Rubber composition comprising phenolic resin

FIELD: chemistry.

SUBSTANCE: invention relates to a rubber composition, which can be used, in particular, in tyres based on at least one diene elastomer, one reinforcing filler, one cross-linking system, one phenolic resin and one polyaldehyde, where the phenol resin fraction ranges between 2 and 15 phr, and the polyaldehyde fraction ranges between 1 and 20 phr. The use of polyaldehyde makes it possible to advantageously replace conventional methylene donors while preventing the production of formaldehyde during the vulcanization of the rubber compositions and thus to limit the environmental impact of these compounds.

EFFECT: polyaldehyde compounds make it possible not only to obtain the rubber compositions exhibiting the same low-strain stiffness as the conventional rubber compositions using conventional methylene donors but also, to greatly improve the fatigue strength of the rubber compositions and thus the endurance of the tyres.

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The present invention relates to rubber compositions intended in particular to obtain tires or semi-finished products for tires, in particular, to rubber compositions having increased rigidity.

Aware in some parts of the tire rubber compositions having strong stiffness at low deformations of the tyre (cf WO 02/10269). The low resistance to deformation is one of the properties that should have a tire to match the loads to which it is exposed.

This increase in stiffness can be obtained by increasing the proportion of reinforcing filler or entering certain reinforcing resin in the rubber composition constituting the portion of the tire.

However, as we know, the increasing rigidity of the rubber composition by increasing the proportion of the filler may have a negative effect on the hysteresis properties and, consequently, the rolling resistance of the tyres. But the rolling resistance of the tyres are always striving to reduce to reduce fuel consumption and thus protect the environment.

Classically, this increased stiffness get, inserting a reinforcing resin system based on the acceptor/donor of methylene chloride. The expression "methylene acceptor and methylene donor" is well known to the specialist and is widely used to refer to compounds that can react with each other to re�altace condensation to form a three-dimensional reinforcing resin, which is superimposed, to form an inclusive system of reinforcing filler/elastomer, on the one hand, and system elastomer/sulfur, on the other hand (if cross-linking agent is sulphur). With the above-described acceptor methylene combine the hardener, able to sew or to cure it, also commonly called "methylene donor". Cross-linking of the resin in this case is called when the vulcanization of the rubber matrix by forming bridges (-CH2-) between carbon atoms in the ortho - and para-positions of the phenolic nuclei in the resin and methylene donor, creating, thus, a three-dimensional network resin.

Donors of methylene chloride, classically used in rubber compositions for tires, are hexamethylenetetramine (abbreviated as HMT), or hexamethoxymelamine (abbreviated HMMM or H3M), or hexadecanethiol.

However, the combination of the classically used phenolic resin, a methylene acceptor to methylene donor ΗΜΤ or Η3Μ produces formaldehyde during the curing of the rubber composition. However, the formation of formaldehyde in rubber compositions, it is desirable to reduce or even in the long term to suppress due to the environmental impact of these compounds. In conducting its study, the authors of this application have unexpectedly found that polyallelic can profitably replace the classic methylene donors�, avoiding the formation of formaldehyde. The application of these polialden connections not only allows to obtain a rubber composition having the same rigidity at low deformation, as classic rubber compositions which contain a methylene donor HMT or H3M, but, surprisingly, can significantly improve the fatigue strength of the rubber compositions and, consequently, the service life of tires.

Therefore, the first object of the invention relates to a rubber composition based on at least one diene elastomer, a reinforcing filler, a crosslinking system, a phenolic resin and polyallelic.

The object of the invention are also tire containing the rubber composition according to the invention.

The object of the invention are also finished rubber articles or semi-finished products containing rubber composition according to the invention.

The tires according to the invention are, in particular, for tourist vehicles such as two-wheelers (motorcycle, Bicycle), industrial vehicles chosen from other used trucks, heavy vehicles, i.e. underground, buses, road transport (trucks, tractors, tugs), off-road vehicles, agricultural or construction machinery, aircraft, other vehicles for transporting or handling� machine.

The invention and its advantages will be easily understood in the light of the following description and examples of implementation.

I - Test

The properties of the rubber compositions was determined before and after crosslinking as described below.

