the most viscous fraction produced during the direct distillation of crude oil. The composition of the bitumen is variable and depends on the origin of the crude oil. Bitumens consist essentially of saturated oils, aromatic oils, resins, called maltenes, and asphaltenes. For more information in this regard, it is useful to refer for example to the European patent EP-B-0 246 956.
Le bitume est utilisé dans de nombreuses applications routières et/ou industrielles.Bitumen is used in many road and / or industrial applications.
Ainsi, pour les applications routières, on utilise notamment des enrobés bitumineux comme matériaux pour la construction et l'entretien des corps de chaussée et de leur revêtement, ainsi que pour la réalisation de tous travaux de voirie. Les enrobés bitumineux comprennent au moins un liant bitumineux et des granulats.Thus, for road applications, bituminous mixes are used as materials for the construction and maintenance of pavement bodies and their pavement, as well as for carrying out all road works. Bituminous mixes comprise at least one bituminous binder and aggregates.
Cependant, du fait de la viscosité élevée du bitume à température ambiante, sa mise en œuvre est problématique. Plusieurs techniques visant à diminuer la viscosité du bitume ont été développées, afin de résoudre ce problème.However, because of the high viscosity of the bitumen at room temperature, its implementation is problematic. Several techniques to reduce the viscosity of bitumen have been developed to solve this problem.
On classe ainsi les enrobés bitumineux en deux catégories : les enrobés à chaud et les enrobés à froid.Bituminous mixes are classified in two categories: hot mixes and cold mixes.
Dans le cas des enrobés à chaud, le bitume est porté à une température élevée, supérieure à 160°C, ce qui permet de diminuer sa viscosité. Cependant, ces techniques sont fortement consommatrices d'énergie (stockage, transport des bitumes). Elles entraînent en outre une manutention difficile qui oblige à contrôler les différentes étapes pour faciliter les conditions d'application du bitume chaud, porté à des températures élevées.In the case of hot mixes, the bitumen is heated to an elevated temperature of greater than 160 ° C., which makes it possible to reduce its viscosity. However, these techniques consume a lot of energy (storage, transportation of bitumen). They also cause difficult handling which requires control of the various steps to facilitate the application conditions of hot bitumen, raised to high temperatures.
Les enrobés à froid sont réalisés par la mise en émulsion d'un bitume en phase aqueuse, à l'aide d'un agent tensioactif, par apport d'énergie mécanique nécessaire à la dispersion du liant en gouttelettes dans l'eau, puis par malaxage avec les granulats, à des températures plus faibles, de l'ordre de 60°C.The cold mixes are made by emulsifying a bitumen in aqueous phase, with the aid of a surfactant, by supplying mechanical energy necessary for the dispersion of the binder in droplets in water, then by mixing with the aggregates, at lower temperatures, of the order of 60 ° C.
La réalisation d'enrobés à froid fait intervenir plusieurs phénomènes physiques qui conditionnent la bonne adhésion du bitume aux granulats et la stabilité et la cohésion de l'enrobé. Il est essentiel de pouvoir les contrôler, pour conserver à l'enrobé et à l'émulsion une maniabilité compatible avec leur mise en œuvre, notamment pendant le stockage et le transport et pour maintenir les caractéristiques routières des enrobés (résistance mécanique, résistance aux conditions climatiques). L'un des phénomènes physiques considérés est le mouillage des granulats par l'émulsion bitumineuse.The realization of cold mixes involves several physical phenomena that condition the good adhesion of the bitumen to aggregates and the stability and cohesion of asphalt. It is essential to be able to control them, to keep the mix and the emulsion a manageability compatible with their implementation, in particular during the storage and the transport and to maintain the asphalt road characteristics (mechanical resistance, resistance to the conditions climate). One of the physical phenomena considered is the wetting of the aggregates by the bituminous emulsion.
Il a ainsi été proposé d'utiliser divers types de molécules tensioactives, chacune ayant une fonction particulière au cours du procédé de préparation d'un enrobé bitumineux. Il existe de nombreuses solutions commerciales d'émulsions bitumineuses pour applications routières et/ou industrielles, réalisées par exemple à l'aide d'un ou de plusieurs tensioactifs, notamment azotés.It has thus been proposed to use various types of surfactant molecules, each having a particular function during the process for preparing a bituminous mix. There are many commercial solutions of bituminous emulsions for road and / or industrial applications, made for example using one or more surfactants, especially nitrogen.
Lors de la rupture de l'émulsion, les phases aqueuses et bitumineuses se séparent, du fait de la coalescence des gouttelettes de bitume. Une partie de l'eau utilisée pour la préparation de l'émulsion et de l'enrobé bitumineux devient donc libre.When the emulsion breaks, the aqueous and bituminous phases separate, due to the coalescence of the bitumen droplets. Part of the water used for the preparation of the emulsion and the asphalt becomes free.
La demanderesse s'est fixée pour objectif de proposer un nouveau procédé de préparation d'une association bitume/granulat à froid à l'aide d'une émulsion bitumineuse, pour les applications routières, tout en conservant les caractéristiques mécaniques, de résistance aux contraintes thermiques (froid, chaleur), de maniabilité et de maîtrise lors de l'application, atteintes à ce jour. En particulier, un objectif de l'invention est de fournir un nouveau procédé de préparation d'une association bitume/granulat à froid à l'aide d'une émulsion bitumineuse dont les conditions d'applications sont facilitées par rapport aux solutions déjà connues.The applicant has set itself the objective of proposing a new process for preparing a combination bitumen / cold aggregate with a bituminous emulsion, for road applications, while maintaining the mechanical characteristics, resistance to stress thermal (cold, heat), maneuverability and control during application, achieved so far. In particular, an object of the invention is to provide a novel process for preparing a bitumen / cold aggregate combination using a bituminous emulsion whose application conditions are facilitated over previously known solutions.
Un objectif supplémentaire est de proposer un nouveau procédé de préparation d'un enrobé bitumineux, à l'aide d'une émulsion bitumineuse, pour les applications routières, tout en conservant les caractéristiques mécaniques, de résistance aux contraintes thermiques, de maniabilité et de maîtrise lors de l'application, atteintes à ce jour.An additional objective is to propose a new process for the preparation of a bituminous mix, using a bituminous emulsion, for road applications, while retaining the mechanical characteristics, resistance to thermal stress, maneuverability and control. during the application, achieved so far.
Par ailleurs, lors de la rupture de l'émulsion, une partie de l'agent d' émulsion pourrait se retrouver libre dans l'eau de rupture, laquelle est susceptible de s'écouler. Ainsi, un autre objectif de l'invention est de proposer, pour la préparation d'une émulsion bitumineuse comprise dans une association bitume/granulat, l'utilisation d'agents tensioactifs dont l'impact sur l'environnement est réduit (en particulier non étiqueté R50 ni R53 selon la réglementation en vigueur).Moreover, during the rupture of the emulsion, a part of the emulsion agent could become free in the water of rupture, which is likely to flow. Thus, another object of the invention is to propose, for the preparation of a bituminous emulsion included in a bitumen / granulate combination, the use of surfactants whose impact on the environment is reduced (in particular not labeled R50 or R53 according to the regulations in force).
Ces objectifs, parmi d'autres, sont atteints par la présente invention, qui concerne en premier lieu un procédé de préparation d'une association bitume/granulat à froid comprenant :These objectives, among others, are achieved by the present invention, which concerns in the first place a process for preparing a bitumen / cold aggregate combination comprising:
• l'utilisation d'au moins une émulsion (EB) de bitume dans une phase aqueuse, ladite émulsion comprenant au moins un agent tensioactif (TA) de type alkylpolyglycoside, • la mise en contact de ladite émulsion avec des granulats (G).The use of at least one emulsion (EB) of bitumen in an aqueous phase, said emulsion comprising at least one surfactant (TA) of alkylpolyglycoside type, • bringing said emulsion into contact with aggregates (G).
