GB2208270A - Process for breaking an emulsion - Google Patents

Process for breaking an emulsion Download PDF

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Publication number
GB2208270A
GB2208270A GB8817512A GB8817512A GB2208270A GB 2208270 A GB2208270 A GB 2208270A GB 8817512 A GB8817512 A GB 8817512A GB 8817512 A GB8817512 A GB 8817512A GB 2208270 A GB2208270 A GB 2208270A
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GB
United Kingdom
Prior art keywords
emulsion
breaking
agent
process according
microcapsules
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.)
Granted
Application number
GB8817512A
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GB8817512D0 (en
GB2208270B (en
Inventor
Patrick Mondi
Michel Ullman
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APPLIC DES DERIVES de l ASPHAL
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APPLIC DES DERIVES de l ASPHAL
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Publication of GB8817512D0 publication Critical patent/GB8817512D0/en
Publication of GB2208270A publication Critical patent/GB2208270A/en
Application granted granted Critical
Publication of GB2208270B publication Critical patent/GB2208270B/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L95/00Compositions of bituminous materials, e.g. asphalt, tar, pitch
    • C08L95/005Aqueous compositions, e.g. emulsions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D17/00Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02Separation of non-miscible liquids
    • B01D17/04Breaking emulsions
    • B01D17/047Breaking emulsions with separation aids
    • EFIXED CONSTRUCTIONS
    • E01CONSTRUCTION OF ROADS, RAILWAYS, OR BRIDGES
    • E01CCONSTRUCTION OF, OR SURFACES FOR, ROADS, SPORTS GROUNDS, OR THE LIKE; MACHINES OR AUXILIARY TOOLS FOR CONSTRUCTION OR REPAIR
    • E01C19/00Machines, tools or auxiliary devices for preparing or distributing paving materials, for working the placed materials, or for forming, consolidating, or finishing the paving
    • E01C19/02Machines, tools or auxiliary devices for preparing or distributing paving materials, for working the placed materials, or for forming, consolidating, or finishing the paving for preparing the materials
    • E01C19/10Apparatus or plants for premixing or precoating aggregate or fillers with non-hydraulic binders, e.g. with bitumen, with resins, i.e. producing mixtures or coating aggregates otherwise than by penetrating or surface dressing; Apparatus for premixing non-hydraulic mixtures prior to placing or for reconditioning salvaged non-hydraulic compositions
    • E01C19/1059Controlling the operations; Devices solely for supplying or proportioning the ingredients
    • E01C19/1063Controlling the operations
    • EFIXED CONSTRUCTIONS
    • E01CONSTRUCTION OF ROADS, RAILWAYS, OR BRIDGES
    • E01CCONSTRUCTION OF, OR SURFACES FOR, ROADS, SPORTS GROUNDS, OR THE LIKE; MACHINES OR AUXILIARY TOOLS FOR CONSTRUCTION OR REPAIR
    • E01C7/00Coherent pavings made in situ
    • E01C7/08Coherent pavings made in situ made of road-metal and binders
    • E01C7/18Coherent pavings made in situ made of road-metal and binders of road-metal and bituminous binders

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  • Chemical & Material Sciences (AREA)
  • Structural Engineering (AREA)
  • Engineering & Computer Science (AREA)
  • Civil Engineering (AREA)
  • Architecture (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Materials Engineering (AREA)
  • Road Paving Structures (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Sealing Material Composition (AREA)

