FR2765229A1 - New clear or bituminous binders in a subdivided solid form at ambient temperature - Google Patents

Abstract

A new clear or bituminous binder for the preparation of highway coatings, asphalt flows nd sealed membranes, having the following properties :- -a penetrability at 25 deg C. of less than 50 1/10 mm(preferably less than 35 1/10 mm) (NFT 66 -OO4); -a softening point greater than 70 deg C.(preferably 80 deg C.)(NFT 66-008) ; -a dynamic viscosity (180 deg C.) less than 1000 mPa.s.(preferably less than 500, and more preferably 300). Also claimed is the composition and preparation of the solid particles and their use.

Description

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  The present invention relates to new clear or bituminous binders capable of being present in the solid state subdivided at ambient temperature as well as particles of binders, in particular granules and pellets. These binders are mainly intended for the manufacture of coatings, mixes, mastic asphalts or waterproofing membranes, by incorporation

  direct production units for these products.

  Because of their double action on the reinforcement of safety and the improvement of the living environment, colored coatings find multiple applications, most often in urban areas, in particular for the realization of cycle tracks, pedestrian zones, sidewalks, car parks, playgrounds, places,

bus lanes, crossroads.

  These mixes consist of mixtures of aggregates and binders of light shades, colored by incorporation of pigments (metallic oxides in general). The selection of clear materials makes it possible to obtain bright colors and to significantly reduce the cost of the mix by minimizing the quantity of pigment

  necessary to obtain the desired coloring.

  Therefore, the binders of choice for these applications are synthetic binders obtained by the mixture of oils, resins, waxes and polymers. Unlike bitumens which come from the distillation of crude oil, synthetic binders have the ability to be easily colorable because they do not contain asphaltenes. It is, in fact, the asphaltenes naturally present in the bitumens which give them a black coloring and therefore make them

difficult to color.

  The clear binders available on the market are in liquid form either hot in the case of anhydrous binder, or cold when the binder is in aqueous emulsion. In both cases, the product in liquid form has a limited stability over time, which prevents the product from being stored and therefore requires it to be made to order. The liquid state of the binder creates logistical constraints both in terms of product management and in terms of

Implementation.

  From a logistical point of view, the product is offered in bulk, given the relatively large volumes generally required for the realization of

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  construction sites. Packaging in barrels or containers would entail very high handling costs. However, the bulk delivery method has the disadvantage that the quantities delivered are dependent on the tonnages of production capacity and delivery tanks, and therefore do not necessarily correspond to the quantity useful for the site. Excess unused product is often lost because it cannot be stored for a long time without risk

of degradation.

  In terms of implementation, it is essential to avoid contamination of the binder with any product likely to change its color, such as bitumen. Thus, the transport and storage tanks, the manufacturing and processing units and the transfer lines must either be assigned to clear binders, or perfectly cleaned in case they are also used for bitumens. Similar storage problems arise

  also in the case of bituminous type binders.

  The present invention provides a solution to all the problems set out above by providing binders which, due to their physical and rheological characteristics, lend themselves to shaping in the subdivided state for direct use in the asphalt coating units or mixers. Preferred compositions of binders have been identified. This technology is of particular interest in the case of clear binders since, unlike the products currently on the market, they offer the following advantages * Storage of the binder can be done for an extended period (at least several months to 1 year) at temperature ambient, energy saving, and under simple shelter from the weather, which allows

  avoid using intermediate storage capacities.

  * The binder can be packaged in bags which can contain, for example, from kg to 1000 kg of product, which makes it possible to detail the quantity of binder

  strictly necessary for the user to carry out his work.

  * Due to the packaging of the binder, transport, storage and handling are particularly simple. Thus, the solid state of the binder makes it possible to avoid affecting or having to clean up the equipment when these operations would be essential for the

bulk liquid binders.

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  The solid form of the binder allows it to be pre-additive into fines without the risk of settling. The binder can be premixed during its manufacture with part or all of the fillers (limestone, talc) and / or colored pigments (metal oxides) incorporated during the manufacture of the mixes or asphalts. The advantages of going through a premix are on the one hand to reinforce the resistance of the binder during storage and on the other hand to promote the homogeneity of the mastic (mixture of binders + fines) normally

  formed during the aggregation coating operation.