Dans le cadre de l'invention, on entend par "émulsion" une composition d'au moins deux phases liquides comprenant une phase aqueuse -ou phase de dispersion- continue liquide et au moins une phase liquide dispersée sous forme de gouttelettes dans la phase de dispersion. Une émulsion bitumineuse comprend, par exemple, une phase aqueuse et des gouttelettes ou globules de bitumes, dispersées dans la phase aqueuse. Il s'agit alors d'une émulsion de type huile-dans-1'eau.In the context of the invention, the term "emulsion" means a composition of at least two liquid phases comprising an aqueous phase -or continuous liquid dispersion phase and at least one liquid phase dispersed in the form of droplets in the dispersion. A bituminous emulsion comprises, for example, an aqueous phase and droplets or globules of bitumen, dispersed in the aqueous phase. It is then an oil-in-water emulsion.
Une association bitume/granulat à froid peut servir de base à l'élaboration de divers revêtements routiers : couche de roulement, couche de liaison et couche de base. Une couche de roulement est un revêtement routier superficiel de la structure de la chaussée, sur lequel s'exercent directement les agressions du trafic et du climat. On distingue parmi les couches de roulement, les enduits superficiels, les enrobés à froid et les enrobés coulés à froid, qui résultent de la mise en œuvre de techniques différentes connues de l'homme du métier. Une couche de liaison est un revêtement routier, situé dans la structure de la chaussée à une position intermédiaire entre une couche de roulement et une couche de base. Une couche de base est un revêtement routier qui constitue une assise de la chaussée. Une couche de liaison et une couche de base peuvent être constituées par exemple d'un enrobé à froid ou d'une grave-émulsion.A bitumen / cold aggregate association can serve as a basis for the development of various road surfaces: wearing course, tie layer and base course. A wearing course is a superficial road surface covering the structure of the road surface, which is directly affected by traffic and climate aggression. Among the wearing courses, superficial coatings, cold mixes and cold-cast asphalts, which result from the implementation of different techniques known to those skilled in the art, are distinguished. A tie layer is a road surface, located in the pavement structure at an intermediate position between a wearing course and a base course. A base layer is a road surface that is a foundation of the roadway. A bonding layer and a base layer may consist for example of a cold mix or a serious-emulsion.
Dans le cadre de l'invention, on désigne indifféremment par "enrobé à froid" ou par "enrobé bitumineux à froid", un enrobé bitumineux à froid au sens strict (BBDF), un enrobé bitumineux coulé à froid (ECF) et une grave-émulsion (pouvant notamment être fabriquée à température ambiante? dans une centrale de malaxage fixe ou mobile? et répandue également à température ambiante).In the context of the invention, the term "cold mix" or "cold bituminous mix" is used interchangeably to mean a cold bituminous mix in the strict sense (BBDF), a cold-poured bituminous mix (ECF) and a severe emulsion (which can especially be manufactured at room temperature in a stationary or mobile mixing plant and also spread at room temperature).
Lors de la préparation des enrobés bitumineux à froid, la mise en contact de l'émulsion bitumineuse et des granulats est réalisée par malaxage ou mélange. Dans le cas des enduits superficiels, la mise en contact de l'émulsion bitumineuse et des granulats est réalisée par épandage de l'émulsion et des granulats puis compactage.During the preparation of cold bituminous mixes, the bitumen emulsion is brought into contact with the aggregates by mixing or mixing. In the case of surface coatings, the contact between the bituminous emulsion and the aggregates is carried out by spreading the emulsion and granules and compacting them.
Ainsi, l'invention concerne également un procédé de préparation d'un enrobé bitumineux à froid comprenant :Thus, the invention also relates to a process for preparing a cold bituminous mix comprising:
• l'utilisation d'au moins une émulsion (EB) de bitume dans une phase aqueuse, ladite émulsion comprenant en outre au moins un agent tensioactif (TA) de type alkylpolyglycoside,The use of at least one emulsion (EB) of bitumen in an aqueous phase, said emulsion further comprising at least one surfactant (TA) of alkylpolyglycoside type,
• le mélange de ladite émulsion à des granulats (G). Pour les besoins de la présente invention, on définit les alkylpolyglycosides de la façon suivante. Ce sont des molécules comprenant une fraction saccharidique de 1 à 10 unités saccharidiques, reliée par une liaison éther à une fraction hydrocarbonée en C6 à C20. La fraction saccharidique possède des propriétés hydrophiles, tandis que la fraction hydrocarbonée possède des propriétés hydrophobes. Les alkylpolyglycosides constituent une famille d'agents tensioactifs non-ioniques particulièrement intéressante pour leurs propriétés et car les matières premières utilisées pour leur fabrication proviennent de la biomasse. Le procédé de fabrication des alkylpolyglycosides est largement décrit dans la littérature scientifique. En ce qui concerne la fraction saccharidique, on se reportera avantageusement aux recommandations (1996) de l'IUPAC (Internation Union of Pure and Applied Chemistry) relatives à la nomenclature des hydrates de carbone. Selon l'invention, les unités saccharidiques comprennent de 3 (triose) à 7 (heptose) atomes de carbone, de préférence de 5 (pentose) à 6 (hexose) atomes de carbone. Avantageusement, il s'agit d'arabinose, de xylose, de glucose, de mannose, de galactose et/ou de fructose, mais d'autres pentoses et/ou hexoses sont également envisageables. Les unités saccharidiques se trouvent sous forme cyclique hémiacétal (dans le cas d'un aldose) ou hémicétal (dans le cas d'un cétose), de préférence sous forme furan (cycle de 5 atomes) et/ou pyran (cycle de 6 atomes).• mixing said emulsion with aggregates (G). For the purposes of the present invention, the alkylpolyglycosides are defined as follows. These are molecules comprising a saccharide fraction of 1 to 10 saccharide units, linked by an ether linkage to a C6 to C20 hydrocarbon fraction. The saccharide fraction has hydrophilic properties, while the hydrocarbon fraction has hydrophobic properties. Alkylpolyglycosides are a family of nonionic surfactants particularly interesting for their properties and because the raw materials used for their manufacture come from biomass. The process for producing alkylpolyglycosides is widely described in the scientific literature. With regard to the saccharide fraction, reference is made to the recommendations (1996) of IUPAC (International Union of Pure and Applied Chemistry) relating to the nomenclature of carbohydrates. According to the invention, the saccharide units comprise from 3 (triose) to 7 (heptose) carbon atoms, preferably from 5 (pentose) to 6 (hexose) carbon atoms. Advantageously, it is arabinose, xylose, glucose, mannose, galactose and / or fructose, but other pentoses and / or hexoses are also possible. The saccharide units are in hemiacetal (in the case of an aldose) or hemiketal (in the case of ketosis) cyclic form, preferably in the form of furan (5-atom ring) and / or pyran (6-atom ring) ).
Dans les unités saccharidiques, il est possible de remplacer une fonction alcool -OH par une fonction aminé -NH2 ou par une fonction thiol -SH. Eventuellement, le(s) atomes d'hydrogène des fonctions alcool et/ou aminé et/ou thiol peuvent être remplacés par un (des) groupe(s) alkyle(s) en Cl à C4.In the saccharide units, it is possible to replace an alcohol function -OH with an amino function -NH 2 or with a thiol function -SH. Optionally, the hydrogen atom (s) of the alcohol and / or amine and / or thiol functions may be replaced by a Cl-C4 alkyl group (s).
De préférence, la fraction saccharidique comprend de 1 à 10 unités et mieux encore 1, 2 ou 3 unités jusqu'à 6 unités. Il peut, par exemple, s'agir, outre les pentoses et hexoses cités ci-dessus, de saccharose, de maltose, de lactose, de cellobiose, de tréhalose, de raffinose, de cellotriose et/ou de panose. Les fractions saccharidiques constituées d'unités glucoses sont plus particulièrement préférées. L'agent tensioactif (TA) est alors un alkylpolyglucoside (APG).Preferably, the saccharide moiety comprises from 1 to 10 units and more preferably 1, 2 or 3 units up to 6 units. It may, for example, be, in addition to the pentoses and hexoses mentioned above, sucrose, maltose, lactose, cellobiose, trehalose, raffinose, cellotriose and / or panose. Saccharide fractions consisting of glucose units are more particularly preferred. The surfactant (TA) is then an alkylpolyglucoside (APG).
