WO2012160553A1 - Compositions de bitume stabilisées, leur procédé de production et leur utilisation à titre de matériaux de construction - Google Patents

Compositions de bitume stabilisées, leur procédé de production et leur utilisation à titre de matériaux de construction Download PDF

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Publication number
WO2012160553A1
WO2012160553A1 PCT/IL2012/000204 IL2012000204W WO2012160553A1 WO 2012160553 A1 WO2012160553 A1 WO 2012160553A1 IL 2012000204 W IL2012000204 W IL 2012000204W WO 2012160553 A1 WO2012160553 A1 WO 2012160553A1
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Prior art keywords
bitumen
stabilized
composition according
weight
polymer
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Ceased
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PCT/IL2012/000204
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English (en)
Inventor
Ronen Alexander Peled
Andrey Vorobiev
Gregory Svechinsky
Ilan Ishai
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DSI Dimona Silica Industries Ltd
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DSI Dimona Silica Industries Ltd
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Publication of WO2012160553A1 publication Critical patent/WO2012160553A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/17—Amines; Quaternary ammonium compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/10—Homopolymers or copolymers of propene
    • C08L23/12—Polypropene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L53/00—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
    • C08L53/02—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers of vinyl-aromatic monomers and conjugated dienes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L95/00—Compositions of bituminous materials, e.g. asphalt, tar, pitch
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C08K2003/265—Calcium, strontium or barium carbonate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2555/00—Characteristics of bituminous mixtures
    • C08L2555/20—Mixtures of bitumen and aggregate defined by their production temperatures, e.g. production of asphalt for road or pavement applications
    • C08L2555/22—Asphalt produced above 140°C, e.g. hot melt asphalt
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2555/00—Characteristics of bituminous mixtures
    • C08L2555/40—Mixtures based upon bitumen or asphalt containing functional additives
    • C08L2555/50—Inorganic non-macromolecular ingredients
    • C08L2555/52—Aggregate, e.g. crushed stone, sand, gravel or cement
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2555/00—Characteristics of bituminous mixtures
    • C08L2555/40—Mixtures based upon bitumen or asphalt containing functional additives
    • C08L2555/80—Macromolecular constituents
    • C08L2555/84—Polymers comprising styrene, e.g., polystyrene, styrene-diene copolymers or styrene-butadiene-styrene copolymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2555/00—Characteristics of bituminous mixtures
    • C08L2555/40—Mixtures based upon bitumen or asphalt containing functional additives
    • C08L2555/80—Macromolecular constituents
    • C08L2555/86—Polymers containing aliphatic hydrocarbons only, e.g. polyethylene, polypropylene or ethylene-propylene-diene copolymers