I. 1 - tensile Test

These tests allow us to determine the elastic resistance. Unless otherwise specified, they shall be conducted in accordance with French standard NF T 46-002 of September 1988. In the second elongation (i.e. after a cycle of accommodation to the degree of stretch provided for actual measurements) measured nominal secant modulus (or apparent stress, in MPa) elongation 10% (indicated by MA10). Also measured elongation at break (AR %). All these measurements are stretching under normal conditions of temperature (23±2°C) and humidity (relative humidity 50±5%), according to the French standard NF T 40-101 (December 1979).

I. 2 - Test for fatigue

Fatigue strength, expressed in number of cycles or in relative units (Rel.ed.), measured in a known manner on 12 samples subjected to repeated sprains low frequency to elongation 30%, at 23°C using the device for Monsanto (type "MFTR") held until rupture of the sample, according to ASTM D4482-85 and ISO 6943.

The result is expressed in relative units (Rel.ed.). The value above the reference values, PR�izvorno taken as 100, indicates an improved result, that is the best fatigue strength of samples of rubber.

II - Conditions for carrying out the invention

The rubber composition according to the invention is based on at least:

- diene elastomer,

- reinforcing filler,

- crosslinking system,

phenolic resin,

- polyallelic.

The expression composition "based on" should be understood as the composition comprising the mixture and/or reaction product of the various components used, and some of these basic components capable of reacting or intended to react among themselves, at least partially, at different stages of the preparation of the composition, in particular during the crosslinking or vulcanization.

In the present description, unless expressly stated otherwise, all given percentages (%) are percent by weight (%). On the other hand, the intervals of values denoted by the expression "from more than a to less than b" means the range of values that are greater than a but less than b (that is, the boundaries a and b excluded), whereas any interval of values denoted by the words "from a to b" means the range of values from greater than or equal to a less than or equal to b (i.e. including the strict limits a and b).

II.1 - Diene elastomer

The rubber composition according to the invention comprises a diene elastomer.

"Diene" e�storeroom or rubber should be understood, as you know, the elastomer (meaning one or more) derived at least in part (i.e. a homopolymer or a copolymer) from diene monomers (monomers having two double bonds of carbon-carbon, conjugated or not).

These diene elastomers can be classified into two categories: "essentially unsaturated" or "essentially saturated". Usually under the "essentially unsaturated" is understood to mean a diene elastomer obtained at least in part from conjugated diene monomers, having a proportion of diene units, or links (conjugated dienes) which is higher than 15% (mol%); so, for example, diene elastomers, as butilovyi or copolymers of dienes and alpha-olefins of the type EPDM, do not fall within the above definition and may be attributed, in particular, to "essentially saturated" diene elastomers (percent units derived from dienes, low or very low, always below 15%). In particular, in the category of "essentially unsaturated" diene elastomers, "highly unsaturated" diene elastomer is understood to mean a diene elastomer, in which the proportion of units of diene origin (conjugated dienes) above 50%.

Under these definitions under the diene elastomer that can be used in the compositions according to the invention, more specifically refers to:

(a) any homopolymer obtained polymer�ization conjugated diene monomer, containing from 4 to 12 carbon atoms;

(b) - any copolymer obtained by copolymerizing one or more conjugated dienes with each other or with one or more vinylaromatic compounds containing from 8 to 20 carbon atoms;

(c) is a terpolymer obtained by copolymerization of ethylene, α-olefin containing from 3 to 6 carbon atoms, non-conjugated diene monomer containing from 6 to 12 carbon atoms, such as, for example, the elastomers obtained from ethylene and propylene with a non-conjugated diene monomer of the type specified above, in particular, as hexadiene-1,4, ethylidenenorbornene, Dicyclopentadiene;

(d) copolymer of isobutene and isoprene (butyl rubber) and also the halogenated versions of this type of copolymer, in particular chlorinated or brominated.

Although applicable to any type of diene elastomer, a specialist in tyres should be understood that the present invention is preferably used with essentially unsaturated diene elastomers, in particular of type (a) or (b) above.