La fraction hydrocarbonée est un groupe aliphatique saturé ou insaturé, linéaire ou ramifié, comprenant de 6 à 20 atomes de carbones, et mieux encore, 8, 10, 12, 14 ou 16 atomes de carbone. Avantageusement, la fraction hydrocarbonée dérive d'un alcool gras linéaire saturé, tel que l'alcool caprylylique (C8), caprylique (ClO), laurylique (C12), myristique (C 14), palmitique (C 16) ou stéarique (Cl 8).The hydrocarbon fraction is a saturated or unsaturated, linear or branched aliphatic group comprising from 6 to 20 carbon atoms, and more preferably, 8, 10, 12, 14 or 16 carbon atoms. Advantageously, the hydrocarbon fraction is derived from a saturated linear fatty alcohol, such as caprylyl (C8), caprylic (ClO), lauryl (C12), myristic (C14), palmitic (C16) or stearic (Cl8) alcohol. ).
L'agent tensioactif est présent, de préférence, sous la forme d'un mélange de plusieurs alkylpolyglycosides variables au niveau de la fraction saccharidique et/ou au niveau de la fraction hydrocarbonée. Avantageusement, dans un tel mélange, par exemple un mélange d'APG, la fraction saccharidique présente un degré de polymérisation moyen de 1 à 5, de préférence de 1 à 3, et mieux encore proche de 1,5.The surfactant is preferably present in the form of a mixture of several variable alkylpolyglycosides at the level of the saccharide fraction and / or at the level of the hydrocarbon fraction. Advantageously, in such a mixture, for example a mixture of APG, the saccharide fraction has an average degree of polymerization of 1 to 5, preferably 1 to 3, and more preferably close to 1.5.
Dans le mélange d'agents tensioactifs mis en œuvre selon l'invention, la fraction hydrocarbonée comprend de préférence des groupes alkyles linéaires en C8, ClO, Cl 2 et/ou C14.In the surfactant mixture used according to the invention, the hydrocarbon fraction preferably comprises linear C8, ClO, Cl 2 and / or C14 alkyl groups.
A titre indicatif, le pH d'une solution aqueuse d'un mélange d'alkylpolyglycosides à lOg/L, peut être notamment supérieur à 10 et vaut de préférence de 11 à 13, et mieux encore, de 11,5 à 12,5. On peut ajuster le pH de la solution aqueuse d'alkylpolyglycosideBy way of indication, the pH of an aqueous solution of a mixture of alkylpolyglycosides at 10 g / l may in particular be greater than 10 and is preferably from 11 to 13, and more preferably from 11.5 to 12.5. . The pH of the aqueous alkylpolyglycoside solution can be adjusted
(éventuellement en mélange) en fonction des caractéristiques des alkylpolyglycosides utilisés, pour aboutir à une mise en émulsion du bitume satisfaisante.(optionally mixed) depending on the characteristics of the alkylpolyglycosides used, to result in emulsification of the satisfactory bitumen.
Pour la préparation d'une émulsion bitumineuse, l'agent tensioactif (ou le mélange d'agents tensioactifs) est apporté, par exemple, sous la forme d'une solution aqueuse comportant au moins 25% en poids d'agent tensioactif alkylpolyglycoside dans la solution.For the preparation of a bituminous emulsion, the surfactant (or the surfactant mixture) is provided, for example, in the form of an aqueous solution comprising at least 25% by weight of alkylpolyglycoside surfactant in the solution.
De préférence, ce pourcentage pondéral est au moins égal à 50% et inférieur à 70% en poids.Preferably, this weight percentage is at least 50% and less than 70% by weight.
Les alkylpolyglycosides, et plus particulièrement les alkylpolyglucosides, sont des produits disponibles commercialement, notamment auprès des sociétés Cognis, AkzoAlkylpolyglycosides, and more particularly alkylpolyglucosides, are commercially available products, in particular from Cognis, Akzo
Nobel ou BASF. A titre d'exemples, on citera les agents tensioactifs suivants : GLUCOPONNobel or BASF. By way of examples, mention may be made of the following surfactants: GLUCOPON
650 EC (Cognis), GLUCOPON 215 es (Cognis), AG 6210 (Akzo Nobel), LUTENSOL GD70 (BASF).650 EC (Cognis), GLUCOPON 215 es (Cognis), AG 6210 (Akzo Nobel), LUTENSOL GD70 (BASF).
Dans le procédé selon l'invention, on utilise préférentiellement comme agent tensioactif un mélange d'alkylpolyglucosides de degré de polymérisation moyen sensiblement égal à 1,5 et dont la fraction hydrocarbonée est en C8 à ClO, et/ou en C8 à C14. Du point de vue de la biodégradabilité, ces agents tensioactifs sont classésIn the process according to the invention, a mixture of alkylpolyglucosides of average degree of polymerization substantially equal to 1.5 and whose hydrocarbon fraction is C8 to C10 and / or C8 to C14 is preferably used as surfactant. From the point of view of biodegradability, these surfactants are classified
« facilement biodégradables » selon la législation allemande en vigueur. De plus, aucun d'entre eux n'est classé R50 ou R53."Easily biodegradable" according to the German legislation in force. In addition, none of them is rated R50 or R53.
Le bitume utilisé est choisi parmi les bitumes naturels, les bitumes de distillation ou les bitumes synthétiques ou leurs mélanges. Ces bitumes peuvent être utilisés purs, fluxés, et/ou modifiés par au moins un polymère. On peut notamment distinguer les bitumes purs, les bitumes fluidifiés, les bitumes fluxés, les bitumes oxydés et les bitumes polymères.The bitumen used is chosen from natural bitumens, distillation bitumens or synthetic bitumens or mixtures thereof. These bitumens can be used pure, fluxed, and / or modified with at least one polymer. In particular, it is possible to distinguish pure bitumens, fluidized bitumens, fluxed bitumens, oxidized bitumens and polymer bitumens.
Un bitume naturel est un mélange naturel de bitume et de fines minérales. Un bitume de distillation est obtenu à partir de la fraction la plus visqueuse produite lors de la distillation directe de pétrole brut. D'autres techniques physico-chimiques telles que le désasphaltage au solvant et le soufflage permettent d'obtenir des bitumes synthétiques.A natural bitumen is a natural blend of bitumen and mineral fines. A distillation bitumen is obtained from the most viscous fraction produced during the direct distillation of crude oil. Other physicochemical techniques such as solvent deasphalting and blowing make it possible to obtain synthetic bitumens.
Les bitumes fluxés sont des compositions de bitume(s) obtenues à partir de bitumes purs dont on a abaissé la viscosité par addition de solvants volatils. Traditionnellement, les bitumes fluxés sont obtenus par mélange, par exemple à 150°C, d'une part, de liant bitumineux, et d'autre part, de fluxant. De manière générale, on connaît les fluxants d'origine pétrolière et les fluxants végétaux.Fluxed bitumens are compositions of bitumen (s) obtained from pure bitumens, the viscosity of which has been lowered by the addition of volatile solvents. Traditionally, fluxed bitumens are obtained by mixing, for example at 150 ° C, on the one hand, bituminous binder, and on the other hand, fluxing. In general, petroleum fluxes and plant fluxes are known.
Les bitumes fluidifiés sont obtenus par mélange de liants bitumineux avec des huiles carbochimiques ou pétrolières. Les bitumes fluxés diffèrent des bitumes fluidifiés, en particulier par la courbe de distillation de leurs fluxants, plus étendue vers le haut essentiellement, mais on considérera dans la suite de l'exposé que les termes "fluidifié" etThe fluidized bitumens are obtained by mixing bituminous binders with carbochemical or petroleum oils. Fluxed bitumens differ from fluidized bitumens, in particular by the distillation curve of their fluxes, more essentially upwards, but it will be considered in the rest of the description that the terms "fluidized" and
"fluxé" sont synonymes."fluxed" are synonymous.
