Synthetic resins or natural rubbers -- part of the class 520 ser – Synthetic resins – At least one aryl ring which is part of a fused or bridged...
Reexamination Certificate
2001-08-27
2004-07-27
Szekely, Peter (Department: 1714)
Synthetic resins or natural rubbers -- part of the class 520 ser
Synthetic resins
At least one aryl ring which is part of a fused or bridged...
C524S474000, C524S475000, C524S476000, C524S477000, C524S499000, C524S526000, C524S552000
Reexamination Certificate
active
06767957
ABSTRACT:
This invention relates to new synthetic bitumen oil-water emulsions that are essentially made of clear synthetic binders that do not contain any asphaltenes and of polymers, as well as the preparation thereof. The invention also relates to the applications of said emulsions in the manufacture of surface treatments that can be colored, in particular for pigmented dampproofing materials such as colored sealing coats for roofs, as well as for roadway usage.
It is common in prior the art, to use clear synthetic binders, that have, with the exception of the coloring, characteristics that are close to those of natural bitumens (from crude oil, oil shales, heavy oils, bituminous sands, etc . . . obtained in particular by distillation and deasphalting of the heavy fraction resulting from the distillation), in the manufacture of colored coatings. Said clear binders do not contain any asphaltenes and can be obtained in particular, as described in the European patent EP 179 510, through a mixture of a mineral lubricating oil extract and a modified oil resin and/or coumarone-indene resin. They are used to make pigmentable compositions, mixed with colored pigments and possibly other polymers. They are set up using complicated techniques under heat that take a lot of energy.
It is also common knowledge to emulsify natural bitumens, so as to be able to use them in techniques called “cold” techniques for roadway applications.
Furthermore, we can also make clear synthetic binder oil-water emulsions, with aggregates and colored pigments, to make colored coatings designed for roadway or urban surfaces that are placed “cold.” However, if, for other applications, we wish to increase the performance of the binder, in particular its cohesiveness and/or its softening point (or “ball-ring” temperature) by adding polymers, the polymer ratio is rapidly limited to a threshold of approximately 7% by weight. This limit stems from the high viscosity of the modified binders obtained, that makes their emulsification very difficult, if not impossible, under common temperature and pressure conditions implemented in the manufacturing procedures.
This is the case in particular in the European patent EP 0 604 258, which belongs to the applicant, and describes an example for obtaining a bitumen-polymer oil-water emulsion, in which the bitumen can be a synthetic bitumen, to which is added a polymer, that is grafted or reticulated in situ under heat in the bitumen. The ratio of polymer in the emulsion does not exceed 5% by weight and the preparation procedure requires a relatively complex implementation.
The applicant has established that, surprisingly, through the emulsification of a clear synthetic binder in combination with at least one compound of the latex family, we can obtain an enhanced synthetic bitumen emulsion particularly advantageous thanks to its especially high polymer content, while maintaining a viscosity that is satisfactory, which makes its implementation easier in particular for the applications using techniques called “cold”. This emulsion is particularly advantageous in making surface treatments or layers, in particular colored, and it provides these coatings with increased characteristics, thanks to the high ratio of polymer that can be incorporated, in particular concerning their softening point, their cohesion, their resistance to aging, as well as an enhanced rheological behavior.
Thus the invention's first object is a synthetic bitumen emulsion that can be used namely in the making of colored coatings, made essentially of clear binders and possibly of colored pigments, characterized by the fact that it contains:
at least one clear synthetic binder whose softening point or Ball-Ring Temperature (TBT), measured according to the NFT 66-008 standard, that ranges between 30 and 100° C.,
at least one compound of the latex family, introduced in a quantity that ranges between 3 and 40% by weight of the emulsion,
water
and at least one emulsifying agent
More particularly, the compound of the latex family is chosen from among the acrylic polymers or the natural or synthetic rubbers that can be used in the form of an aqueous dispersion such as:
EPDM (ethylene-propylene-diene-monomer),
EPM (ethylene-propylene monomer),
S.B.R. (styrene-butadiene rubber) statistic or S.B.S. (styrene-butadiene-styrene) sequenced, linear or star-shaped, or S.I.S. (styrene-isoprene-styrene) styrene-butadiene copolymers,
polyisobutylene,
polybutadiene,
polyisoprene,
polychloroprene.
Preferably, the compound of the latex family is introduced in a quantity that ranges between 5 and 30% by weight of the emulsion.
In a first method of execution, the clear synthetic binder contains at least one plasticizing agent with an aromatic extract base from a petroleum fraction and at least one structuring agent with an oil resin base.
However, the clear synthetic binder can also contain at least one plasticizing agent with an aliphatic hydrocarbonic compound base whose number of carbon atoms is greater than or equal to 20, and at least one structuring agent with a cycloaliphatic hydrocarbonic polymer.
The plasticizing agent used in the context of this invention, is preferably chosen from among:
a) natural or synthetic aliphatic oils
b) polymers with a low degree of polymerization, such as polyolefins.
In particular, the aliphatic oils have an aniline point that is greater than or equal to 90° C. (according to the ASTM D 611 method) and, preferably greater than or equal to 110° C.
Preferably, these aliphatic oils are chosen from among the hydrogenated white oils, that contain at least 60% of paraffin base carbon atoms (according to the ASTM D 2140 method).
The polymers that constitute the plasticizing agent have a viscosity index (VI) (according to the ASTM D 2270 method) that is greater than or equal to 100 and preferably greater than or equal to 120.
Preferably, these polymers are of the polybutene type, whose molecular mass number ranges between 900 and 2600 and whose cinematic viscosity at 100° C. (according to the ASTM D 445 method) ranges between 200 and 4600 cSt (200 to 4600 mm
2
/s).
The structuring agent as set forth in the invention is a polycycloaliphatic thermoplastic resin, in particular of the polycyclopentane type, with a low molecular mass.
More particularly, the polycyclopentane type thermoplastic resin has a softening point (or Ball-Ring temperature, TBA, measured according to the NFT 66-008 standard) that is greater than 125° C. and a Gardner color index (according to the NFT 20-030 standard) of at the most 1.
The ratio by weight between the structuring agent and the plasticizing agent, as set forth in the invention, advantageously ranges between 0.4 and 1.5.
As set forth in the invention, the plasticizing agent is used in a quantity that ranges between 40 and 70% by weight of the clear synthetic binder.
The clear synthetic binder, as defined above, has a penetrability that ranges between 20 and 300 tenths of a mm (according to the NF T66-044 standard).
In addition, the clear synthetic binder of the emulsion as set forth in the invention can contain either vinyl ethylene-acetate (EVA) or S.B.S. sequenced styrene-butadiene type copolymers, or low density polyethylene type polymers. The incorporation of these polymers proves useful in hardening the binder, reducing the penetrability values and strengthening the cohesion.
Thus, in order to perform the emulsion as set forth in the invention, the applicant successfully used a non ionic or cationic, polychloroprene latex emulsion, with a concentration of dry matter of 55 to 59% and a specific mass that ranges between 1.09 and 1.14 g/cm
3
.
The emulsion as set forth in the invention can contain, preferably:
between 40 and 70% by mass of synthetic binder
between 5 and 30% by mass of latex
between 60 and 30% by mass of water
between 3 and 10% by mass of emulsifying agent
The preparation of the emulsion as set forth in the invention requires the use of an emulsifier, that is preferably cationic or non ionic. A range of preferred emulsifiers consists, for example, of emulsifi
Gillet Jean-Philippe
Jolivet Yannick
Lemoine Guy
Szekely Peter
Total Raffinage Distribution , S.A.
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