  * The state of the binder allows its implementation according to an original process since it can be incorporated in the form of solid granules directly in the mixer for mixes or poured asphalts. The rate of addition is generally between 4% to 10% of the mass of the minerals (aggregates, sands and fines). In the case where the granules consist of a premix of binder and fines (limestone, talc, metal oxides, ...), the rate of addition of the granules is adjusted according to the precise content of binder which composes them . The quantity of filler fines normally incorporated during the manufacture of the asphalt or asphalt

  must then be reduced by the quantity of fines present in the granules.

  Thus, the invention relates to binders having specific properties allowing access for the first time to binders in the form of solid subdivided in the solid state, which has, as we have seen

  previously considerable progress compared to binders of the prior art.

  More precisely, according to one of these essential characteristics, the invention relates to a clear or bituminous binder, in particular intended for the manufacture of road mixes or mastic asphalts having the following properties: -penetrability at 25 C less than 50 1 / 10 mm, measured according to standard NFT 66-004, - softening point above 70 C, measured according to standard

NFT 66-008,

  - dynamic viscosity at 180 C less than 1000 mPa.s.

  According to particularly advantageous variants, the following will be chosen: - a penetration lower than 35 1/10 mm, - a softening point higher than 80 C and preferably higher than 90 C,

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  -a dynamic viscosity less than 500 mPa.s and preferably

less than 300 mPa.s.

  According to a particularly advantageous variant, the binder will also have a viscosity at 130 C of less than 2500 mPa.s and preferably less than 1500 mPa.s. According to a particularly advantageous variant of the invention, these binders contain from 3 to 40% by weight of at least one wax, hereinafter called HF wax

  with a melting point above 90 C.

  Such waxes are synthetic waxes which can be obtained by

chemical synthesis.

  According to a first advantageous variant of the invention, the HF wax will be a hydrocarbon wax obtained by polymerization, or copolymerization

  C2 to C6 olefins, preferably of the ethylene, propene or hexene type.

  Such waxes will then be in the form of N-alkanes or hydro-

branched carbides.

  According to another particularly advantageous variant of the invention, the HF wax will be chosen from among the amide type waxes resulting from the reaction of a

  carboxylic acid or a mixture of carboxylic acid with a diamine.

  Among these products, the products corresponding to formula (1) below will be chosen in a particularly advantageous manner: o o R '- Cx //, C-R "(1)

NH-RF-NH

  in which: R'l and R "1 are identical or different and each represent a hydrocarbon group comprising 4 to 20 carbon atoms, optionally hydroxylated, saturated or unsaturated, linear or branched, aliphatic or aromatic, R2 is an alkylaliphatic hydrocarbon group or aromatic including

  from 2 to 6 carbon atoms, preferably an ethylene group.

  An example of a particularly preferred product in this family is the synthetic wax resulting from the action of stearic acid on ethylene diamine which leads to the formation of N, N'-ethylene-bis-stearamide of formula (2)

0 0,

H3C- (CH2) 16 C C- (CH2) 16CH3 (2)

NH- (CH2) 2 NH

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  with a melting point of 143 C and a penetration of

  1/10 mm at 25 C measured according to ASTM D1321.

  Another particularly interesting wax according to the invention is p N, N'-phenylene-bis-stearamide obtained by reaction of stearic acid with p-phenylene-bis-stearamide. This wax has a melting point of 167 C and a

9 1/10 mm penetration.

  All of these synthetic waxes are distinguished from natural waxes from petroleum refining, also called microcrystalline waxes, essentially by higher melting points, more precisely by melting points.

higher than 90 C.

  These waxes also advantageously have relatively low molecular weights (typically from 400 to 3000), which leads to viscosities in the molten state (measured according to the ASTM D 3226 method).

  also weak, typically below 150 cP at 149 C.

  Preferably, these waxes have a molecular mass of between 500

  and 2000 and a viscosity of less than 50cP, more preferably less than 20cP.