Les bitumes modifiés sont obtenus en mélangeant à une composition de bitume(s) au moins un composé de type polymère, en vue d'améliorer ses performances mécaniques et thermiques. Pour modifier le bitume, on peut utiliser un polymère choisi notamment parmi :The modified bitumens are obtained by mixing with a bitumen composition (s) at least one polymer-type compound, in order to improve its mechanical and thermal performance. To modify the bitumen, it is possible to use a polymer chosen in particular from:
- les homopolymères et copolymères oléfiniques d'éthylène, propylène, butylène, hexène, 4-méthyl-l-pentène, - les élastomères tels que l'éthylène propylène diène monomère (EPDM), l'éthylène propylène monomère (EPM), le polyisobutylène, le polybutadiène, le polyisoprène,olefinic homopolymers and copolymers of ethylene, propylene, butylene, hexene, 4-methyl-1-pentene, elastomers such as ethylene propylene diene monomer (EPDM), ethylene propylene monomer (EPM), polyisobutylene polybutadiene, polyisoprene,
- les élastomères thermoplastiques comme les copolymères statistiques ou séquences de styrène et de butadiène, linéaire ou en étoile (SBR, SBS) ou de styrène et d'isoprène (SIS), éventuellement réticulés, - le poly(chlorure de vinyle),thermoplastic elastomers, such as random or styrene and butadiene random or styrene or block copolymers (SBR, SBS) or styrene and isoprene (SIS) copolymers, optionally crosslinked, polyvinyl chloride,
- les copolymères d'éthylène et d'acétate de vinyle, etcopolymers of ethylene and vinyl acetate, and
- leurs mélanges.- their mixtures.
Les granulats utilisés sont des granulats routiers, répondant aux normes pertinentes : NF EN 13043 "Granulats pour mélanges hydrocarbonés et pour enduits superficiels utilisés dans la construction des chaussées, aérodromes et autres zones de circulation" en Europe, ASTM C33 "Standard spécification for concrète Aggregates" auxThe aggregates used are road aggregates, meeting the relevant standards: NF EN 13043 "Aggregates for hydrocarbon mixtures and for surface coatings used in the construction of pavements, airfields and other traffic areas" in Europe, ASTM C33 "Standard Specification for Concrete Aggregates " to the
Etats-Unis d'Amérique.United States of America.
On distingue diverses qualités de granulats, par exemple en fonction de la taille des grains, de leur acidité au sens pétrographique, c'est-à-dire de leur teneur en silice, ou encore de la présence d'une phase vitreuse ou non. Des granulats représentatifs et leur acidité pétrographique sont listés dans le tableau 1 ci-dessous. Tableau 1 - Exemples de granulats routiersThere are various grades of aggregates, for example depending on the size of grains, their acidity in the petrographic sense, that is to say, their silica content, or the presence of a glassy phase or not. Representative aggregates and their petrographic acidity are listed in Table 1 below. Table 1 - Examples of Road Aggregates
Nature Acidité pétrographique pétrographique(1) Nature Petrographic Petrographic Acidity (1)
Gl Quartzite TSGl Quartzite TS
G2 Calcaire UBG2 UB Limestone
G3 Diorite BG3 Diorite B
G4 Basalte BG4 Basalt B
G5 Rhyolite AG5 Rhyolite A
G6 Amphibolite BG6 Amphibolite B
G7 Gneiss AG7 Gneiss A
G8 Granité AG8 Granite A
(1) TS granulats très siliceux ; A granulats silicates acides > 65 % SiO2 ; I granulats silicates intermédiaires SiO2 entre 52 et 65 % ; B granulats silicates basiques SiO2 entre 42 et 52 % ; UB granulats calcaire ultrabasique SiO2 < 42 %. (1) TS very siliceous aggregates; With silicate acidic aggregates> 65% SiO 2 ; SiO 2 intermediate silicate aggregates between 52 and 65%; B basic silicate granules SiO 2 between 42 and 52%; UB ultrabasic limestone aggregates SiO 2 <42%.
Selon l'invention, pour préparer une association bitume/granulat à froid, par exemple un enrobé bitumineux à froid, on commence par préparer une émulsion (EB) de bitume dans une phase aqueuse, en utilisant un agent tensioactif (TA) pour faciliter la mise en émulsion du bitume. On aboutit à une émulsion de type huile-dans-1'eau. Puis on met en contact des granulats (G) de préférence humides et ladite émulsion bitumineuse, pour obtenir l'association bitume/granulat recherchée. La mise en contact de l'émulsion bitumineuse et des granulats peut être réalisée par malaxage ou mélange, épandage et compactage.According to the invention, in order to prepare a cold bitumen / granulate combination, for example a cold bituminous mix, an emulsion (EB) of bitumen is initially prepared in an aqueous phase, using a surfactant (TA) to facilitate the emulsification of the bitumen. The result is an oil-in-water emulsion. Then contacting granules (G) preferably wet and said bituminous emulsion, to obtain the bitumen / granular association sought. The bituminous emulsion and the aggregates can be brought into contact by mixing or mixing, spreading and compacting.
L'émulsion bitumineuse (EB) est préparée de la façon suivante : on dissout au moins un agent tensioactif (TA) dans une phase aqueuse, puis on ajoute le bitume à la phase aqueuse et on réalise la dispersion du bitume par apport d'énergie mécanique, par exemple dans un moulin colloïdal ou une turbine.The bituminous emulsion (EB) is prepared in the following manner: at least one surfactant (TA) is dissolved in an aqueous phase, then the bitumen is added to the aqueous phase and the dispersion of the bitumen is effected by means of energy input. mechanical, for example in a colloid mill or a turbine.
Préalablement à l'incorporation de bitume, et notamment pendant la dissolution de l'agent tensioactif dans la phase aqueuse, on chauffe la phase aqueuse à une température comprise entre 20 et 120°C, de préférence entre 40 et 80°C et mieux encore entre 55 et 65°. Avantageusement, la température est choisie sensiblement égale à 60°C.Prior to the incorporation of bitumen, and especially during the dissolution of the surfactant in the aqueous phase, the aqueous phase is heated to a temperature between 20 and 120 ° C, preferably between 40 and 80 ° C and better still between 55 and 65 °. Advantageously, the temperature is chosen substantially equal to 60 ° C.
Selon l'invention, l'émulsion bitumineuse (EB) comprend de 20 à 50 parties en poids d'eau pour 100 parties en poids d'émulsion bitumineuse. L'agent tensioactif (TA) est utilisé en une quantité de 0,1 à 2,0 % en poids par rapport à la quantité d'émulsion, de préférence en une quantité de 1,0 à 1,5 % en poids. En d'autres termes, une émulsion bitumineuse (EB) présente, de préférence, la composition suivante :According to the invention, the bituminous emulsion (EB) comprises from 20 to 50 parts by weight of water per 100 parts by weight of bituminous emulsion. The surfactant (TA) is used in an amount of 0.1 to 2.0% by weight based on the amount of emulsion, preferably in an amount of 1.0 to 1.5% by weight. In other words, a bituminous emulsion (EB) preferably has the following composition:
- au moins un bitume, de 50 à 80 % en poids de Fémulsion, de préférence de 50 à 65 % en poids, - au moins un agent tensioactif (TA) de formule générale (I), de 0,1 à 2 % en poids de l'émulsion, de préférence de 1,0 à 1,5 % en poids,at least one bitumen, from 50 to 80% by weight of emulsion, preferably from 50 to 65% by weight, at least one surfactant (TA) of general formula (I), from 0.1 to 2% by weight; weight of the emulsion, preferably from 1.0 to 1.5% by weight,
- éventuellement d'autres adjuvants (polymère(s), agent tensioactif, fluxant...), de 0 à 10 % en poids de l'émulsion,optionally other adjuvants (polymer (s), surfactant, fluxing agent), from 0 to 10% by weight of the emulsion,
- de l'eau en quantité suffisante pour compléter à 100 % en poids. De préférence, le bitume destiné à être incorporé dans la phase aqueuse, est porté à une température comprise entre 80 et 200°C, de préférence comprise entre 100 et 150°C et plus préférentiellement encore, entre 135 et 145°C. Selon une mise en œuvre particulière, la température est sélectionnée proche de 140°C.- water in sufficient quantity to complete 100% by weight. Preferably, the bitumen intended to be incorporated in the aqueous phase is brought to a temperature of between 80 and 200 ° C., preferably of between 100 and 150 ° C. and more preferably of between 135 and 145 ° C. According to one particular implementation, the temperature is selected close to 140 ° C.