Description

1. 4 4 Cl$ 6) Sf-, PROCESS FOR BREAKING AN EMULSION The invention relates
to the breaking of cationi emulsions, and more particularly of bituminous emulsions
employed in the field of road surfacings. it surfacings
0;; A 25 Y is general practice to prepare binders for road in the form of cationic bituminous emulsions comprising an aqueous dispersant phase, it being necessary to break this emulsion to impart the desired physical and mechanical properties to the road surfacing.
To break an emulsion it is known to add thereto a breaking agent, that is to say a substance capable of diffusing homogeneously within the emulsion, and whose physical andlor chemical action makes the emulsion unstable and causes it to break. Since cationic emulsions are, in principle, acidic in nature and are stable only at a tow pH, a basic breaking agent, which raises the pH of the medium. is commonly empLoye,d.
Bringing the breaking agent into contact with the emulsion causes the latter to break immediately. In the case of road surfacings, the bituminous binder inust remain in the emulsion form to permit it to be handled until it is spread onto the road, and it is then very difficult to disperse the breaking agent homogeneously therein in order to produce uniform breaki ng. For this reason, use is generally made of emulsions of Limited stability, which break spontaneously after a certain time.
However, the breaking rate of the emulsions depends on many factors such as ambient temperature, the temperature of the ground, of the aggregates and of the emulsion, and on the moisture content of the atmosphere and of the aggregatesp with the result that there is a risk that the breaking may take place sooner or later than desired.
The present invention seeks to permit the breaking of a cationic emulsion at a desired precise time, and especially the breaking of a bituminous emulsion soon after it has been spread onto a road.
The present invention provides a process for breaking a cationic emulsion by dispersing in it microcapsules containing a breaking agent, the outer casing of the microcapsules comprising a substance susceptible to attack chemically and/or physically by the emulsion to release the breaking agent after a pre-determined period of contact with the emulsion. Since the approximate period taken to release the breaking agent is known the microcapsules may be introduced into and dispersed in the emulsion at a time which ensures that the breaking occurs at the desired time.
The microcapsules or the microspheres are obtained in a known mannert by enclosing the breaking agent by adding a thin layer of a suitable substance.
Since the emulsion generally comprises an aqueous phase, a substance capable of being attacked by water may be TI 1 1 1-, 3 - chosen for the outer casing, that is to say one which dissolves or disintegrates on contact with water, or water-permeable substance. In the case of an emulsion which is acidic in nature. a substance capable of being attacked by acidic solutions may be chosen.
Sugars (especially glucose), silicates, celluLose-based polymers and various synthetic polymers such as polyisoprene, acrylic polymers and ethylenelvinyl acetate copolymers may be mentioned as substances which are sensitive to water and to acids and which can be employed with acidic aqueous emulsions, no limitation being implied by this List.
As indicated above, in the case of an acidic emulsion, the breaking agent is typically a basic agent.
It is preferred that the breaking agent comprises-an agent with strong action, - especi-ally a strong base such as sodium hydroxide, and an agent with mild action especially an intermediate or weak base such as calcium oxide, which are present in separate microcapsuLes and are released in succession. so that the breaking of the emulsion is initiated by the mild agent and continued or-finished by the energetic agent.
It has been observed in fact that. when the break ing of a bituminous emulsion is initiated in the presence of a strong base, Lumps of bitumen are sometimes formed instead of a continuous film and that. if a base which is too weak is employed. the breaking may be incomplete.
f - 4 This probLem is overcome by reLeasing an intermediate or weak base and a strong base in succession.
To this end, the microcapsuLes of both types may be introduced at the same time and may reLease the break- ing agents after different periods, for exampLe by virtue of different waLL thicknesses. The microcapsuLes may aLso be introduced in succession.
It is possibLe to empLoy breaking agents in gaseous form, for exampLe ammonia, breaking agents in Liquid form, for exampLe sodium hydroxide in soLution in water, and breaking agents in pasty form or in a divided soLid form, for exampLe saLts of a basic nature, such as carbonates, chLorates, perchLorates, basic nitrates or trimetaL phosphates, it being possibLe for different agents to be optionaLLy combined in different forms.
However, the microencapsulation of gases is a technology which is still relatively undeveloped. Microcapsules whose outercasings are susceptible to attack by water are used with breaking agents in aqueous solution.
moreover basic salts are not always sufficiently energetic in their action.
it is therefore preferred to use in the microcapsules a breaking agent in the form of a Liquid immobiLized in and/or at the surface of a soLid support, especiaLLy of powder, the combination formed by the said Liquid and the soLid support having the behaviour of a soLid. A combination of this kind, known by the 4 M, 1 z, 0 1 Z W I name of "dry Liquid", h as the appearance of a homogeneous solid and handles Like a powder, and may be placed in contact with a substance capable of being attacked by the liquid which forms part of it, without this substance being appreciably attacked. - The powder support employed may be advantageously a micronized and porous- precipitated silica such as that marketed by Degussa under the reference Sipernat 50. A support of this kind may absorb into its pores and adsorb on its surf ace e.g. a sodium hydroxide solution to which a wetting agent has been added, in a quantity which is greater than its own weight, to give a dry Liquid.
As described above the breaking process is particularly useful in a situation where the emulsion to be broken has already been placed in position making it difficult to apply subsequently a breaking agent and achieve a homogeneous dispersion thereof. To obtain'uniform breaking after the application of the emulsion is complete, the microcapsules are dispersed in the emulsion beforehand by mixing. This applies especially to bituminous emulsions intended for the production of a road-surface binder, the breaking taking place after the binder has been spread onto a road or other surface.
When the binder is to be combined with solid particles, for example with aggregates or granulates, in a road surfacing, the microcapsules may be dispersed in the emulsion at the saffle time as these aggregates.
By way of example, a caustic solution having the following composition by weight may be employed as a breaking agent:
sodium LauryL sulphate 2 % - sodium hydroxide in PeLLet form 10 % - S 200 P base marketed by Barnier in Valence 2 % - water 86 % The S 200 P base is an aLk.yLamidoimidazopoLyamine which contributes to the alkalinity of the solution and has, like sodium lauryl sulph-ate, surface-active properties which make it easier to disperse the solution in the emulsion to be broken, especially in contact with the granulates which may be mixed therein. Other poLyamines may be employed as a replacement for the S 200 P base. 15 100 parts by weight of the caustic solution are combined with 75 parts by weight of Sipernat 50 to produce a dry Liquid which is then microencapsuLated under a ceLLuLose-based outer casing of appropriate thickness, for exampLe between 150 and 500 micrometres. 20 When 0.5 to 1.5 parts by weight of this dry Liquid, depending on the composition of the emulsion, are introduced in the form of microcapsuLes into 100 parts by weight of the emulsion, immediate and clean breaking of the Latter is obtained after the period of attack on the outer casing.
In another example, a breaking agent containing an agent with utild action -and an agent with strong ne 1 k 4 Z X 11 Ir 1,1 9 - 7 1 action is employed. The 100 parts by weight of caustic solution of the preceding example are then replaced with 60 parts of calcium alginate, encapsulated with an acrylic polymer, and 40 parts of sodium hydroxide solution, e ncapsulated with the same polymer, and with capsule. thicknesses which are 30% greater. The 75 parts of Sipernat 50 remain unchanged.
In the preceding examples, the composition of the bituminous emulsion which may be employed may be the fol- towing: 1801220 bitumen, 600 kg; CECCA polyram S, 4 kg; HCL, 6 kg; and water q.s. 1 tonne.
An example of application of the invention is the production of a bituminous grout, manufactured on site from aggregates and a bitumen emulsion which, in order to make use of the invention, contains emulsifiers and, optionally, other additives endowing it with a high stability at a pH of between 2 and 5.
These constituents are mixed in a continuous mixer with two horizontal shafts and the mixture is cast on the ground from a sLed which is responsible for distributing and metering it out onto the surface to be coveted. The bitumen must remain in emulsion form during these opera tions. but the breaking inust be produced after 10 to 15 minutes, for example, in order to restart the traffic.
To this end. an appropriate quantity. depending on the emulsion characteristicso of the microcapsules described above, whose outer casing thickness is chosen so as to release the breaking agent during the 10 to 15 minutes which follow the spreading of the mixture, is in troduced into the emulsion during or immediately before its passage through the mixer.
Obviously, the application of the invention is not Limited to the example which has just been described. It extends to all the cases of coating of materials (cold open-grain mixes, emulsion base course, cold dressing mixes) and to the cases of asphalt spreading, particularly when a spreading emulsion is applied during uncertain weather. The invention can also find application in different technical fields where problems similar to those encountered with the bituminous road-surface binders may arise.
1 1 61 1