  The clear binders of the invention will advantageously have the following composition, in which the proportions are indicated in percentages by weight: Oils 40-90 Waxes * + Resins 10-40 including HF wax 3-40 and preferably 5-40 Polymers 0- 25 Various additives 0-5 * by waxes, all the waxes are therefore included including HF waxes (from

  melting above 100 C) and other waxes (melting point below 90 C).

  In these compositions, the oils, the waxes with a melting point below 90 ° C., the resins, the polymers and the additives are those

  conventionally used in the manufacture of clear binders.

  More specifically: * In the clear binder compositions according to the invention, the petroleum oil used may be any type of oil conventionally used in clear binders. It may, in particular, be a paraffinic oil. of an oil

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  naphthenic or aromatic of petroleum origin. We will preferably choose a

  oil from a heavy petroleum cut.

  This oil will advantageously have a viscosity at 40 C greater than cSt or mnm2 / s (measured according to standard ASTM D 445) and greater than 30 cSt at

100 C.

  This viscosity will advantageously be chosen greater than 500 cSt at C. The polymers included in the clear binder compositions of the invention are also those conventionally used in clear binders. They may in particular be plastomers or elastomers making it possible to modulate

  the physical or rheological properties of the compositions of the invention.

  As polymers of the plastomer type which can be used in the compositions of the invention, non-limiting mention will be made of copolymers of ethylene and vinyl acetate (EVA), copolymers of ethylene and of

  methylacrylate (EMA), polyethylene (PE) or polypropylene (PP).

  As elastomeric polymers, mention will be made of styrene butadiene styrene (SBS) block copolymers, styrene and butadiene (SB) copolymers,

polyisobutylene (PIB).

  The compositions of the invention may, in addition, contain waxes other than HF waxes, in particular microcrystalline waxes resulting from the refining of crude petroleum conventionally used in the field as well as resins. The compositions of the invention also advantageously contain an agent intended to improve the adhesiveness of the binder. This agent

  could be any agent conventionally used for this purpose.

  The bituminous binders of the invention will advantageously correspond to the following compositions expressed in percentages by weight Bitumens 20-95 HF wax (s) 3-40, preferably 5-40 Resin (s) 0-40 Polymer (s) 0-75 Various additives and / or fillers 0-5 The components of these bituminous binder compositions are those

  conventionally used in the intended uses (asphalt or mastic asphalt).

  These bituminous type binders may, in particular, contain resins or polymers which are those conventionally used for the preparation of bitumens modified with polymers, for example EVA, EMA, SB, SBS, PIB. The advantages of clear or bituminous binders are summarized below.

  the invention linked to the presence of wax with a high melting point in their composition.

  Adding such a wax to a bituminous or synthetic binder has the following effects on its characteristics:

  * Decreased penetrability, which leads to hardening.

  * Strong increase in the softening point, which improves their resistance to deformation at high temperature and leads to

  increased penetration index.

  * Decrease in viscosity at high temperature (T> 120 C).

  This results in the following advantages in application.

  All these clear or bituminous binders may also contain a filler. The filler content will then be such that it will represent from 0 to 50% in

weight of the loaded binder.

  The binders described above prove to be particularly advantageous because of their specific properties which give them a certain ability to be formed into solid particles at room temperature, in particular under

form of granules or pellets.

  Thus, because of their characteristics, these binders are very particularly intended to be used by direct introduction in the solid state into a mix. More specifically, their particular characteristics give them, in addition to the general properties of the binders, specific properties such as an ability to be in the form of granules or pellets, good storage stability against mass recovery and sufficient workability.

during implementation.

  According to another of its characteristics, the invention relates to a process for preparing a binder in the form of pellets. Such a method comprises a step of draining a binder as described above on a cooled plate. According to another characteristic, the invention also relates to a process for preparing a binder in the form of granules. This method comprises a step of extruding and granulating a composition of binders as it has

previously defined.