On obtient ainsi une émulsion bitumineuse (EB) stable au cours du temps, comme cela peut être mesuré conformément à la norme NF EN 12850. Sa teneur en bitume, est comprise entre 50 et 65 % en poids, de préférence entre 57 et 62 % en poids.A bituminous emulsion (EB) that is stable over time is thus obtained, as can be measured according to the NF EN 12850 standard. Its bitumen content is between 50 and 65% by weight, preferably between 57 and 62%. in weight.
L'émulsion bitumineuse (EB) peut être préparée dans une usine d'enrobage, au moment de la préparation de l'enrobé bitumineux, ou bien être préparée et stockée avant utilisation puis transportée, par camion citerne par exemple, en fonction des besoins.The bituminous emulsion (EB) can be prepared in a coating plant, at the time of preparation of the bituminous mix, or be prepared and stored before use and then transported, for example by tanker truck, as needed.
L'association bitume/granulat peut être préparée de diverses façons. Pour préparer un enduit superficiel, on épand une couche de granulat puis une couche d'émulsion bitumineuse, et on compacte l'ensemble. L'homme du métier pourra préparer d'autres types d'enduits superficiels, par exemple en multipliant le nombre de couches, en modifiant l'ordre d'épandage des couches de granulats et d'émulsion bitumineuse, selon des techniques connues par ailleurs. En ce qui concerne les enrobés bitumineux à froid, on les prépare en malaxant (ou mélangeant) des granulats préalablement humidifiés et l'émulsion bitumineuse, à l'aide d'un malaxeur approprié. Ce mode de préparation couvre les enrobés coulés à froid et les enrobés à froid. Avantageusement, l'association bitume/granulat, par exemple un enrobé bitumineux, comprend, avant rupture, 4 à 20 parties en poids d'émulsion bitumineuse pour 100 parties en poids de granulats.The bitumen / granulate combination can be prepared in various ways. To prepare a superficial coating, a layer of granulate is then applied and a bituminous emulsion layer, and the assembly is compacted. Those skilled in the art may prepare other types of surface coatings, for example by multiplying the number of layers, by modifying the spreading order of the aggregates and bituminous emulsion layers, according to techniques known elsewhere. Cold bituminous mixes are prepared by mixing (or mixing) previously moistened aggregates and the bituminous emulsion with a suitable mixer. This method of preparation covers cold-cast asphalts and cold mixes. Advantageously, the bitumen / granulate combination, for example a bituminous mix, comprises, before breaking, 4 to 20 parts by weight of bituminous emulsion per 100 parts by weight of aggregates.
Préalablement à la mise en contact de ladite émulsion et desdits granulats, par exemple par malaxage, on peut avantageusement procéder au traitement des granulats par un agent de traitement de surface apte à former notamment un film lipophile à la surface des granulats. L'agent de traitement de surface s'adsorbe sur les granulats et forme de préférence une monocouche, ce qui permet en particulier de s'affranchir de la nature chimique des granulats lors de la préparation de l'enrobé. Les caractéristiques de rupture de l'émulsion et de cohésion de l'enrobé peuvent ainsi être mieux contrôlées. L'agent de traitement de surface est utilisé en phase liquide, de préférence aqueuse, lors du mouillage des granulats. Il est constitué de préférence, de composés aminoacides (polyalkylamphopolycarboxy- glycinate, notamment des suif-amphopolycarboxyglycinates) ou alkylamines (alkylsuif- polypropylènepolyamine), de composés "water repellent", ou de composés tensioactifs macromoléculaires (polyoxyéthylènepolyalkylétherphosphate, tel que du polyoxyéthylène oléyl étherphosphate) .Prior to bringing said emulsion into contact with said granulates, for example by kneading, the treatment of the aggregates can advantageously be carried out by a surface treatment agent capable of forming in particular a lipophilic film on the surface of the aggregates. The surface treatment agent is adsorbed on the aggregates and preferably forms a monolayer, which makes it possible in particular to overcome the chemical nature of the aggregates during the preparation of the mix. The characteristics of rupture of the emulsion and cohesion of the asphalt can thus be better controlled. The surface treatment agent is used in the liquid phase, preferably aqueous, during the wetting of aggregates. It is preferably composed of amino acid compounds (polyalkylamphopolycarboxyglycinate, especially tallow-amphopolycarboxyglycinates) or alkylamines (alkylsulfpropylenepolyamine), "water repellent" compounds, or macromolecular surfactant compounds (polyoxyethylenepolyalkyletherphosphate, such as polyoxyethyleneolephosphate). .
Puis on peut introduire un agent de coalescence, avant ou après ladite mise en contact, afin de contrôler la rupture de l'émulsion.Then it is possible to introduce a coalescence agent, before or after said contacting, in order to control the rupture of the emulsion.
L'ajout dans l'émulsion d'un agent de coalescence iàvorise la rupture de l'émulsion ce qui entraîne l'agglomération des globules de bitume en amas, sur les granulats. L'agent de coalescence est introduit dans l'émulsion bitumineuse, en phase aqueuse. Il est composé par exemple d'aminés éthoxylées et propyloxylées en C12 à C14, d'alcools éthoxylés et propyloxylés en C8 à C12, de polyacrylate de sodium, de composés glycoliques ou de composés antimousse tels que les huiles minérales en C20 à C30 avec des sites silicones éthoxylés ou des mélanges d'huiles silicones et de silice. De préférence, l'agent de coalescence est introduit au taux d'au moins 0,03% en poids par rapport aux granulats, immédiatement avant leur mélange avec l'émulsion. Cet agent de coalescence est introduit dans l'émulsion bitumineuse, de préférence en phase aqueuse.The addition in the emulsion of a coalescing agent iavorise the rupture of the emulsion which causes the agglomeration of globules of bitumen in clusters on the aggregates. The coalescing agent is introduced into the bituminous emulsion in the aqueous phase. It is composed, for example, of C 12 to C 14 ethoxylated and propyloxylated amines, of C 8 to C 12 ethoxylated and propyloxylated alcohols, of sodium polyacrylate, of glycol compounds or of antifoaming compounds such as C mineral oils. 20 to 30 with ethoxylated silicone sites or mixtures of silicone oils and silica. Preferably, the coalescing agent is introduced at a level of at least 0.03% by weight with respect to the aggregates, immediately before mixing them with the emulsion. This coalescence agent is introduced into the bituminous emulsion, preferably in the aqueous phase.
D'autres adjuvants peuvent également être prévus, en fonction des propriétés recherchées pour l'enrobé bitumineux. De tels adjuvants sont connus de l'homme du métier. Il s'agit par exemple de tensioactifs supplémentaires, de pigments, de colorants, d'agents de rupture, de fluxants, de polymères, de sels etc.Other adjuvants may also be provided, depending on the properties desired for the bituminous mix. Such adjuvants are known to those skilled in the art. It is for example additional surfactants, pigments, dyes, breaking agents, fluxing agents, polymers, salts, etc.
Après la mise en contact de l'émulsion bitumineuse et des granulats, ou de façon simultanée, on fait en sorte que la rupture de l'émulsion bitumineuse ait lieu, de sorte que les globules ou gouttelettes de bitumes adhèrent aux granulats. Dans le cas des enrobés bitumineux à froid au sens strict et des enduits superficiels, la rupture a lieu lors du compactage du revêtement routier que l'on prépare. Dans le cas des enrobés bitumineux coulés à froid, la rupture de l'émulsion bitumineuse se déroule lors de l'épandage.After contacting the bituminous emulsion and the aggregates, or simultaneously, it is arranged that the breakage of the bituminous emulsion takes place, so that globules or droplets of bitumen adhere to the aggregates. In the case of cold bituminous mixes in the strict sense and superficial coatings, the rupture takes place during the compaction of the road surface that is being prepared. In the case of cold-poured bituminous mixes, the breakage of the bituminous emulsion takes place during spreading.