As conjugated dienes are suitable, in particular, 1,3-butadiene, 2-methyl-1,3-butadiene, 2,3-di(C1-C5-alkyl)-1,3-BUTADIENES, such as 2,3-dimethyl-1,3-butadiene, 2,3-diethyl-1,3-butadiene, 2-methyl-3-ethyl-1,3-butadiene, 2-methyl-3-isopropyl-1,3-butadiene, an aryl-1,3-butadiene, 1,3-pentadien�, 2,4-hexadien. As vinylaromatic compounds are suitable, for example, styrene, ortho-, meta-, para-methylsterol, the commercial mixture "vinyl-toluene", para-tert-butalbiral, methoxystyrene, chloresterol, minimization, divinylbenzene, vinylnaphthalene.

The copolymers may contain between 99% to more than 20 wt.% diene units and from 1% to less than 80 wt.% vinylaromatic links. The elastomers may have any microstructure which depends on the polymerization conditions, in particular, from the presence or absence of the modifier and/or agent of randomization and the amount of modifier and/or agent of randomization. The elastomers may for example be block, statistical, sequenced, microsectioning, and can be prepared in dispersion or in solution; they may be bound and/or star-shaped, or may be functionalized binder agent and/or agent of star formation, or functionalization agent. To bind with the carbon black include, for example, a functional group containing a bond of C-Sn, or a functional amino group, such as benzophenone; to associate with an inorganic reinforcing filler such as silica, can be called, for example, of silanol or polysiloxane functional groups having at the end of silanol combined with caffeine (ka�s described, for example, in documents FR 2740778 or US 6013718), the alkoxysilane group (which is described for example in FR 2765882 or US 5977238), carboxyl group (which is described for example in WO 01/92402 or in US 6815473, WO 2004/096865 or US 2006/0089445) or groups of simple ether (which is described for example in EP 1127909 or US 6503973). As other examples of functionalized elastomers can also be called elastomers epoxy type (such as SBR, BR, NR or IR).

Suitable polybutadiene, in particular, those that have content (in mole %) of units -1,2 ranges from over 4% to less than 80%, or in which the content (mol%) of CIS-1,4 links above 80%, polyisoprene, butadiene-styrene copolymers, in particular having a Tg (glass transition temperature, Tg is measured according to ASTM D3418) in the range from 0°C to more than -70°C, in particular from less than -10°C to more than -60°C, the styrene content is more than 5% to less than 60 wt.%, in particular, from over 20% to less than 50%, a content (mol%) of -1,2 linkages in butadiene portion is from over 4% to less than 75%, a content (mol%) bonds TRANS-1,4 ranges from over 10% to less than 80%; copolymers of butadiene with isoprene, in particular, those in which the content of isoprene is from over 5% to less than 90 wt.%, and Tg is in the range from less than -40°C up to more than -80°C, copolymers of isoprene with styrene, in particular, those in which the styrene content is from 5% to less than 50 wt.%, and sost Tg�possessing from less than -25°C to more than -50°C. In the case of the copolymers of butadiene-styrene-isoprene suitable, in particular, copolymers having a styrene content from 5% to 50 wt.%, in particular, from over 10% to less than 40%, the content of isoprene is from over 15% to less than 60 wt.%, in particular, from over 20% to less than 50%, a butadiene content is from 5% to less than 50 wt.%, in particular, from over 20% to less than 40%, a content (molar %) of units -1.2 V butadiene part is from over 4% to 85%, a content (mol%) of links of the TRANS-1,4 butadiene in part is from over 6% to less than 80%, the total content (mol%) of units -1,2 -3,4 and in isoprene portion constitutes from 5% to less than 70%, and the content (mol%) of links of the TRANS-1,4 in isoprene portion ranges from over 10% to less than 50%, and, more generally, the copolymer is a butadiene-styrene-isoprene has a Tg in the range from less than -20°C up to more than -70°C.

In total, the diene elastomer of the composition according to the invention is preferably selected from the group of highly unsaturated diene elastomers consisting of polybutadienes (abbreviated to "BR"), synthetic polyisoprenes (IR), natural rubber (NR), copolymers of butadiene, copolymers of isoprene and mixtures of these elastomers. Such copolymers are more preferably selected from the group consisting of styrene-butadiene copolymers (SBR), copolymers of isoprene with butadiene (BIR), copolymers of isoprene with styrene (SIR) and�polymers of isoprene-butadiene-styrene (SBIR).