Claims (13)

1. Process for breaking a cationic emulsion by dispersing in it microcapsules containing a breaking agent, the outer casing of the microcapsules comprising a substance susceptible to attack chemically and/or physically by the emulsion to release the breaking agent after a pre-determined period of contact with the emulsion.
2. Process according to claim 1, in which the emulsion comprises an aqueous phase and the substance of outer casing is susceptible to attack by water.
3. Process according to claim 1 or 2, in which the emulsion is acidic and the substance of the outer casing is susceptible to attack by acidic solutions.
4. Process according to claim 3, in which the breaking agent is basic.
is
5. Process according to any one of the preceding claims. in which the breaking agent comprises an agent strong action and an agent with mild action, which are present in separate microcapsules and are released in succession, so that the breaking of the emulsion is initiated by the mild agent and continued by the strong agent.
6. Process according to claim 5, in which the strong agent is a strong base and the mild agent is an intermediate or weak base.
1 - 10
7. Process according to any one of the preceding claims, in which the breaking agent in the microcapsules is in the form of a liquid immobilized in and/or at the surface of a solid support, the combination formed by the said liquid and the solid support having the behaviour of a solid.
8. Process according to claim 7, in which the solid support is based on a micronsized and porous silica.
9. Process according to any one of the preceding claims, in which the microcapsules are dispersed in the emulsion by mixing and the breaking takes place while the mixture obtained is at rest.
10. Process according to any one of the preceding claims, in which the emulsion is a bituminous emulsion suitable for the production of a road-surface binder.
11. Process according to claim 10, in which the breaking of the emulsion takes place after the binder has been spread onto a surface.
12. Process according to claim 10 or 11, in which the microcapsules are dispersed in the emulsion at the same time as solid particles intended to be combined with the binder in a road surfacing.
13. Process for breaking a cationic emulsion substantially as hereinbefore described.
Pab'isiied 1985 a, T--e Paten- Office. S-=-,e Hc-.;Sc 667^ F_c' 4TF cc:)ie= mav ve dbza.ne: f:,= -!- Pa:,en- Offcc SaIeE Branch, St Mary Cray, Orpington, Kent BR5 3RD- Printed Iky MWtiplex techniques Itd. St Mary Crky. Kenz. Con. 187 f-1 Q
GB8817512A 1987-07-24 1988-07-22 Process for breaking an emulsion Expired - Fee Related GB2208270B (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR8710592A FR2618350B1 (en) 1987-07-24 1987-07-24 METHOD FOR CAUSING THE BREAKAGE OF AN EMULSION USING A BREAKING AGENT