Selon un autre de ses aspects, l'invention est relative à l'utilisation d'au moins un agent tensioactif non ionique (TA) du type alkylpolyglycoside pour la préparation d'une émulsion bitumineuse. L'invention concerne par ailleurs l'utilisation, à titre d'enduit superficiel ou d'enrobé bitumineux, pour une application à froid, d'une association bitume/granulat, telle que définie ci-dessus en tant que telle et en tant que produit obtenu pour la mise en œuvre du procédé de préparation, conformément à l'invention. L'invention concerne en outre une association bitume/granulat, comprenant une émulsion bitumineuse (EB) préparée en utilisant en agent tensioactif non ionique (TA) de type alkylpolyglycoside. Ladite association bitume/granulat est e.g un enduit superficiel ou un enrobé bitumineux à froid.According to another of its aspects, the invention relates to the use of at least one nonionic surfactant (TA) of the alkylpolyglycoside type for the preparation of a bituminous emulsion. The invention furthermore relates to the use, as surface coating or bituminous mix, for a cold application of a bitumen / granulate combination, as defined above as such and as a product obtained for the implementation of the preparation process according to the invention. The invention furthermore relates to a bitumen / granulate combination, comprising a bituminous emulsion (EB) prepared using nonionic surfactant (TA) of the alkylpolyglycoside type. Said bitumen / granulate association is eg a surface coating or a bituminous cold mix.
L'invention a également trait à un revêtement routier comprenant au moins une couche à base d'une association bitume/granulat définie ci-dessus, en particulier un enduit superficiel, un enrobé bitumineux à froid, un enrobé bitumineux coulé à froid ou une grave-émulsion.The invention also relates to a road surface comprising at least one layer based on a combination bitumen / aggregate defined above, in particular a surface coating, a cold bituminous mix, a cold-poured bituminous mix or a severe -emulsion.
Enfin, l'invention est relative à une émulsion bitumineuse (EB) comprenant de l'eau comme phase de dispersion, au moins un bitume, par exemple, comme phase dispersée, et au moins un agent tensioactif non ionique (TA) de type alkylpolyglycoside.Finally, the invention relates to a bituminous emulsion (EB) comprising water as dispersion phase, at least one bitumen, for example as dispersed phase, and at least one nonionic surfactant (TA) of alkylpolyglycoside type. .
Plus particulièrement, ledit agent tensioactif comprend une fraction saccharidique de 1 à 10 unités saccharidiques, reliée par une liaison éther à une fraction hydrocarbonée aliphatique en C6 à C20, ainsi qu'il a été décrit précédemment. Il peut s'agir d'un mélange de plusieurs types d'alkylpolyglucosides, le mélange étant apporté sous la forme d'une solution aqueuse.More particularly, said surfactant comprises a saccharide fraction of 1 to 10 saccharide units, linked by an ether linkage to a C 6 to C 20 aliphatic hydrocarbon fraction, as previously described. It can be a mixture of several types of alkylpolyglucosides, the mixture being provided in the form of an aqueous solution.
De préférence, ledit agent tensioactif est de type alkylpolyglucoside et comprend une fraction saccharidique de 1 à 6 unités glucose, reliée à une fraction hydrocarbonée aliphatique linéaire en C8 à Cl 6. Avantageusement ledit agent tensioactif se présente sous la forme d'un mélange d'alkylpolyglucosides dont la fraction saccharidique présente un degré de polymérisation moyen de 1 à 5, de préférence de 1 à 3, et dont la fraction hydrocarbonée comprend des groupes alkyles linéaires en C8, ClO, Cl 2 et/ou C 14.Preferably, said surfactant is of the alkylpolyglucoside type and comprises a saccharide fraction of 1 to 6 glucose units, connected to a C8 to C6 linear aliphatic hydrocarbon fraction. Advantageously, said surfactant is in the form of a mixture of alkylpolyglucosides, the saccharide fraction of which has an average degree of polymerization of from 1 to 5, preferably from 1 to 3, and wherein the hydrocarbon fraction comprises linear C8, ClO, Cl 2 and / or C 14 alkyl groups.
L'invention va maintenant être illustrée par les exemples suivants, qui n'ont pas vocation à en limiter la portée. EXEMPLES DE PREPARATION D'ENROBES A FROIDThe invention will now be illustrated by the following examples, which are not intended to limit the scope. EXAMPLES OF COLD COATING PREPARATION
Produits mis en oeuvreProducts implemented
Les agents tensioactifs sont les agents TAl et TA 2, identifiés dans le tableau 2 ci- après. Le bitume utilisé est de type TOTAL 50/70 ED.The surfactants are the agents TA1 and TA2, identified in Table 2 below. The bitumen used is TOTAL 50/70 ED type.
Les granulats sont de type silico-calcaire Meilleraie (diorite porphyrique de nature siliceuse, pouvant être assimilée à un mélange SiO2ZCaO 60/40 % en poids), de granulométrie 0/10. Il s'agit d'un granulat de type G3 (voir tableau 2).The aggregates are of silico-calcareous type Meilleraie (porphyry diorite of siliceous nature, which can be assimilated to a mixture SiO 2 ZCaO 60/40% by weight), of particle size 0/10. It is a G3 type granulate (see Table 2).
Les agents de traitement de surface, notamment les hydrophobants, utilisés sont un copolymère styrène-maléimide (H). L'agent de coalescence utilisé est un mélange d'aminés grasses et d'amidoamines (STABIRAM® CM 506, CECA) (Cl) ou une solution de chlorure de calcium (C2).Surface treatment agents, especially hydrophobants, used are a styrene-maleimide copolymer (H). The coalescing agent used is a mixture of fatty amines and amidoamines (STABIRAM ® CM 506, CECA) (Cl) or a solution of calcium chloride (C2).
Tableau 2Table 2
Chaîne Viscosité (2) Densité (3) %MA DP pH (1) grasse (mPa.s) (g/cm3) (4) (5)Chain Viscosity (2) Density (3) % MA DP pH (1) Fat (mPa.s) (g / cm 3 ) (4) (5)
TA 1 (COGNIS)TA 1 (COGNIS)
C8-C14 11 ,5-12,5 (40 0C) 500-1500 (40 0C) 1,13-1,14 50-53 1,5C8-C14 11.5-12.5 (40 ° C.) 500-1500 (40 ° C.) 1.13-1.14 50-53 1.5
GLUCOPONΘ 650 ECGLUCOPON Θ 650 EC
TA 2 (COGNIS) (20 0C) 1500-3000TA 2 (COGNIS) (20 0 C) 1500-3000
C8-C10 11 ,5-12,5 (40 0C) 1,07-1,08 62-65 1,5C8-C10 11.5-12.5 (40 ° C) 1.07-1.08 62-65 1.5
GLUCOPON® 215 CS (400C) 600-1200 (1) pH : solution aqueuse à lOg/LGLUCOPON ® 215 CS (40 0 C) 600-1200 (1) pH: aqueous solution at 10 g / L
(2) Viscosité : DIN53015 (Hôppler) (2) Viscosity: DIN53015 (Hoppler)
(3) Densité : DIN51757 (3) Density: DIN51757
(4) %MA : % en poids de matière active dans la solution aqueuse. Le contenu en eau est égal au complément à 100% (5) DP : Degré de polymérisation moyen de la fraction oligosaccharidique (4) % MA:% by weight of active material in the aqueous solution. The water content is equal to the complement of 100% (5) DP: Average degree of polymerization of the oligosaccharide fraction
Préparation des émulsions bitumineusesPreparation of bituminous emulsions
On prépare des émulsions bitumineuses comprenant 60 % en poids de bitume rapport à l'émulsion (soit 600 kg de bitume par tonne d'émulsion) et l'agent tensioactif dissous dans de l'eau, selon les doses indiquées dans le tableau 3. La solution d'agent tensioactif est portée à 60 °C avant d'y introduire le bitume chauffé à une température proche de 140 °C. La mise en émulsion est réalisée dans un moulin colloïdal. Tableau 3 - Préparation d'émulsions bitumineusesBituminous emulsions are prepared comprising 60% by weight of bitumen relative to the emulsion (ie 600 kg of bitumen per ton of emulsion) and the surfactant dissolved in water, according to the doses indicated in Table 3. The surfactant solution is brought to 60 ° C. before introducing the heated bitumen at a temperature close to 140 ° C. The emulsification is carried out in a colloid mill. Table 3 - Preparation of bitumen emulsions
Figure imgf000013_0001
Figure imgf000013_0001
Diverses caractéristiques des émulsions bitumineuses sont mesurées et reportées dans le tableau 4 : - dépôt sur tamis de 630 μm, mesuré selon la norme NFT 66 016. On fait passer pour cela une certaine quantité d' emulsion sur un tamis de 630 μm et on recueille les particules qui ne passent pas à travers le tamis. Cela donne une indication de la qualité de l'émulsion : plus la teneur en particules est faible plus l'émulsion est fine ; - teneur en bitume de l'émulsion ; - stabilité de l'émulsion, mesurée selon la norme NF EN 12847 "Stabilité au stockage des émulsions de bitume à 7 jours". Le but de cette mesure est de connaître la teneur en bitume en haut et en bas d'une éprouvette contenant une emulsion bitumineuse, après 7 jours de stockage, afin d'évaluer les phénomènes de sédimentation et de crémage. Après avoir préparé l'émulsion bitumineuse, on la stocke pendant 7 jours dans une éprouvette munie de deux robinets, l'un en haut de l'éprouvette, l'autre en bas. Puis on prélève un volume d'émulsion (environ 300 mL) en haut et en bas de l'éprouvette et on mesure la teneur en bitume de chaque aliquote. La différence entre ces teneurs donne une indication de la stabilité de l'émulsion. Plus la différence est réduite, plus l'émulsion est stable.Various characteristics of the bituminous emulsions are measured and reported in Table 4: - sieve deposit of 630 μm, measured according to the standard NFT 66 016. To do this, a certain quantity of emulsion is passed over a sieve of 630 μm and collected particles that do not pass through the sieve. This gives an indication of the quality of the emulsion: the lower the particle content, the thinner the emulsion; - bitumen content of the emulsion; - Stability of the emulsion, measured according to standard NF EN 12847 "Storage stability of bitumen emulsions at 7 days". The purpose of this measure is to know the bitumen content at the top and bottom of a specimen containing a bituminous emulsion, after 7 days of storage, in order to evaluate the phenomena of sedimentation and creaming. After preparing the bituminous emulsion, it is stored for 7 days in a test tube equipped with two valves, one at the top of the test tube, the other at the bottom. Then a volume of emulsion (about 300 mL) is taken from the top and bottom of the test tube and the bitumen content of each aliquot is measured. The difference between these levels gives an indication of the stability of the emulsion. The smaller the difference, the more stable the emulsion.