According to one private variant implementation, the diene elastomer is predominantly (i.e. more than 50 phr, phr=parts by weight per hundred parts of rubber) consists of an SBR, whether an SBR obtained in emulsion ("ESBR") or SBR obtained in solution ("SSBR"), or a mixture (blend) of SBR/BR, SBR/NR (or SBR/IR), BR/NR (or BR/IR), or SBR/BR/NR (or SBR/BR/IR). In the case of elastomer SBR (ESBR or SSBR) is used, in particular, SBR, whose average styrene content is, for example, from over 20% to less than 35 wt.%, or SBR with a high styrene content, for example, from 35 to 45%, and the content of vinyl bonds in the butadiene portion ranges from 15% to less than 70%, a content (in mol%) bonds TRANS-1,4 ranges from 15% to less than 75%, and Tg is below -10°C and above to -55°C; such an SBR can profitably be used in a mixture with a BR preferably having more than 90% (mol%) bonds CIS-1,4.

"Isoprene elastomer" is understood, as is known, the homopolymer or copolymer of isoprene, in other words a diene elastomer selected from the group consisting of natural rubber (NR), which can be plasticized or patitirion, synthetic polyisoprenes (IR), various copolymers of isoprene and mixtures of these elastomers. From copolymers of isoprene call, in particular, copolymers of isobutene-isoprene (butyl rubber - IIR), isoprene-styrene (SIR), isoprene-butadiene (BIR) or isoprene-butadiene�ene-styrene (SBIR). This isoprene elastomer is preferably natural rubber or synthetic CIS-1,4-polyisoprene; from these synthetic polyisoprenes preferably used polyisoprene, which is the proportion (mol%) bonds CIS-1,4 above 90%, even more preferably above 98%.

According to another preferred embodiment of the invention, the rubber composition comprises a blend of (one or more) diene elastomer, called "high Tg, which Tg is more from -70°C to 0°C, and (one or more) diene elastomer, called "low Tg", component more from -110°C to less than -80°C, more preferably from more than -105°C to less than -90°C. with high Tg Elastomer is preferably selected from the group consisting of S-SBR E-SBR, natural rubber, synthetic polyisoprenes having a proportion (mol%) units CIS-1,4 preferably above 95%, from BIR SIR, SBIR and mixtures of these elastomers. An elastomer having a low Tg, preferably contains a butadiene units in the proportion (mol%), at least equal to 70%; preferably it consists of a polybutadiene (BR) having a proportion (mol%) of sequences of CIS-1,4 above 90%.

According to another private embodiment of the invention, the rubber composition comprises, for example, from 30 to 100 phr (per 100 parts of polymer), in particular from 50 to 100 phr of elastomer with a high Tg in a mixture to 70 phr, in particular, 0-50 phr, of an elastomer having a low Tg; according to another example, it contains a total of 100 phr of one or more SBR obtained in solution.

According to another private embodiment of the invention, the diene elastomer of the composition according to the invention contains a mixture of BR (as an elastomer having a low Tg) having a proportion (mol%) units CIS-1,4 above 90%, with one or more S-SBR or E-SBR (as of elastomer(s) with high Tg).

The composition of the invention may contain a single diene elastomer or a mixture of several diene elastomers, wherein the diene elastomer or elastomers can be used in combination with any type of synthetic elastomer, non-diene, and even with other polymers other than elastomers, for example thermoplastic polymers.

II.2 - Reinforcing filler

You can use any type of reinforcing filler known for its ability to reinforce a rubber composition suitable for obtaining tires, for example an organic filler such as carbon black, a reinforcing inorganic filler, such as silica, or a mixture of these two types of fillers, in particular a mixture of carbon black and silica.

As carbon black suit all kinds of carbon black, in particular, carbon black of the type HAF, ISAF, SAF, usually used in the tire (soot, called with�Jay varieties for tires). Of these the last call, in particular, carbon black series 100, 200 or 300 (brand according to ASTM), such as carbon black N115, N134, N234, N326, N330, N339, N347, N375, or, depending on the intended application, soot higher series (for example, N660, N683, N772). For example, soot could be introduced already in the isoprene elastomer in the form of masterbatches (see, for example, applications WO 97/36724 or WO 99/16600).