  As will become apparent from the description which follows, these two forms

  Preferred solid state binders subdivided at room temperature are made possible due to the characteristics presented by these binders. The shaping in the state of pellets requires, in fact, to be able to drain the binder easily when hot without however reaching temperatures above 180 ° C. which can rapidly degrade the properties of the binder. In practice, this condition is satisfied when the dynamic viscosity of the binder is less than 3000 mPa.s at 180 C. Preferably, the pelletizing temperature

  is defined for a viscosity of the binder close to 2000 mPa.s.

  To obtain granules, the binder at the outlet of the extrusion die must be cooled until it has a rigidity allowing it to be cut. This condition is generally encountered when the binder is brought to a temperature at least 20 C below its softening point. Cooling being done in practice with water at room temperature, the binder has

  advantageously a softening point of at least 70 C.

  To ensure the stability of the binder during storage, it must have a high rigidity (needle penetration at 25 C less than 50 1/10 mm and preferably less than 35 1/10 mm - Method NFT 66-004) , as well as an ability to resist softening at high storage temperatures (Ball and Ring softening point greater than 70 C, and preferably greater than

   C, preferably still greater than 90 C - (Method NF T 66-008).

  The ease of coating the aggregates with the binder introduced cold in the coating plant directly depends on the ability of this binder to melt (it is advantageous to use grains with a mass of less than 1 g, preferably with a mass of 0 , 03 g and 0.3 g) and its fluidity / wettability properties after

  melting (dynamic viscosity of the binder at 180 C less than 1000 mPa.s.

  This viscosity at 180 ° C. will preferably be less than 500 mPa.s, more preferably less than 300 mPa.s and preferably less than 2500 and

even at 1500 mPa.s at 130 C.

  The incorporation of a wax with a high melting point (HF wax) has the advantage of promoting the required conditions since it makes it possible both to decrease the viscosity, to increase the softening point and to decrease the

penetrability.

  The binder can be produced according to various methods including the

  production of the mixture and its shaping.

  According to a first variant, the manufacture of the mixture can be done

  according to a conventional mode by mixing.

  This mixture is thus advantageously prepared by: * dispersing the polymers in oil at 160 ° C.-180 ° C. with vigorous stirring for a period generally of 1 hour to 2 hours * reduction of the heating to 130 ° C.-150 ° C. and addition of waxes and resins and

  possibly dopes of adhesiveness. This operation generally lasts-

  about lh * possible incorporation of fines and pigments at the end of mixing

 C-150 C with moderate stirring.

  The mixture thus produced is then subjected to a step intended to put it in the form of solid particles at room temperature, in particular in

  using extrusion or tableting techniques.

  According to another variant, the manufacture of particles of binders in the solid state can also be done according to an original extrusion process or else according to a mixed kneading / extrusion process: According to the extrusion process, the constituents solid at room temperature of the binder are mixed at the inlet of the extruder, the oil is injected online at a sufficiently high temperature (100-180 C) to promote its association with the molten compounds, typically 160 C and under overpressure relative to the internal pressure in the extrusion cylinder. The shearing of the products during extrusion makes it possible to obtain a homogeneous paste at the outlet of

the extrusion unit.

  According to a mixed process, a mother mixture containing the oils, waxes, resins and optionally adhesive dopes is produced with stirring at a temperature advantageously of the order of 150 C. The mixture is then introduced into the extruder with the polymers and powdery fillers so

  to obtain a homogeneous mixture at the output.

  Two techniques have proven to be particularly advantageous for preparing solid grains of binder according to the invention. These are granulation extrusion techniques to prepare granules with dimensions advantageously between 1 and 10 mm in length and 2 and 6 mm in diameter and pelletizing to prepare pellets with dimensions between 7 and

  17 mm in diameter and between 2 and 5 mm thick.

  According to extrusion-granulation techniques, the binder is extruded through a die, cooled by jet or water bath and cut into granules by means of a rotary knife. The granules are dried by centrifugation or

  ventilation then packaged in bags.

  The dimensions of the granules are adjusted by acting on the extrusion rate, the geometry of the nozzle at the outlet of the extrusion die and the speed of

rotation of the rotary knife.