Tableau 4 - Propriété des émulsions bitumineuses ré aréesTable 4 - Property of Refined Bituminous Emulsions
Figure imgf000013_0002
Figure imgf000013_0002
Les émulsions bitumineuses obtenues présentent ainsi de bonnes caractéristiques. En effet, le dépôt sur tamis est particulièrement faible et la stabilité est tout à fait satisfaisante. Cela signifie, en particulier, que le bitume est dispersé sous forme de fines gouttelettes dans la phase aqueuse, et que ces gouttelettes ont peu tendance à se regrouper au cours du temps.The bituminous emulsions obtained thus have good characteristics. Indeed, the sieve deposit is particularly low and the stability is quite satisfactory. This means, in particular, that the bitumen is dispersed as fines droplets in the aqueous phase, and that these droplets have little tendency to cluster over time.
Préparation des enrobés bitumineux A partir des émulsions obtenues dans les essais 1 à 4 décrits ci-dessus, on a préparé des enrobés bitumineux A a G pour une application à froid, selon les proportions indiquées dans le tableau 5.Preparation of bituminous mixes From the emulsions obtained in the tests 1 to 4 described above, bituminous mixes A to G were prepared for cold application, according to the proportions indicated in Table 5.
Les granulats sont de type Meilleraie. L'enrobé bitumineux est préparé avec 6,4 parties en poids d'émulsion bitumineuse pour 100 parties en poids de granulat. Les enrobés A, C et F comprennent un agent de coalescence ; les enrobés E et F comprennent un agent de traitement de surface. Les enrobés B et D ne comprennent ni agent de coalescence ni agent de traitement de surface.The aggregates are Meilleraie type. The bituminous mix is prepared with 6.4 parts by weight of bituminous emulsion per 100 parts by weight of granulate. The mixes A, C and F comprise a coalescing agent; the mixes E and F comprise a surface treatment agent. The mixes B and D do not include a coalescing agent or a surface treatment agent.
Après malaxage de l'émulsion bitumineuse et des granulats, l'enrobé est épandu puis compacté, ce qui provoque la rupture de l'émulsion et l'adhésion des gouttelettes de bitume aux granulats. L'eau de rupture est prélevée pour analyse.After mixing the bituminous emulsion and the aggregates, the mix is spread and then compacted, which causes the breaking of the emulsion and the adhesion of the bitumen droplets to the aggregates. The water of rupture is taken for analysis.
Différentes caractéristiques des enrobés formulés à froid sont mesurées. Les résultats sont reportés dans le tableau 5. En particulier, il s'agit de :Different characteristics of cold formulated mixes are measured. The results are reported in Table 5. In particular, these are:
- la quantité d'eau dans l'enrobé après fabrication, après compactage et après 24h à 18°C sous 50 % d'humidité relative (HR) ;the quantity of water in the mix after manufacture, after compacting and after 24 hours at 18 ° C. at 50% relative humidity (RH);
- la teneur en extrait sec de l'eau de rupture (% en poids). Cette mesure est une indication de la qualité de l'émulsion. Une teneur en extrait sec de l'eau de rupture élevée indique que les gouttelettes de bitume n'ont pas adhéré correctement aux granulats à la suite de la rupture de l'émulsion. Une teneur réduite indique une moindre quantité de bitume non adhérent aux granulats, et donc une émulsion de bonne qualité ;- the solids content of the water of rupture (% by weight). This measurement is an indication of the quality of the emulsion. A dry solids content of the high water of rupture indicates that the bitumen droplets did not adhere properly to the aggregates as a result of the breakage of the emulsion. A reduced content indicates a lesser amount of bitumen not adherent to the aggregates, and therefore a good quality emulsion;
- l'adhésivité passive, mesurée selon la norme NFT 66 018 ;passive adhesiveness, measured according to standard NFT 66 018;
- la résistance à la compression sous différentes conditions, mesurée suivant l'essai DURIEZ décrit dans la norme NF P 98-251-4. Cet essai DURIEZ a pour but de déterminer, pour une température et un compactage donnés, la tenue à l'eau d'un mélange hydrocarboné, à partir du rapport I/C des résistances à la compression avec et sans immersion des éprouvettes d'enrobés. Il s'agit d'évaluer la résistance de l'enrobé bitumineux au désenrobage.the compressive strength under different conditions, measured according to the DURIEZ test described in standard NF P 98-251-4. The purpose of this DURIEZ test is to determine, for a given temperature and compaction, the water resistance of a hydrocarbon mixture, based on the I / C ratio of the compressive strengths with and without immersion of the asphalt specimens. . This is to evaluate the resistance of the bituminous mix to the stripping.
Pour cet essai, on iàbrique une éprouvette cylindrique de 1 kg d'enrobé que l'on conditionne selon les indications ci-dessous. Le conditionnement commence par 1 jour correspondant au démoulage de l'éprouvette, puis se poursuit par la maturation dans des conditions de température et d'humidité relative prédéfinies ou en immersion : Condition 1 : après 1 jour à température ambiante (soit environ 20°C) plus 6 heures àFor this test, a cylindrical test specimen of 1 kg of asphalt is prepared and packaged according to the indications below. The conditioning begins with 1 day corresponding to the demolding of the test piece, then continues with the maturation under pre-defined conditions of temperature and relative humidity or immersion: Condition 1: After 1 day at room temperature (ie around 20 ° C) plus 6 hours at
18 °C sous 50 % d'humidité relative Condition 2 "AIR" C : après 8 jours, dont 7 jours à 18 °C sous 50 % d'humidité relative, à l'air libre Condition 3 "EAU" I : après 8 jours, dont 7 jours à 18 °C en immersion dans l'eau18 ° C at 50% relative humidity Condition 2 "AIR" C: after 8 days, including 7 days at 18 ° C at 50% relative humidity, in the open air Condition 3 "WATER" I: after 8 days, including 7 days at 18 ° C immersed in water
Le test de résistance à la compression est réalisé sous une compression axiale de l'éprouvette, à une vitesse de 1 mm/s, jusqu'à rupture de l'éprouvette.The compressive strength test is performed under axial compression of the test piece, at a speed of 1 mm / s, until the test piece is broken.