As examples of organic fillers that are different from soot, carbon, can be called organic fillers of functionalized polyvinyl, which is described in applications WO-A-2006/069792, WO-A-2006/069793, WO-A-2008/003434 and WO-A-2008/003435.

"Reinforcing inorganic filler" in the present application, by definition, should be understood as any inorganic or mineral filler, whatever its colour and its origin (natural or synthetic), also referred to as "white" or "light" filler and even nesheim filler ("non-black filler"), which, in contrast to carbon black, capable of independently, i.e., without other means, such as an intermediate bonding agent, reinforcing a rubber composition intended for the manufacture of tyres, in other words, capable of replacing, in its reinforcing functions of the conventional particulate filler grades for tires, this filler usually differs, as is well known, the presence of hydroxyl groups (-OH) on its surface.

The physical state in which the reinforcing inorganic filler, it doesn't matter whether it's a powder, microbeads, granules, balls or any other appropriate densified form. Of course, under the reinforcing inorganic filler is understood to mean mixtures of different reinforcing inorganic fillers, in particular, a mixture of highly dispersed silica and/or alumina fillers, which are described below.

As reinforcing inorganic fillers are suitable, in particular mineral fillers of siliceous type, in particular silica (SiO2), or aluminous type, in particular alumina (Al2O3). Used silica may be any reinforcing silica known to the expert, in particular any precipitated or pyrogenic silica, and whose surface on the BAT, and specific surface CTAB below 450 m2/g, preferably ranging from 30 to 400 m2/G. as highly dispersed precipitated silicas (referred to as "HDS") include, for example, the silicas Ultrasil 7000 and Ultrasil 7005 from Degussa, the silicas Zeosil 1165MP, 1135MP and 1115MP from the company Rhodia, the silica Hi-Sil EZ150G from PPG, the silicas Zeopol 8715, 8745 and 8755 from Huber, silicas with high specific surface area as described in the application WO 03/16837.

Applied inorganic increased�schy filler in particular if it is silica, preferably has a specific surface according to BET of from more than 45 to less than 400 m2/g, more preferably from more than 60 to less than 300 m2/g.

Preferably, the total proportion of reinforcing filler (carbon black and/or inorganic reinforcing filler such as silica) is from more than 20 to 200 phr, more preferably from more than 30 to 150 phr, and the optimal value, as is known, depends on the particular intended application: for example, the expected gain level Bicycle tires is, of course, below the level required to the bus, capable of continuously roll at high speed, for example, the tire of the motorcycle, bus tourist vehicle or a goods vehicle, heavy goods transport.

According to one preferred embodiment of the invention, the reinforcing filler is used, containing from more than 30 to less than 150 phr, more preferably from more than 50 to less than 120 phr of inorganic filler, particularly silica, and possibly carbon black; the carbon black, when used, is preferably used in an amount of less than 20 phr, more preferably less than 10 phr (for example, from more than 0.1 to less than 10 phr).

To bind the reinforcing inorganic filler to the diene elastomer, use�I, as you know, the binder agent (or agent combinations), at least bifunctional, designed to provide sufficient traction, chemical and/or physical nature, between the inorganic filler (surface of its particles) and the diene elastomer, in particular bifunctional organosilanes or polyorganosiloxanes.

In particular, apply polysulfone silanes, called "symmetrical" or "asymmetrical" depending on their specific structure, which is described, for example, in applications WO 03/002648 (or US 2005/016651) and WO 03/002649 (or US 2005/016650).

Suitable, in particular, but not including the following definition is restrictive, polysulfone silanes, called "symmetric", corresponding to the following General formula (I):

(I) Z-A-Sx-A-Z

in which:

- x means an integer from 2 to 8 (preferably from 2 to 5);

A divalent hydrocarbon radical (preferably1-C18alkylene group or C6-C12Allenova group, in particular, alkylene1-C10more specifically - C1-C4in particular propylene);

- Z meets one of the following formulas

in which:

- the radicals R1substituted or unsubstituted, identical or different from each other, mean C1-C18alkyl, C5 -C18cycloalkyl or C6-C18aryl group (preferably1-C6alkyl, pirazinokarbazolovogo cyclohexyl or phenyl group, in particular, With1-C4alkyl group, more particularly methyl and/or ethyl),

- the radicals R2substituted or unsubstituted, identical or different from each other, mean C1-C18alkoxylic one or5-C18cycloalkenyl group (preferably a group selected from alkoxyl1-C8and cycloalkenyl5-C8even more preferably a group selected from alkoxyl1-C4, more particularly methoxyl and ethoxyl).