  According to tableting techniques, the liquid binder at 140 ° C. is deposited in the form of droplets on a mobile metal plate cooled by circulation of water on its lower surface. The droplets freeze in the form of pellets which are detached from the plate to be directly bagged. Such

  Pelletizing is advantageously carried out on a band of the Rotoform Sandvick type.

EXAMPLES

Example 1

  Manufacture of a binder in the state of pellets on industrial units A). Preparation of the binder A binder is prepared containing, expressed in parts by weight: - 58.0 parts of an aromatic type oil having a viscosity at 1 00 C greater than 30 cSt, and at 40 C greater than 500 cSt, -10.5 parts of polymer granules consisting of an ethylene-vinyl acetate copolymer (EVA) having a Melt Flow Index of 20, - 25.0 parts of a petroleum resin having an acidity index measured according to ASTM D 974 less than 0.1 mg KOH / g and a melting point of 155 C, in the form of flakes, - 5.0 parts of a synthetic wax obtained by polymerization of ethylene and characterized by a melting point of 11 0 C, - 1.5 parts d '' a fatty acid of animal origin having a melting point of 57 C, and

  - 15 parts of a talc filler in powder form.

  This binder is prepared in a mixer / kneader as follows a) The oil is loaded into the clean mixer b) The oil is heated to 170 C +/- 5 C c) The polymer is added to the state of granules d) Maintained at 170 C +/- 5 C until dissolution (approximately 0:30) After dissolution of the polymer, the heating is reduced

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  e) At 150 C, the resin is gradually added in the form of flakes f) The set temperature is maintained at 140 C until the resin dissolves.

  g) The wax is gradually added and the mixture is stirred until complete dissolution.

  h) The additive is added and the mixture is stirred until complete dissolution while maintaining the

heating at 140 C.

  i) The heating is reduced to 130 C.

  j) The load is gradually incorporated with moderate stirring.

  B). Binder shaping - pastilla2e The binder, heated to 130 C, is transferred from the mixer to the Sandvik Strip type pelleting machine. Using a Rotoform type device suitable for viscous products, droplets of about 0.2 cm3 at 130 C are deposited at 130 C on the steel plate cooled on its lower surface by

  circulation of water at low temperature (5 C).

  At the end of the strip, the droplets then cooled in the form of solid pellets are sprinkled with talc and scraped to be taken away by means

  from a conveyor belt to bagging.

  Buckets convey the talcated pellets towards the bags which are

  filled then sealed then placed on a pallet.

  Products prepared during three different productions

  have the characteristics shown in Table 1 below.

Table 1

  Features Manufacturing Manufacturing Manufacturing

1 2 3

  Penetration, 1/10 mm 31 27 23 Softening point, C 98 96 98 Dynamic Viscosity, mPa.s

at 130 C 1700 1900 2100

at 150 C 800 840 1000

at 170 C 400 500 500

at 180 C 290 300 370

  Stability no recovery in mass after 3 months of storage

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  The binder produced made it possible to produce perfectly stable pellets

  against mass recovery after 3 months of storage at room temperature.

Example 2

  Binder in the form of granules The binder is prepared from the same constituents as that of

Example 1.

  A first premix A is prepared in a 200 kg capacity mixer equipped to maintain a temperature of 1555 C. comprising: 68.6% by weight of an aromatic type oil having a viscosity at 100 C greater than 30 cSt, and at 40 ° C. greater than 500 cSt, - 29.6% by weight of resin, - 1.8% by weight of additive, A premix called B is also prepared, comprising, in weight percentages: - 25, 9% polymer (EVA) - 12.4% wax (HF wax)

- 61.7% of fines (talc).

  This premix is carried out in a powder mixer.

  The premix A is transferred from the mixer to an extrusion chain consisting of a double-entry extruder for dry matter and liquid material and equipped with a die, a rotary knife and means of cooling by

water jets at the outlet.

  We feed the extruder with premix B and we inject in the middle

  premix A extruder at 155 C.

  The injection rates of these two mixtures are adjusted so that the weight ratio A / B is 67.6% of A for 32.4% of B. The homogeneous mixture obtained leaves the extruder by a die (orifice 3 mm) o the product is simultaneously cooled by a circulation of water

  cold and cut by the action of the rotary knife.