Definitions

  • the present invention relates to stabilized bitumen compositions with improved properties useful as construction materials and to a method for producing the compositions.
  • the present invention seeks to provide a stabilized bitumen composition that has superior properties and is more economical than existing bitumen compositions.
  • a stabilized bitumen composition including bitumen, and a structurizer including porcelanite and an activating agent.
  • the activating agent includes a quaternary ammonium compound.
  • the quaternary ammonium compound includes at least two alkyl chains of 10 - 30 carbons, more preferably 15 - 18 carbons. Most preferably, the quaternary ammonium compound is di(hydrogenated tallow)dimethylammonium chloride.
  • the activating agent includes the quaternary ammonium compound in an amount of about 1 - 15% of the porcelanite weight, more preferably about 1 - 10% of the porcelanite weight.
  • the composition includes about 0.5 - 25% of the structurizer by weight, more preferably about 5 - 15% of the structurizer by weight.
  • the bitumen is selected from asphalt cement, asphalt binder and performance grade bitumen.
  • the composition preferably includes about 20 - 90% of the bitumen by weight, more preferably about 30 - 80% of the bitumen by weight, and most preferably about 40 - 70% of the bitumen by weight.
  • the composition further includes a diluent.
  • the diluent is preferably a light hydrocarbon, more preferably naphtha.
  • the compositions preferably includes about 10 - 30% diluent by weight, more preferably, about 15 - 25% diluent by weight.
  • the composition further includes at least one additive selected from a solvent, a polymer and a filler.
  • the solvent is preferably selected from kerosene, toluene and trichloroethylene, most preferably toluene.
  • the composition includes not more than about 15% solvent by weight.
  • the polymer is selected from polyurethane, silicones, atactic polypropylene (APP), ethylene-vinyl acetate (EVA), styrene-butadiene (SB) and styrene-butadiene-styrene (SBS), more preferably APP and SBS.
  • the composition preferably includes not more than about 20% polymer by weight, more preferably not more than about 15% polymer by weight.
  • the filler is selected from calcium carbonate, coal ash, clay, limestone and dolomite, most preferably calcium carbonate.
  • the composition preferably includes not more than about 30% filler by weight, more preferably not more than about 25% filler by weight.
  • a method of providing a stabilized bitumen composition including providing bitumen at a temperature of about 100 - 140°C, adding a structurizer including porcelanite and an activating agent to the bitumen and mixing to form a homogenous composition.
  • the method further includes cooling the composition to ambient temperature.
  • the structurizer is added to the bitumen before the cooling.
  • the structurizer is added to the mixture after the cooling.
  • the method further includes adding a diluent to the bitumen.
  • the method further includes heating the bitumen to about 160 - 200°C, adding a polymer to the bitumen, mixing the polymer with the bitumen for up to two hours, and cooling the bitumen to provide bitumen at about 100 - 140°C.
  • the method further includes adding to the composition at least one additive selected from a solvent, a polymer and a filler.
  • Fig. 1 is a graph showing the thixotropic properties of the stabilized bitumen composition of the present invention. DETAILED DESCRIPTION OF THE INVENTION
  • Bitumen-containing compositions are among the most widely used materials for road construction, waterproofing, damp proofing, corrosion-resistance, insulation, coating applications and other uses. These materials typically comprise bitumen, fillers, solvents, diluents and other additives.
  • bitumen itself, as the most important ingredient and often the basis for these materials, has a number of defects, the most significant of which are: narrow working temperature range, limited elasticity and short operating life. Oxidation due to atmospheric influences destroys the bitumen, resulting in crack formation and splitting.
  • bitumen - the change of its properties by addition of different additives - is one of the ways of improving of the stability of bitumen- containing materials under heavy stresses and extreme ambient temperatures.
  • One of the most common modification methods is to blend bitumen with a polymer, such as polyurethane, silicones and atactic polypropylene (APP).
  • APP atactic polypropylene
  • SBS tri-block copolymer styrene-butadiene-styrene
  • polymer structural blocks leads to the creation of self-organizing three-dimensional polymer network in the volume of the polymer-bitumen binding agent due to the physical stitching of the polymer macromolecules. Owing to this, the polymer -bitumen composition acquires elastomeric properties, such as reduction of fragility at low temperatures, and increased shear resistance at high operational temperatures.
  • the polymer modifier can increase the cost of the bitumen by 100% or more.
  • bitumen is already the most expensive component of construction materials, the increased cost of polymer modification affects the overall construction cost significantly.
  • bitumens Another problem with polymer-modified bitumens is their lack of adhesion to hydrophilic surfaces such as stone and metal. Since the polymer-modified bitumens are highly hydrophobic, there is a tendency for water to creep into the space between the bitumen and the surface to which it is applied and strip the bitumen away from the surface. Unmodified bitumen suffers the same stripping from hydrophilic surfaces.
  • Another method of modifying bitumen is the addition of filaments, usually cellulose or mineral fibers to the mix. Polymer fibers can also be used for this purpose. The usual content of fibers in construction materials is about 5%. While fibers impart stability to bitumen, they also cause an increase in viscosity which renders mixing difficult.