Publications (3)

Publication Number Publication Date
GB8817512D0 GB8817512D0 (en) 1988-08-24
GB2208270A true GB2208270A (en) 1989-03-22
GB2208270B GB2208270B (en) 1991-03-06

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ID=9353579

Family Applications (1)

Application Number Title Priority Date Filing Date
GB8817512A Expired - Fee Related GB2208270B (en) 1987-07-24 1988-07-22 Process for breaking an emulsion

Country Status (5)

Country Link
CH (1) CH677451A5 (en)
ES (1) ES2007260A6 (en)
FR (1) FR2618350B1 (en)
GB (1) GB2208270B (en)
IT (1) IT1223716B (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1994010247A1 (en) * 1992-11-02 1994-05-11 Aktiebolaget Nynäs Petroleum Bitumen emulsion, its preparation and use and breaking additive for use therein
US5474607A (en) * 1990-05-07 1995-12-12 Emoleum (Australia) Limited Bitumen emulsions
US6106604A (en) * 1997-03-10 2000-08-22 Colas Bitumen emulsion, process of producing a bitumen emulsion and process of producing a bituminous material for the construction or maintenance of pavements
WO2001057139A1 (en) * 2000-02-07 2001-08-09 Tieliikelaitos Emulsion surfacing mix for paving a road, and a road surfacing made thereof

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ES2050601B1 (en) * 1992-06-10 1994-12-16 Espanola Explosivos PROCEDURE FOR THE RUPTURE OF EXPLOSIVE EMULSIONS.

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1594762A1 (en) * 1965-03-03 1970-05-21 Wm Hilgers Chem Fabrik Process for the production of bituminous coatings on road surfaces using a hose
US4194023A (en) * 1978-09-22 1980-03-18 Mobil Oil Corporation Controlled deposition of asphalt emulsions
US4202795A (en) * 1978-09-28 1980-05-13 Halliburton Company Methods and additives for delaying the release of chemicals in aqueous fluids
FR2573455B1 (en) * 1984-11-21 1986-12-26 Colas Sa PROCESS FOR OBTAINING SURFACE ROAD COATINGS BY SPREADING AQUEOUS BITUMEN EMULSIONS AND COATINGS OBTAINED

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5474607A (en) * 1990-05-07 1995-12-12 Emoleum (Australia) Limited Bitumen emulsions
US5518538A (en) * 1990-05-07 1996-05-21 Emoleum (Australia) Limited Bitumen emulsions
WO1994010247A1 (en) * 1992-11-02 1994-05-11 Aktiebolaget Nynäs Petroleum Bitumen emulsion, its preparation and use and breaking additive for use therein
CN1058740C (en) * 1992-11-02 2000-11-22 阿克逖博拉盖特·尼纳斯石油公司 Asphalt emulsion, preparation and application thereof, and demulsification additive used therein
US6106604A (en) * 1997-03-10 2000-08-22 Colas Bitumen emulsion, process of producing a bitumen emulsion and process of producing a bituminous material for the construction or maintenance of pavements
WO2001057139A1 (en) * 2000-02-07 2001-08-09 Tieliikelaitos Emulsion surfacing mix for paving a road, and a road surfacing made thereof

Also Published As

Publication number Publication date
IT8867697A0 (en) 1988-07-22
CH677451A5 (en) 1991-05-31
GB8817512D0 (en) 1988-08-24
IT1223716B (en) 1990-09-29
FR2618350B1 (en) 1991-07-12
ES2007260A6 (en) 1989-06-01
FR2618350A1 (en) 1989-01-27
GB2208270B (en) 1991-03-06

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Legal Events

Date Code Title Description
PCNP Patent ceased through non-payment of renewal fee

Effective date: 19930722