EP0582626A1 - Emulsions de bitume - Google Patents

Emulsions de bitume

Info

Publication number
EP0582626A1
EP0582626A1 EP19920909630 EP92909630A EP0582626A1 EP 0582626 A1 EP0582626 A1 EP 0582626A1 EP 19920909630 EP19920909630 EP 19920909630 EP 92909630 A EP92909630 A EP 92909630A EP 0582626 A1 EP0582626 A1 EP 0582626A1
Authority
EP
European Patent Office
Prior art keywords
bitumen
emulsion
water
mixer
static mixer
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP19920909630
Other languages
German (de)
English (en)
Inventor
Christopher Scott Rayner
Jean-Luc Marchal
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
ExxonMobil Technology and Engineering Co
Original Assignee
Exxon Research and Engineering Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Exxon Research and Engineering Co filed Critical Exxon Research and Engineering Co
Publication of EP0582626A1 publication Critical patent/EP0582626A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
    • 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
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2395/00—Bituminous materials, e.g. asphalt, tar or pitch

Definitions

  • This invention relates to bitumen emulsions, mixes of bitumen emulsions with aggregate material, and their use in road-making and similar operations.
  • a mix of aggregate and cut-back asphalt i.e. bitumen diluted with an organic solvent such as kerosene or creosote to provide workability to the aggregate-bitumen mix.
  • bitumen diluted with an organic solvent such as kerosene or creosote to provide workability to the aggregate-bitumen mix.
  • organic solvent such as kerosene or creosote
  • This has the advantage that it can be applied at ambient or near ambient temperatures and there can be some time delay, if desired, between preparing the mix and applying it to the surface.
  • the bitumen takes longer to harden after application to the road surface, as the rate of hardening is dependent upon evaporation of the solvent, and, even so, some solvent remains in the bitumen ca_sing the road surface to be slightly soft V and therefore have a tendency to deform under the weight of passing traffic.
  • the evaporation of the solvent into the atmosphere during hardening of the bitumen is an environmental pollutant and therefore
  • a mix of aggregate and bitumen-in-water emulsion has the advantage that it can be applied to the road surface at ambient temperature but the disadvantage that it must be applied immediately as the action of mixing the aggregate with the emulsion causes the emulsion to break, i.e. the bitumen and water phases separate, and the bitumen starts to harden.
  • increased amounts of emulsifier can be included in the emulsion, but this has the disadvantage that the emulsion can take a considerable time to break after application to the road, which delays the hardening of the bitumen and increases the time that the road has to be closed to traffic.
  • the storage life of the mix can be improved by adding organic solvent to the emulsion, but this has the disadvantage of a soft road surface and pollution as described under (ii) above for the cut-back asphalt mixes.
  • the present invention provides a bitumen emulsion comprising by weight based on the total weight of the emulsion: a) 40 to 85 per cent bitumen; b) 0.05 to 1.0 per cent emulsifier; c) 14 to 59.95 per cent water,
  • the emulsion being substantially free of organic solvent, and containing emulsified bitumen droplets having a mean particle size of from 2 to 10 micrometres (urn) with a standard deviation of no more than 0.3.
  • bitumen droplets which have a particle size that is within a specific range and is substantially uniform, it is possible to form an emulsion which remains sufficiently stable when mixed with aggregate to act as a delayed-set emulsion without the need for an organic solvent and/or increased amounts of emulsifier, but which breaks sufficiently quickly after it has been applied to the road so there is as short a time as possible before the road can be opened to traffic.
  • the absence or substantial absence of solvent provides an 'environmentally friendly 1 emulsion with little, if any, pollutants evaporating into the atmosphere when the emulsion breaks.
  • the absence of solvent also has the advantage that, once the emulsion has broken, the road surface sets completely and is not subject to damaging deformation.
  • bitumen droplets in the emulsion according to the invention have a mean particle size of from 3 to 9 um, more preferably from 5 to 8 ⁇ m.
  • the standard deviation of this mean is preferably no more than 0.2, for example in the range from 0.1 to 0.2.
  • the bitumen employed in the emulsion may be any commercially available natural or petroleum-based bitumen (also known as asphalt) suitable for use in road construction, maintenance and repair. It may be a straight-run bitumen or a blown or oxidised grade.
  • the penetration (IP 49) may vary from 20 to 500 at 25°C, preferably 50 to 400, more preferably 100 to 250.
  • Its Ring and Ball softening point (IP 58) is generally from 35 to 100°C, preferably 35 to 60°C.
  • the amount of bitumen contained in the emulsion is from 40 to 85 weight percent, preferably 50 to 75 percent, more preferably 60 to 70 percent, based on the total weight of the emulsion.
  • the amount of emulsifier employed may range from 0.05 to 1.0 weight percent, but usually an amount from 0.1 to 0.5 wt.%, more preferably 0.2 to 0.4 wt.% is employed, i.e. a typical amount of emulsifier for a bitumen emulsion.
  • the emulsifier may be cationic, anionic or non-ionic, or a mixture of cationic and non-ionic, or anionic and non-ionic emulsifiers, depending upon the chemical nature of the aggregate with which the emulsion is to be mixed, and upon the desired electrochemical properties of the emulsion.