In the case of a mixture polysulfonic of alkoxysilanes corresponding to the formula (I) described above, in particular the usual mixtures available commercially, the mean value of x is a fractional number, preferably ranging between more than 2 to less than 5, more preferably close to 4. But the invention may also with advantage be used, for example, with desulfuromonas the alkoxysilanes (x=2).

As examples polysulfonic silanes can be called, in particular, the polysulphides (in particular disulphides, trisulfide or tetrasulfide) bis-(alkoxy(C1-C4)-alkyl(C1-C4)silyl-alkyl(C1-C4)), as for example the polysulphides of bis(3-triethoxysilylpropyl�La) or bis(3-triethoxysilylpropyl). Of these compounds are used, in particular, bis(3-triethoxysilylpropyl) tetrasulphide, abbreviated TESPT, of formula [(C2H5O)3Si(CH2)3S2]2or bis-(triethoxylylpropyl) disulphide, abbreviated TESPD, of formula [(C2H5O)3Si(CH2)3S]2. Let us mention also as preferred examples of the polysulphides (in particular disulphides, trisulfide or tetrasulfide) bis-(monoalkyl(C1-C4-dialkyl(C1-C4)silylpropyl), more particularly bis - monomethoxypolyethylene tetrasulfide what is described in the patent application WO 02/083782 (or US 2004/132880).

As a binding agent, which is not polysulfonyl the alkoxysilane, call, in particular, bifunctional POS (polyorganosiloxanes) or polysulfides of hidroxizina (R2=OH in formula I, described above) as described in patent applications WO 02/30939 (or US 6774255) and WO 02/31041 (or US 2004/051210), or silanes or POS containing azodicarbonamide functional groups as described, for example, in patent applications WO 2006/125532, WO 2006/125533, WO 2006/125534.

In the rubber compositions according to the invention the content of the binding agent preferably ranges from more than 4 to less than 12 phr, more preferably from more than 4 to less than 8 phr.

The specialist will understand that, as filler equivalent to n�organic reinforcing filler, described in this paragraph could be used a reinforcing filler of another nature, in particular organic, if only this reinforcing filler is covered with an inorganic layer such as silica, or will contain on its surface a functional centers, in particular, hydroxyl, requiring the use of a binding agent to establish a connection between the filler and the elastomer.

II.3 - Phenolic resin

The composition according to the invention contains a phenolic resin.

Suitable, in particular, phenols (the name of a homologous series of hydroxyl derivatives, aromatic hydrocarbons and equivalent compounds; this definition covers, in particular, monophenol, for example, actually phenol, or hydroxybenzene, bisphenola, polyphenols (polyhydroxyethyl), substituted phenols, the alkyl phenols or kalcifer, for example, bisphenol, diphenylolpropane, diphenylmethan, Naftali, cresol, tert-butylphenol, Octylphenol, Nonylphenol, Xylenol, resorcinol or similar products).

Preferably phenolic resin, called "Novolac", and also called phenolaldehyde precondensation. These Novolac resins (also referred to as two-stage resins curing) are thermoplastic and require the use of a curing agent for crosslinking; he� have sufficient plasticity in order to facilitate the processing of rubber compositions. After crosslinking curing agent they become "thermosetting" resins. Novolac resins have already been described in rubber compositions, in particular intended for tires or rolling surfaces of tires for many different applications, such as adhesion or reinforcement; we refer, for example, the documents US-A-3842111, US-A-3873489, US-A-3978103, US-A-3997581.

According to one preferred embodiment of the invention, the amount of phenolic resin is preferably from more than 1 to less than 20 phr; below the specified minimum desired technical effect is insufficient, whereas above the indicated maximum, there is a risk that the resin becomes too hard, and too much hysteresis will deteriorate. Because of all this, more preferably selects the number from more than 2 to less than 15 phr.