Les enrobés ainsi obtenus présentent une bonne montée en cohésion, compatible avec une remise sous trafic rapide. Les résistances à la compression augmentent rapidement en fonction du temps de maturation. Ceci indique un comportement satisfaisant de l'enrobé.The asphalt mixes thus obtained have a good cohesion increase, compatible with rapid re-circulation. The compressive strengths increase rapidly depending on the ripening time. This indicates satisfactory behavior of the asphalt.
Les rapports I/C sont au moins équivalents à ceux d'autres enrobés à froidI / C ratios are at least equivalent to those of other cold mixes
Tableau 5 - Pro riété des enrobésTable 5 - Pro riety of asphalt
Figure imgf000015_0001
Figure imgf000015_0001
(1) Teneur en agent de traitement de surface dans la solution aqueuse (% poids) (1) Surface treatment agent content in the aqueous solution (% by weight)
(2) Teneur en agent de coalescence dans la solution aqueuse (% poids) (2) Content of coalescing agent in the aqueous solution (% by weight)

Claims

REVENDICATIONS
1. Procédé de préparation d'une association bitume/granulat à froid comprenant :A process for preparing a bitumen / cold aggregate combination comprising:
• l'utilisation d'au moins une émulsion (EB) de bitume dans une phase aqueuse, ladite émulsion comprenant au moins un agent tensioactif non-ionique (TA) de type alkylpolyglycoside,The use of at least one emulsion (EB) of bitumen in an aqueous phase, said emulsion comprising at least one nonionic surfactant (TA) of alkylpolyglycoside type,
• la mise en contact de ladite émulsion avec des granulats (G).• bringing said emulsion into contact with aggregates (G).
2. Procédé selon la revendication précédente, dans lequel ledit agent tensioactif comprend une fraction saccharidique de 1 à 10 unités saccharidiques, reliée par une liaison éther à une fraction hydrocarbonée aliphatique en C6 à C20.2. Method according to the preceding claim, wherein said surfactant comprises a saccharide fraction of 1 to 10 saccharide units, linked by an ether linkage to a C6 to C20 aliphatic hydrocarbon fraction.
3. Procédé selon l'une quelconque des revendications précédentes, dans lequel ledit agent tensioactif est de type alkylpolyglucoside, comprenant une fraction saccharidique de 1 à 6 unités glucose, reliée à une fraction hydrocarbonée aliphatique linéaire en C8 à Cl 6.3. Method according to any one of the preceding claims, wherein said surfactant is of alkylpolyglucoside type, comprising a saccharide fraction of 1 to 6 glucose units, connected to a linear aliphatic hydrocarbon fraction C8 to Cl6.
4. Procédé selon la revendication précédente, dans lequel ledit agent tensioactif se présente sous la forme d'un mélange d'alkylpolyglucosides, dont la fraction saccharidique présente un degré de polymérisation moyen de 1 à 5, de préférence de 1 à 3, et dont la fraction hydrocarbonée comprend des groupes alkyles linéaires en C8, ClO, C12 et/ou C14.4. Method according to the preceding claim, wherein said surfactant is in the form of a mixture of alkylpolyglucosides, the saccharide fraction has an average degree of polymerization of 1 to 5, preferably 1 to 3, and the hydrocarbon fraction comprises linear C8, ClO, C12 and / or C14 alkyl groups.
5. Procédé selon l'une quelconque des revendications précédentes, dans lequel ledit agent tensioactif est utilisé en une quantité de 0,1 % à 2,0 % en poids rapporté à la quantité d'émulsion utilisée, de préférence de 1,0 à 1,8 % en poids et mieux encore, près de 1,5 % en poids.The process according to any one of the preceding claims, wherein said surfactant is used in an amount of from 0.1% to 2.0% by weight based on the amount of emulsion used, preferably from 1.0 to 1.8% by weight and better still, nearly 1.5% by weight.
6. Procédé selon l'une quelconque des revendications précédentes, dans lequel ladite émulsion comprend de 20 à 50 parties en poids d'eau pour 100 parties en poids d'émulsion bitumineuse.The method of any of the preceding claims, wherein said emulsion comprises from 20 to 50 parts by weight of water per 100 parts by weight of bituminous emulsion.
7. Procédé selon l'une quelconque des revendications précédentes, dans lequel ledit agent tensioactif est apporté en solution aqueuse.7. Process according to any one of the preceding claims, wherein said surfactant is provided in aqueous solution.
8. Procédé selon l'une quelconque des revendications précédentes, dans lequel préalablement à la mise en contact de ladite émulsion et desdits granulats, on procède au traitement des granulats par un agent de traitement de surface apte à former un film lipophile à la surface des granulats. 8. Method according to any one of the preceding claims, wherein prior to contacting said emulsion and said aggregates, the granules are treated with a surface treatment agent capable of forming a lipophilic film on the surface of the granules. aggregates.
9. Utilisation pour la préparation d'une émulsion bitumineuse, d'au moins un agent tensioactif non ionique (TA) de type alkylpolyglycoside.9. Use for the preparation of a bituminous emulsion, at least one nonionic surfactant (TA) of alkylpolyglycoside type.
10. Utilisation d'une association bitume/granulat obtenue par la mise en œuvre d'un procédé selon l'une quelconque des revendications 1 à 8 ou comprenant une émulsion bitumineuse préparée selon la revendication 9, à titre d'enduit superficiel ou d'enrobé bitumineux, pour une application à froid.10. Use of a combination bitumen / aggregate obtained by the implementation of a process according to any one of claims 1 to 8 or comprising a bituminous emulsion prepared according to claim 9, as a surface coating or bituminous mix, for cold application.
11. Revêtement routier comprenant au moins une couche à base d'une association bitume/granulat selon la revendication précédente.11. Roadway comprising at least one layer based on a bitumen / aggregate combination according to the preceding claim.
12. Emulsion bitumineuse (EB) comprenant de l'eau, au moins un bitume et au moins un agent tensioactif non ionique (TA) de type alkylpolyglycoside.12. Bituminous emulsion (EB) comprising water, at least one bitumen and at least one nonionic surfactant (TA) of alkylpolyglycoside type.
13. Emulsion bitumineuse selon la revendication précédente, dans lequel ledit agent tensioactif comprend une fraction saccharidique de 1 à 10 unités saccharidiques, reliée par une liaison éther à une fraction hydrocarbonée aliphatique en C6 à C20.13. Bituminous emulsion according to the preceding claim, wherein said surfactant comprises a saccharide fraction of 1 to 10 saccharide units, linked by an ether linkage to a C6 to C20 aliphatic hydrocarbon fraction.
14. Emulsion bitumineuse selon l'une quelconque des revendications 12 à 13, dans lequel ledit agent tensioactif est de type alkylpolyglucoside, comprenant une fraction saccharidique de 1 à 6 unités glucose, reliée à une fraction hydrocarbonée aliphatique linéaire, comprenant en C8 à Cl 6.A bituminous emulsion according to any one of claims 12 to 13, wherein said surfactant is of the alkylpolyglucoside type, comprising a saccharide fraction of 1 to 6 glucose units, connected to a linear aliphatic hydrocarbon fraction, comprising C8 to Cl6. .
15. Emulsion bitumineuse selon l'une quelconque des revendications 12 à 14, dans lequel ledit agent tensioactif se présente sous la forme d'un mélange d'alkylpolyglucosides, dont la fraction saccharidique présente un degré de polymérisation moyen de 1 à 5, de préférence de 1 à 3, et dont la fraction hydrocarbonée comprend des groupes alkyles linéaires en C8, ClO, C12 et/ou C 14. A bituminous emulsion according to any one of claims 12 to 14, wherein said surfactant is in the form of a mixture of alkylpolyglucosides, the saccharide fraction of which has an average degree of polymerization of from 1 to 5, preferably from 1 to 3, and wherein the hydrocarbon fraction comprises linear C8, ClO, C12 and / or C14 alkyl groups.
PCT/EP2005/053726 2004-07-30 2005-07-29 Method for preparing a cold process road surfacing composition WO2006013194A1 (en)

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FR0408479 2004-07-30
FR0408479A FR2873708B1 (en) 2004-07-30 2004-07-30 PROCESS FOR PREPARING A COLD ROAD COATING

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