  • Suitable cationic emulsifiers include hydro- chlorides of fatty amines, fatty amido-amines, ethoxylated amines, imidoazalines, quartenary ammonium salts, and mixtures thereof.
  • the cationic emulsifier is a diamine, for example tallow diamine hydrochloride, and more preferably is a mixture of a diamine with a quatenary ammonium salt.
  • an acid in the bitumen emulsion it is preferred to include an acid in the bitumen emulsion to counteract the alkalinity of the emulsifier. Generally acid is added to adjust the pH of the emulsion to approximately pH 3.
  • Suitable acids include inorganic acids, for example hydrochloric acid.
  • Suitable anionic emulsifiers include long chain carboxylic and sulphonic acids, their salts and mixtures thereof.
  • Suitable non-ionic emulsifiers include ethoxylated compounds, for example ethoxylates of sorbitan esters, alcohols and alkyl phenols, and mixtures thereof.
  • a salt for example a mineral salt such as calcium chloride, may be included in the emulsion according to the invention to balance the salinity, and also to modify the emulsion viscosity. If a salt is employed, typically the amount is from 0.05 to 0.5, preferably from 0.1 to 0.3 weight percent based on the total weight of the emulsion.
  • the bitumen may be modified by the incorporation into the bitumen of a polymeric additive, for example ethylene vinyl acetate or styrene-butadiene polymers, or mixtures thereof. These can be added in amounts up to about 25 weight percent based on the total weight of the emulsion.
  • the polymers modify the bitumen to increase its resilience, which is benefi ⁇ cial, for example, when the bitumen is used for a road surface subject to heavy traffic.
  • the remainder of the bitumen emulsion according to the invention comprises water. This remainder may be from 14 to just under 60 weight percent, but is preferably 20 to 50 percent, more preferably 30 to 40 percent, based on the total weight of the emulsion.
  • the emulsion is usually produced as a bitumen-in-water emulsion, i.e. the bitumen particles are surrounded by water molecules, although it may alternatively be produced as a water-in-bitumen emulsion. ⁇ P
  • bitumen emulsion may be prepared by a static mixing process as disclosed in published European Patent Application 283246A, the disclosure of which is incorporated herein by reference.
  • the process preferably comprised the following steps:
  • the said other mixer is also a static mixer.
  • the emulsifier in part or in total, may be mixed with the water to be added to the first mixer to form an aqueous solution or "soap".
  • the bitumen may be premixed with the water and/or the emulsifying agent prior to introduction into the first mixer.
  • the bitumen is preferably introduced into the first static mixer at a temperature of 100 to 200°C, more preferably 120 to 190°C, and at a pressure of 2 to 80 bars, more preferably 10 to 30 bars.
  • the water or soap is preferably introduced into the same mixer at a temperature of 20 to 70°C, more preferably 30 to 50°C, and also at a pressure of 2 to 80 bars, more preferably 10 to 30 bars.
  • the temperature in the first mixer is usually 70 to 250°C, more preferably 100 to 150°C. A high temperature facilitates the emulsification of the bitumen and water, and the relatively high pressure prevents the water from evaporating.
  • the resultant mixture from the first static mixer directly into the other mixer, which is also preferably a static mixer.
  • the remainder of the water is introduced into this other mixer, preferably cold, for example 50 to 20°C, so that it cools the emulsion enabling the resultant emulsion to exit the other mixer below the boiling point of water. It is also advantageous to operate this other mixer at a reduced pressure relative to the first mixer so that the emulsion emerges from the other mixture at atmospheric pressure.
  • additives are to be included in the emulsion, they may be added at any stage during the process, although are preferably added to the first t static mixer to ensure thorough mixing, and conveniently are added at the same time as the emulsifier. If they are water soluble, as in an inorganic acid and/or a metal salt, they may be added to the water-emulsifier soap.
  • the process is preferably a two-mixer process, but more than two mixers may be used.
  • These additional mixers may be static mixers or other types of mixers, such as a colloid mill.
  • suitable static mixers are those known as Sulzer or Kenics mixers, which are well known to those skilled in the art of static mixing.
  • the bitumen emulsion may be used in the construc ⁇ tion, maintenance and repair of road surfaces and in other applications where bitumen is required.
  • the bitumen emulsion is especially beneficial for mixing with aggregate to be used for road repair, for example the filling in of cracks and pot-holes caused for example by the passage of heavy and/or frequent vehicles or frost damage, and trenches dug to bury pipelines or cable, for example, under the road.
  • Road repair often requires the use of relatively small amounts of aggregate mix and the delayed-set property of the aggregate-emulsion mix of the invention enables one larger amount of mix to be prepared and stored, with small quantities being taken from the stored mix as and when needed.
  • bitumen emulsion is mixed with aggregate, which may be of any type of aggregate suitable for the required application, provided the bitumen contains an emulsifier appropriate for the type of aggregate selected, and is usually either siliceous or calcareous.