  The speed of the knife is adjusted to obtain granules of

about 6 mm long.

  The granules are then dried and talcated before being packaged.

Example 3

  Asphalt manufacturing from clear solid binder subdivided

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  A solid binder in the form of granules below, called Ag, is prepared by following the protocol described in Example 2 and a binder in the form of pellets, below, called Ap, according to the protocol described in Example 1, as well as a binder in the liquid state prepared from the same components and hereinafter called AI. The compositions of these three binders are given in Table 2 below, the different components of the three binders being those

used in Example 1.

Table 2

  Clear Binders AI Ag Ap Oil 58 46. 4 49.3 Polymer 10.5 8.4 8.9 Resin 25 20 21.2 HF Wax 5 4 4.3 Adhesive Dope 1.5 1.2 1.3 Fine 0 20 15 Table 3 below summarizes the characteristics of the binders clear Al, Ag and Ap in comparison with those of two road bitumens of grade 20/30 and / 50.

Table 3

  Clear Road Binder Bitumens / 30 35/50 AI Ag Ap State --- Liquid - Liquid Granules Pellets of 0.02 g of 0.2 g Penetration, 1/10 min. 28 38 29 25 26 Softening Point, 57 54.5 102 96 96.5 oC Dynamic Viscosity, mPa. s

* at 130 C 1200 1000 1000 2100 1300

* at 150 C 450 350 450 1000 840

* at 180 C 120 100 140 370 300

  From these different binders and bitumens, asphalt mixes are prepared incorporating different types of aggregates and the resistance to homogeneity of these mixtures is determined. Table 4 below summarizes the composition of the mixes as well as

  the results obtained in rutting tests.

  3.1 Asphalt production Three particle size compositions have been chosen: 0/6, 0/10 and 0/14. The aggregates come from the Chailloué quarry and are obtained by crushing.

  The fabrications were made by mixing 20 kg in a kneading machine.

  The formulas 1, 2 and 3 were obtained according to the conventional operating mode, that is to say that the addition of the binder takes place at 170 ° C., therefore in the liquid state in the charge of aggregates brought to 170 ° C. The mineral charge pulverulent preheated to 170 C is gradually incorporated into the mixture once the aggregates are perfectly coated with binder. The mixing operation lasts 5 minutes between the end of the addition of the liquid binder and the obtaining of a homogeneous mixture. The formulas 4, 5, 6 and 7 were obtained according to the same operating protocol as previously with the following differences: * The binder is introduced at room temperature (approximately 20 ° C.) * The fines added are incorporated in a smaller amount to take into account the mineral load possibly contained in the granules / pellets

  * The dye is introduced at the end of mixing.

  The production of these mixtures has shown that perfectly homogeneous mixes are obtained and in times comparable to conventional mixes when the aggregates are preheated to a temperature of 180 C instead of C. This slight increase in temperature allows after addition and fusion of

  solid binder to find a stabilized mixing temperature at 170 C.

  The use of the finely subdivided binder is essential to allow rapid and complete melting of the binder and thus allow a homogeneous dispersion.

of the binder within the asphalt.

  The workability of the mixture is ensured by the low viscosity of the binder

the coating temperature.

  Given these results on laboratory manufacturing, this implementation process by direct incorporation of solid binder can be

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  extrapolated on industrial units for the production of asphalt or mastic asphalts. 3.2 Assessment of the resistance to rutting of asphalt mixes At the end of production, the asphalt mixes are compacted to form plates of dimensions L x W x H = 50 cm x 18 cm x 10 cm. Plates are kept at least 48 hours at rest at room temperature before being evaluated on the rut bench (traffic simulator

type LCPC).

  The tests are carried out according to the NF P98-253-1 method. A wheel applying a load of 5 kN to the plate is subjected to a back-and-forth movement along the length of the plate. The test is carried out in

  a ventilated oven regulated at 60 C.

  Measurements of rut depth are regularly carried out after 3,000, 10,000 and 30,000 A / R cycles of the wheel. For each formula

  of asphalt, the test is doubled and the average result of the 2 tests is determined.