  • a modifier for use in asphalt mixes is disclosed in WO 2010/116354, assigned to the assignee of the present invention and incorporated by reference herein in its entirety. It has now been discovered that this modifier is useful in stabilizing bitumen by creating a three-dimensional elastic reticular structure within the bitumen. Stabilized bitumen compositions comprising this modifier have superior thixotropic properties, which make the compositions especially suitable for use in construction materials.
  • a stabilized bitumen composition comprising bitumen and a stabilizing composition, referred to hereinafter as a "structurizer”.
  • bitumen is preferably asphalt cement grade bitumen in accordance with
  • ASTM D 3381 such as AC-20 or AC-30.
  • the number refers to the viscosity of the bitumen at 60 °C in units of 100 Poise.
  • AC-20 has a viscosity of 2000 P at 60 °C.
  • the bitumen may also be asphalt binder or performance grade bitumen, such as PG-64, PG-70 or PG-76, according to a national standard.
  • the stabilized bitumen composition preferably comprises about 20 - 90% bitumen by weight, more preferably about 30 - 80% bitumen by weight, most preferably about 40 - 70% bitumen by weight
  • the structurizer comprises porcelanite, a mineral found, inter alia, in deposits in the Dead Sea area of Israel and described in detail in WO 2010/116354, and an activating agent.
  • the activating agent is a quaternary ammonium compound.
  • the quaternary ammonium compound preferably has at least two long carbon chains.
  • the long carbon chains preferably comprise between 10 and 30 carbon atoms, more preferably from 15 to 18 carbon atoms.
  • An especially preferred compound is di(hydrogenated tallow)dimethylammonium chloride, available from Akzo-Nobel (Stockholm, Sweden) as Arquad 2HT-75 (hereinafter "2HT-75").
  • Activation of the porcelanite is preferably achieved by crushing the porcelanite to about 3 - 8 mm particle size granules, adding the activating agent, and blending the mixture until the desired particle size is achieved.
  • the porcelanite can be blended for about 5 minutes, followed by addition of the activating agent and further blending for an additional 1 - 5 minutes.
  • the weight of the quaternary ammonium compound is preferably between 1 and 15% of the porcelanite weight. More preferably, the weight of the quaternary ammonium compound in the structurizer is between 1 and 10% of the porcelanite weight.
  • the stabilized bitumen composition preferably comprises about 0.5 - 25% structurizer by weight, more preferably about 5 - 15% structurizer by weight.
  • the stabilized bitumen composition optionally contains a diluent.
  • the diluent can be any liquid miscible with bitumen.
  • the diluent preferably comprises light hydrocarbons. Most preferably, the diluent is naphtha. When present, the diluent comprises about 10 - 30% of the stabilized bitumen composition by weight, more preferably about 15 - 25% of the stabilized bitumen composition by weight.
  • the stabilized bitumen composition optionally further includes additives preferably selected from polymers, fillers, and solvents.
  • the total additives comprise up to about 40% of the stabilized bitumen composition.
  • the stabilized bitumen composition has reduced amounts of the polymers, fibers and other additives necessary to prepare comparable bitumen compositions lacking the structurizer.
  • the polymer is preferably selected from typical polymers used to modify bitumen, such as polyurethane, silicones, atactic polypropylene (APP), ethylene-vinyl acetate (EVA), styrene-butadiene (SB) and styrene-butadiene-styrene (SBS).
  • the polymer is preferably included in an amount that is less than the amount of polymer used in a comparable material without the structurizer.
  • the stabilized bitumen composition comprises no more than about 20% polymer, more preferably no more than about 15% polymer.
  • the filler is preferably a solid inorganic compound.
  • the filler can be in amorphous or crystalline form.
  • Particularly preferably fillers are calcium carbonate, coal ash, clay and other similar soft, fine ground minerals such as limestone and dolomite.
  • the stabilized bitumen composition comprises no more than about 30% filler, more preferably no more than about 25% filler.
  • the solvent can be any solvent that is miscible with bitumen and helps to solubilize the polymer.
  • the solvent is a hydrocarbon solvent such as kerosene, an aromatic hydrocarbon solvent such as toluene or a chlorinated hydrocarbon solvent such as trichloroethylene.
  • the solvent is preferably present in an amount of up to 15% of the stabilized bitumen composition by weight.
  • the stabilized bitumen composition of the present invention is preferably prepared by the following procedure: bitumen is heated to about 100 - 140°C and optionally mixed with a diluent. Optionally, a polymer is added. Structurizer is added and the composition is mixed for about 30 minutes while cooling to ambient temperature. Other ingredients such as fillers, solvents and other additives can be added together with the structurizer or after cooling to ambient temperature. Alternatively, the structurizer can be added after cooling to room temperature.
  • bitumen in order to achieve full mixing with the polymer, bitumen is first heated to about 160 - 200°C and mixed with the polymer additive for up to about two hours. The bitumen-polymer mixture is then cooled to about 100 - 140°C, and the other components are added as described above.
  • the activated porcelanite structurizer was prepared as follows: 100 g of crushed porcelanite with a particle size between 3 and 8 mm was mixed with 5 g of 2HT-75 in a laboratory blender at 20,000 RPM for 5 minutes. The particle size distribution was measured by Malvern Mastersizer 2000. Maximum particle size was 40 ⁇ . This structurizer was used in all of the following Examples.