  • aggregate is mixed with the emulsion using conventional mixing techniques, typical proportions of aggregate to emulsion being from 6:1 to 30:1.
  • the emulsion-aggregate mix can be applied to the road using conventional techniques. ' It may be applied hot or cold, although for ease of handling it is applied at ambient temperatures, for example from 10 to 25°C.
  • the emulsion-aggregate mix breaks and the bitumen hardens relatively rapidly and the road surface is ready for use.
  • the actual time taken for the bitumen to harden depends upon a number of factors in addition to the characteristics of the bitumen emulsion including the speed and pressure of compaction of the bitumen- aggregate layer, for example by rolling; the porosity of the surface to which the emulsion-aggregate mix is being applied; the chemical and physical influence of the aggregate; and the weather conditions.
  • bitumen hardening time for a surface prepared from an emulsion- aggregate mix according to the invention may vary, for example, from about 10 minutes to a number of days, for example 5 days or more, but usually the surface can be used by traffic as soon as the mix has been compacted, especially in the case of road repair. ⁇
  • bitumen emulsion having the following composition and properties was prepared.
  • the percentages of components are weight per ⁇ ents based on the total weight of the emulsion unless otherwise specified:
  • Emulsifier N-tallow diamine hydrochloride 0.6% Hydrochloric acid 0.2%
  • the emulsion was prepared using a two-stage static mixing process as disclosed in published European patent application 0283246A2.
  • the two static mixers employed were both Kenics mixers of the type described in Chemineers brochure 800E published by Chemineers Ltd., 1984.
  • the bitumen and a soap solution comprising the emulsifier, hydrochloric acid, calcium chloride and one-third of the total amount of the water were injected into the first static mixer.
  • the bitumen was injected under a pressure of 2400 kPa and was at a temperature of 150°C.
  • the soap solution and water were both injected under a pressure of 2400 kPa and at a temperature of 50°C.
  • the flowspeed into the first static mixer was about 14m/sec and the flowrate about 15m 3 /hr.
  • the shear produced by the first static mixer was calculated, based on the Darcy equation and taking A ⁇ flowspeed, flowrate and size of pipes into account, to be about 35,000 sec" 1 .
  • the mixture was fed directly into the second static mixer into which the remainder of the water was injected at a pressure of 400 kPa and a temperature of about 18°C.
  • the shear rate in the second static mixer was calculated to be about 5,000 sec ⁇ l and the flowrate was about 20m 3 per hour.
  • the resulting emulsion exited at atmospheric pressure and a temperature of about 85°C.
  • the total amount of water present in the mixture was 35% by weight of the total weight of the final product.
  • bitumen droplets having a median particle diameter of 5.5 urn and a standard deviation of 0.18.
  • An aggregate/bitumen emulsion mix was prepared by combining 93.8 wt.% limestone aggregate and 6.2 wt.% of the above bitumen emulsion.
  • the size gradings of the aggregate conformed to British Standard 4987 (Table 5) for a 20 mm dense graded base coarse macadam and were as follows:
  • the aggregate and emulsion were mixed together at ambient temperature using a conventional mixer and mixing was continued until the emulsion had coated the aggregate particles.
  • the resulting mix was laid into damaged areas and pot-holes in a macadam simulated road surface.
  • the mix was spread and approximately levelled by a hand-held leveller in the usual manner. It was then compacted into place by a small vibrating hard-steel roller machine, the mix becoming hard on compaction.
  • the road which had been closed to traffic during repair, was re-opened immediately after the mix had been compacted. During the following 4-6 hours after compaction the water separated and flowed frqa the emulsion and the repaired patches began to harden. The macadam reached its normal strength of 20 mm pen within about 4 days.
  • An emulsion was prepared using a two-stage-static mixing process similar to that used in Example I.
  • the emulsion had the following composition, with the individual components expressed as weight percentages of the total weight of the emulsion:-
  • the particle size was measured to have a median diameter of 5.2 urn and standard deviation of 0.18.
  • the emulsion was used to coat a granite type material at a rate that resulted in 4% by weight residual bitumen on the aggregates.
  • the composition of the material (as percentages are weight percentages of the total weight of the material) was:
  • the coated material described above can be stored for a period of at least one month, and its performance is not impaired by the storage providing it remains humid enough.
  • the same moulds were prepared, according to the same procedure as above, with an emulsion containing 7% solvent in place of part of the bitumen : the emulsion had the following composition (percentages again being expressed as weight percentages of the total weight of the emulsion) :-
  • bitumen straight run 100 penetration at 25°C (IP49) 7% solvent: kerosene 0.8% emulsifier: N-tallow polyamine, manufactured and sold by the French company CECA under the Trade Mark Polyram S. 0.74% hydrochloric acid 33.46% water.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Dispersion Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Civil Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Road Paving Structures (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