  Comments on the results: * The rut depths measured are all much less than the

  acceptability limit which is 10% at 30,000 cycles.

  The clear binder used in this study has an anti-absorbent power lower than a bitumen 20/30 but higher than a bitumen 35/50

  (comparison of tests 1, 2, 3 and 4).

  * The addition of dye has the effect of reducing the resistance to rutting (tests 5 and 6). The incorporation of 2% dye still allows

  to have a limited rutting (8.7% vs 10% max at 30,000 cycles).

Table 4

  COATING FORMULAS AND ORNAMENT RESULTS

  Formula / Trial I 2 3 4 5 6 7 Aggregates Chailloue Chailloué Chailloué Chailloué Chailloué Chailloué Chailloué

  CaCO3 CaCO3 CaCO3 CaCO3 - ..

  Dye. white white green Binder Bitumen 20/30 Binder AI Bitumen 35/50 Binder Ag Binder Ap Binder Ap Binder Ag * State of the binder Liquid Liquid Liquid Liquid Granules Pastilles Pastilles Granules Formula,% 0/14 0/14 0/10 0/10 0 / 6 0/6 0/6

- 10/14 34 34 0 0 0 0 0

- 6/10 21.5 21.5 29 29 0 0 0

- 2/6 13 13 31 31 63.5 63.5 63.5

- 0/2 30 30 38 38 35 35 35

  - Fine filler 1.5 1.5 2 0.5 0.4 0.4 0 - Colorant - - - - 1 2 1 Binder (F + L) 5.4 5.4 5.9 7.5 7.5 7.5 7.5 * F = Fine 0 0 0 1.5 1.1 1.1 1.5 * L = Pure binder 5.4 5.4 5.9 6.0 6.4 6.4 6.0 - Total,% 105.4 105.4 105.9 106.0 107.4 108.4 107.0 Compactness,% 96 95 94 94 94 92 92/92 Rutting test (NF P 98-253-1) Temperature, C 60 60 60 60 60 60 60 Load, kN 5 5 5 5 5 5 5 Frequency, lz I 1 1 1 1 I 1 -.4 Rut depth,% 3,000 cycles 1.5 2.8 3. 7 2.0 3.7 5.2 3.1 J 000 cycles 3.0 4 4.5 2.3 5.2 7.6 3.3 co 000 cycles 3.2 5.8 5.1 2.4 5.5 8.3 3.6 000 cycles 3.5 6.2 5.9 2.7 5.9 8.7 3.7

Example 4

  Study of formulations of Bituminous Concrete 0/6 and 0/10 discontinuous from

  crushed materials and clear binder.

  1. Object of the study Determination of the mechanical characteristics of bituminous concretes

  made from clear binder granules compared to a bituminous binder.

  2. Composition and characteristics of the binders A binder is prepared: bituminous binder containing, in weight percent bitumen 70/100 97% polymer (EVA) 3% and the characteristics of which are the following penetrability 66 1/10 mm softening point 54 C viscosity at 130 C 1075 mPa.s viscosity at 150 C 390 mrPa.s

viscosity at 180 C 150 mPa.s.

  b) A clear binder containing, in weight percentages: - 76% of a mixture consisting of oil, resin and polymer and having a penetration of 40 to 80 1/10 mm and a softening point "ball and ring "of 55 C - 4% of a polyethylene wax having a melting point of 110 C,

- 20% mineral filler.

  This binder has the following characteristics Penetrability 25 1/10 mm Pt of Softening 96 C Viscosity. at 130 C, 2100 mPa.s Viscosity at 1500C 1400 mPa.s Viscosity at 170 C 500 mPa.s Viscosity at 180 C 350 mPa.s 3. Formulation of "bituminous" mixes The characteristics of the aggregates selected for the study lead to study the following compositions Formula (%) ABC Sable 0 / 2c Ige 35 34 34

Gravillon 4 / 6c Ige 63.5 - -

  Gravel 6 / 10c Ige - 63.5 63.5 Fine filler - 1 2.5 Binder in granules (F + L) 7.5 7.5 F = Fine 1.5 1.5 L = Clear binder 6 6 Bituminous binder - - 6

TOTAL 106 106 106

  Asphalt mixes are produced in a Guedu Type 3 mixer

* in accordance with standard NF P 98-250-1.