  • Structurized bitumen was prepared by heating PG-70 grade bitumen to about 140 °C and adding structurizer in an amount of 15% of the bitumen weight. The viscosities of the structurized bitumen and pure bitumen at 160 °C were measured as a function of shear rate. The results are shown in Fig. 1.
  • This property can be utilized, for example, for waterproofing a vertical surface.
  • the requirements for the thickness of the waterproofing layer according to local specifications in Israel is not less than 3 mm.
  • Bitumen must be heated in order to be applied to the surface, since cold bitumen is too viscous. It is impossible to apply a pure bitumen layer of the required thickness in one pass by spraying or with a brush, since the hot bitumen is too thin and will run down the surface before cooling. Adding about 15% of structurizer to the bitumen will impart high resting viscosity once the bitumen is applied and at rest, and will facilitate the application of a 3 mm thick layer of in one pass.
  • bitumen is not significantly affected by the addition of the structurizer.
  • the softening point the temperature at which a material softens beyond some arbitrary softness, of pure bitumen and bitumen containing 5% structurizer, was measured in accordance with ASTM D 36. Pure bitumen had a softening point of 61 °C, while the softening point of the structurized bitumen was 63 °C.
  • the penetration test in accordance with ASTM D5 - 97 is used as a measure of consistency of a bituminous material expressed as the distance in tenths of a millimeter that a 100 g standard needle vertically penetrates a sample of the material for 5 seconds at a temperature of 25 °C. Higher values of penetration indicate a softer consistency of the bituminous material. Pure bitumen had a penetration of 53 (1/10 mm) while the structurized bitumen had a penetration of 51 (1/10 mm).
  • bitumen containing materials Two bitumen containing materials were prepared, the first containing structurizer and the second being a reference material.
  • the materials were prepared as follows: bitumen was heated to 160 °C and SBS was added followed by mixing for two hours. The mixture was cooled to 100 °C, calcium carbonate, naphtha and toluene were added, and the mixture was mixed for 30 minutes while cooling to room temperature. For material 1, structurizer was also added together with the calcium carbonate. Compositions of the two materials are shown in Table 1. Table 1: Compositions of Waterproofing Materials
  • Material 1 and Reference Material 1 were subjected to the following test in accordance with ASTM D 5329: a layer of 4 mm thickness is applied to an aluminum panel, and the panel is placed in vertical position in a 60 °C oven for five hours. The flow of the layer from its initial position is measured. The permitted shift according to ASTM D 5329 is 5 mm.
  • Both Material 1 and Reference Material 1 had a flow of 0 mm. It can be seen from here that the structurizer is able to replace, at least partially, the polymer stabilizer without compromising the thermal stability of the material. This replacement of the polymer provides an economic advantage, as the polymer additive is much more expensive than the structurizer.
  • the structurizer imparts anti-stripping properties to the bitumen composition. Since the structurizer is a surfactant, it facilitates binding of the hydrophobic bitumen to the hydrophilic surfaces such as stone and metal. This superior binding prevents the stripping phenomenon described hereinabove that is common in unmodified and polymer-modified bitumen compositions.
  • bitumen containing materials Two bitumen containing materials were prepared, the first containing structurizer and the second being a reference material containing fibers.
  • the materials were prepared as follows: bitumen was heated to 160 °C and APP was added followed by mixing for two hours. The mixture was cooled to 100 °C, calcium carbonate was added, together with glass fibers for Reference Material 2 and structurizer for Material 2, and the mixture was mixed for 30 minutes while cooling to room temperature. Compositions of the two materials are shown in Table 2.
  • Material 2 and Reference Material 2 were subjected to the following test in accordance with ASTM D 5329: a layer of 4 mm thickness is applied to an aluminum panel, and the panel is placed in vertical position in a 60 °C oven for five hours. The flow of the layer from its initial position is measured. The permitted shift according to ASTM D 5329 is 5 mm.
  • Both Material 2 and Reference Material 2 had a flow of 0 mm. It can be seen from here that the structurizer is able to replace, at least partially, the polymer stabilizer and to completely replace the fiber stabilizer without compromising the thermal stability of the material. This replacement of the polymer provides an economic advantage and imparts anti-stripping properties to the material. Removing fibers from the composition improves the mixing properties as the increase in viscosity caused by the fibers is avoided.
  • bitumen containing materials Two bitumen containing materials were prepared, the first containing structurizer and the second being a reference material containing a commercial anti- stripping agent.
  • the materials were prepared as follows: bitumen was heated to 100 °C and naphtha was added. Carbon black and Wetfix® N were added for Reference Material 3, and structurizer was added for Material 3. The mixture was mixed for 30 201
  • compositions of the two materials are shown in Table 3.
  • Material 3 and Reference Material 3 were subjected to the following test in accordance with ASTM D 714: a steel plate is covered with a 100 micron thick layer of the material and placed in 15% concentration solution of NaCl in water at 60 °C for one week. The plates are then observed for signs of blistering.