Emulsion de bitume comportant 40 à 80 % en poids de bitume, 0,05 à 1,0 % en poids d'émulsifiant et 14 à 59,95 % en poids d'eau, l'émulsion étant essentiellement exempte de solvants organiques et renfermant des gouttelettes de bitume émulsifié d'une taille moyenne de 2 à 10 micromètres, avec un écart-type d'au plus 0,3. L'émulsion est obtenue par un procédé de mixage statique. Elle peut être utilisée, par exemple, pour des réparations de revêtement routier et elle présente l'avantage de pouvoir être préparée et entreposée avant l'emploi ("prise retardée") sans qu'il soit nécessaire d'y incorporer un solvant organique.
EP19920909630 1991-05-03 1992-04-29 Emulsions de bitume Withdrawn EP0582626A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB9109709A GB2255291A (en) 1991-05-03 1991-05-03 Bitumen emulsions.
GB9109709 1991-05-03

Publications (1)

Publication Number Publication Date
EP0582626A1 true EP0582626A1 (fr) 1994-02-16

Family

ID=10694472

Family Applications (1)

Application Number Title Priority Date Filing Date
EP19920909630 Withdrawn EP0582626A1 (fr) 1991-05-03 1992-04-29 Emulsions de bitume

Country Status (6)

Country Link
EP (1) EP0582626A1 (fr)
JP (1) JPH07507577A (fr)
CA (1) CA2102311A1 (fr)
GB (1) GB2255291A (fr)
NO (1) NO933954L (fr)
WO (1) WO1992019683A1 (fr)