  4. Mechanical characteristics of coated materials They were understood from tests: - PCG NF P98-252 (Giratory Shear Press) Duriez NF P98-251-1 - Omiérage NF P98-253- 1 The results obtained on the 2 formulas tested are presented in the following tables ABC Acceptance Limits BB BBMc BBMc

0/6 0/10 0/10

  MVR t / m3 aggregates 2.718 2.733 2.732 MVR t / m3 coated 2.487 2.499 2.498 Specific surface 13.57 13.03 12. 79 Modulus of wealth 3.65 3.70 3.72 PCG Compactness,% at 10 gyrations 81.0 87.9

852 91.6

86.9 93.5

88.1 94.2

89.6 95.2

89.9 95.4

90.8 95.8

92.0 96.6

  Rutting rutting depth,% at 30 cycles 0.6 1.4 2

1.2 1.8 3.4

300 1.4 2.5 4.5

1000 1.6 3.6 6.1

3000 1.7 4.6 8.7

10,000 2.3 6.1 10.4

Duriez Compact 89.4 92.2

-R (air), MPa 8.5 9.8 7.5 Min.

-r (water), MPa 7.5 8.6

  -riR (Immers.iCompressn. Report) 0.88 0.88 1 0.75 Max.

  5. Comments Examination of the performances of the 3 compositions tested shows that

  the binder gives coated materials excellent mechanical stability properties.

  The results of the Duriez tests carried out on the various mixes based on clear binder are satisfactory with regard to standards concerning concrete

  bituminous for use in road applications.

  The rut depth measured on the clear binder mix (B) is 4% less than that measured on the binder reference formula

bituminous (C).

Claims (11)

  1. Clear binder or bituminous binder, in particular intended for the manufacture of road mixes, poured asphalts or waterproofing membrane, characterized in that it has the following properties: - penetrability at 25 C less than 50 1/10 mm, according to standard NFT 66-004, preferably less than 35 1/10 mm, - softening point greater than 70 C, according to standard NFT 66-008, preferably greater than 80 C, more preferably still greater than C , - dynamic viscosity at 180 C less than 1000 mPa.s, preferably   less than 500 mPa.s, more preferably less than 300 mPa.s.   2. Binder according to claim 1, characterized in that it has a viscosity at 130 C of less than 2500 mPa.s and preferably less than 1500 mPa.s.   3. Binder according to claim 1 or 2, characterized in that it contains 3 to 40% by weight, preferably from 5 to 40%, of at least one wax called HF wax   having a melting point higher than 90 C, preferably higher than 100 C.   4. Binder according to claim 3, characterized in that said HF wax is a hydrocarbon wax obtained by polymerization of C2 to C6 olefins,   preferably by polymerization of ethylene, propylene and hexene.   5. Binder according to claim 3, characterized in that said wax is an amide type wax resulting from the reaction of a carboxylic acid or a   mixture of carboxylic acids with a diamine.   6. Solid particles at room temperature, characterized in that they comprise, as an essential constituent, a binder according to one of claims I to 4.   7. Particles according to claim 6, characterized in that they are   in the form of granules or pellets.   8. Particles according to claim 6 or 7, characterized in that they additionally contain up to 50% of at least one filler, in particular under   form of fines, such as limestone, talc or metallic oxides.   9. Method for preparing binder particles according to one of the   claims 6 to 8, characterized in that it comprises a step of draining on   a cooled plate of a binder according to one of claims 1 to 4 incorporating   in addition, if necessary, at least one charge.   10. Process for the preparation of binder particles according to one of the   Claims 6 to 8, characterized in that it comprises a stage of extrusion and   granulation of a binder composition as defined in one of the   Claims 1 to 5 incorporating, where appropriate, additionally at least one filler.   11. Asphalt, poured asphalt and waterproofing membranes, characterized in that they are obtained by using a binder according to one of   Claims 1 to 5 or of particles according to one of Claims 6 to 8.