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

Abstract

Des compositions de bitume stabilisées ayant des propriétés améliorées sont décrites. Le bitume est stabilisé par une composition comprenant de la porcelanite minérale et un agent d'activation. Les compositions selon l'invention sont stables et satisfont les critères de performance selon les normes nationales. Elles ont des propriétés viscoélastiques et anti-désenrobage supérieures et sont plus économiques que les compositions de bitume stabilisées existantes.
PCT/IL2012/000204 2011-05-24 2012-05-24 Compositions de bitume stabilisées, leur procédé de production et leur utilisation à titre de matériaux de construction Ceased WO2012160553A1 (fr)

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US201161489341P 2011-05-24 2011-05-24
US61/489,341 2011-05-24

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020114940A1 (en) * 2000-11-29 2002-08-22 Clemens Paul L. Engineered composite system, system component compositions, and methods of use
US20100255982A1 (en) * 2009-04-07 2010-10-07 D.S.I. - Dimona Silica Industries Ltd. Composition for improving the stability and operational performance and reducing the environmental impact of asphalt mixes
CN101948622A (zh) * 2010-09-21 2011-01-19 东南大学 一种环保型沥青再生剂及其制备方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020114940A1 (en) * 2000-11-29 2002-08-22 Clemens Paul L. Engineered composite system, system component compositions, and methods of use
US20100255982A1 (en) * 2009-04-07 2010-10-07 D.S.I. - Dimona Silica Industries Ltd. Composition for improving the stability and operational performance and reducing the environmental impact of asphalt mixes
CN101948622A (zh) * 2010-09-21 2011-01-19 东南大学 一种环保型沥青再生剂及其制备方法

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