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Publication number Priority date Publication date Assignee Title
SE470522B (sv) * 1992-11-18 1994-07-04 Nynaes Petroleum Ab Förfarande för att minska viskositeten hos bitumen
GB9306290D0 (en) * 1993-03-26 1993-05-19 Exxon Research Engineering Co Bituminous surface construction
US6595202B2 (en) 1996-05-13 2003-07-22 Universidad De Sevilla Device and method for creating aerosols for drug delivery
US6189803B1 (en) 1996-05-13 2001-02-20 University Of Seville Fuel injection nozzle and method of use
US6405936B1 (en) 1996-05-13 2002-06-18 Universidad De Sevilla Stabilized capillary microjet and devices and methods for producing same
US6386463B1 (en) 1996-05-13 2002-05-14 Universidad De Sevilla Fuel injection nozzle and method of use
US6187214B1 (en) 1996-05-13 2001-02-13 Universidad De Seville Method and device for production of components for microfabrication
US6299145B1 (en) 1996-05-13 2001-10-09 Universidad De Sevilla Device and method for fluid aeration via gas forced through a liquid within an orifice of a pressure chamber
ES2140998B1 (es) * 1996-05-13 2000-10-16 Univ Sevilla Procedimiento de atomizacion de liquidos.
US6792940B2 (en) 1996-05-13 2004-09-21 Universidad De Sevilla Device and method for creating aerosols for drug delivery
US6196525B1 (en) 1996-05-13 2001-03-06 Universidad De Sevilla Device and method for fluid aeration via gas forced through a liquid within an orifice of a pressure chamber
US6116516A (en) 1996-05-13 2000-09-12 Universidad De Sevilla Stabilized capillary microjet and devices and methods for producing same
FR2760461B1 (fr) * 1997-03-10 1999-05-28 Colas Sa Emulsion de bitume, procede d'obtention d'une emulsion de bitume et procede d'obtention d'un materiau bitumineux pour la construction ou l'entretien des chaussees
JP2002508238A (ja) * 1997-12-17 2002-03-19 ユニバーシィダッド デ セビリヤ 流体のエアレーションのためのデバイスおよび方法
US6450189B1 (en) 1998-11-13 2002-09-17 Universidad De Sevilla Method and device for production of components for microfabrication
FR2794468B1 (fr) * 1999-06-01 2001-08-24 Ceca Sa Emulsions bitumineuses, leur utilisation pour la realisation de materiaux et de tapis routiers
FR2852964B1 (fr) * 2003-03-31 2006-09-01 Colas Sa Emulsion de bitume a gouttelettes calibrees et procede d'obtention
US7833338B2 (en) * 2004-02-18 2010-11-16 Meadwestvaco Packaging Systems, Llc Method for producing bitumen compositions
US7297204B2 (en) * 2004-02-18 2007-11-20 Meadwestvaco Corporation Water-in-oil bituminous dispersions and methods for producing paving compositions from the same
ES2394404T3 (es) 2004-02-18 2013-01-31 Meadwestvaco Corporation Procedimiento para producir composiciones bituminosas
FR2876700B1 (fr) * 2004-10-19 2007-01-05 Ceca Sa Sa Emulsions bitumineuses, leur procede de preparation et leur utilisation pour la realisation de materiaux et de tapis routiers
FR2915996B1 (fr) * 2007-05-10 2009-07-10 Ceca Sa Sa Materiaux routiers bitumineux, notamment enrobes a froid et graves-emulsions, et tapis routiers formes a partir de ces materiaux
WO2010096526A2 (fr) * 2009-02-19 2010-08-26 Meadwestvaco Corporation Procédé de production de compositions bitumineuses de pavage
WO2018222476A1 (fr) 2017-05-31 2018-12-06 Exxonmobil Research And Engineering Company Procédé et outil de prédiction des propriétés d'une émulsion d'asphalte
US20220186076A1 (en) * 2020-12-15 2022-06-16 Russell Standard Corp. Void Reducing Asphalt Membrane Emulsion

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FR2109463A5 (en) * 1970-10-19 1972-05-26 Exxon Research Engineering Co Neutral cationic binder emulsion - slow breaking esp for bitumen
GB8706148D0 (en) * 1987-03-16 1987-04-23 Exxon Chemical Patents Inc Dispersions & emulsions

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Also Published As

Publication number Publication date
NO933954D0 (no) 1993-11-02
JPH07507577A (ja) 1995-08-24
WO1992019683A1 (fr) 1992-11-12
CA2102311A1 (fr) 1992-11-04
GB2255291A (en) 1992-11-04
GB9109709D0 (en) 1991-06-26
NO933954L (no) 1993-12-29

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