II.4 - Polyallelic

With the above-described resin blend curing agent, able to sew or to be cured of it. According to the invention, the hardener is polialden. Cross-linking of the resin is called during the vulcanization of the rubber matrix by the formation of covalent bonds between the resin and the aldehyde groups of the hardener. Aldehyde group polialden compounds react with the carbon atoms in ortho - and para-positions of the phenolic nuclei, forming the resulting three-dimensional grid usilivaya� resin, which contributes to the elastomeric composition is more rigid. The absence of the methylene donor type HMT or H3M leads to the fact that there are no formaldehyde emissions during vulcanization of the rubber composition.

The composition according to the invention includes polyallelic containing at least two aldehyde groups.

In particular, polyallelic is a dialdehyde, for example, propertylegal, potentialized, glutaraldehyde, hexane-1,6-dial, glyoxal, 1,2-phthaldialdehyde, terephthalaldehyde, 3,6-dimethoxy-2,7-naphthalenecarboximides, 1,4-naphthalenecarboximides, 1,9-intracervically, 2,7-naphthalenecarboximides, or dialdehyde, for example, 1,1,5-intentionally, 1,4,7-naphthalenetracarboxylic, 1,7,9-intracisternally, or polyallelic, for example, polyacrolein.

According to one preferred embodiment of the invention, polyallelic is a 2-hydroxybenzene-1,3,5-tricarballylic.

According to one preferred embodiment of the invention, the amount of the hardener is preferably from more than 1 to less than 20 phr, more preferably from more than 1 to less than 15 phr; below the specified minimum desired technical effect is insufficient, whereas above the indicated maximum, there is a risk of deterioration of the milling�timemost songs in their raw state or during vulcanization.

II.5 - Various additives

The present invention is a rubber composition for surfaces of the rolling elements also include all or part of the usual additives traditionally used in elastomer compositions intended for receiving the rolling contact surfaces, such as, for example, pigments, protective agents, such as waxes-antiozonant, chemical antiozonants, antioxidants, other plasticizing agents other than those above, substances that increase fatigue strength, reinforcing resins, a crosslinking system based either on sulfur or sulfur donors and/or peroxides and/or bismaleimides, vulcanization accelerators, vulcanization activators.

These compositions may also contain, in addition to binding agents, activators binding agents covering the inorganic fillers or more generally, auxiliary agents for processing capable, as is known, due to improved filler dispersion in the rubber matrix and by reducing the viscosity of the compositions to improve their ability to process in the raw state, such agents are, for example, hydrolyzed silanes, such as alkylalkoxysilane, polyols, polyethers, primary, secondary or tertiary amines, hydroxylated or hydrolyzed polyorganosiloxanes.

II.6 - Preparation of rubber compositions

The invention composition used for the rolling contact surfaces, can be produced in suitable mixers, using two successive stages, a well-known specialist: the first stage of thermomechanical working or kneading (referred to as "non-productive" phase) at high temperature to a maximum temperature comprised between 110°C to 190°C, preferably from 130°C to less than 180°C, followed by a second phase of mechanical work (the stage called "productive") to achieve a lower temperature, typically below 110°C, for example, component from over 40°C to less than 100°C, stage of development, during which introduce cross-linking system.

A method of producing such composition contains, for example, the following steps:

- to enter in the diene elastomer during the first phase (called unproductive), the reinforcing filler, stirring it all thermomechanically (for example, one or more times until a maximum temperature comprised between 110°C to 190°C;

- cooling system to a temperature below 100°C;

- enter then, in the second phase (called productive), a crosslinking system;

- stir everything until a maximum temperature below 110°C.

Phenolic resin and polyallelic you can enter either the non-productive stage, either for p�oductive stage. Preferably, the phenolic resin is introduced for non-productive stage, and polyallelic on a productive phase.

As an example, non-productive stage is performed in a single thermomechanical step during which in a suitable mixer, such as a normal internal mixer, first introduced all the main components required (diene elastomer, reinforcing filler, a phenolic resin, polyallelic), and then, secondarily, for example, after two minutes of mixing, the other additives injected, the possible agents of the coating of the filler or additional processing AIDS, with the exception of the crosslinking system. The total duration of mixing on this non-productive phase is preferably from more than 1 to less than 15 min.

After cooling, the thus obtained mixture in an external mixer such as a roll mixer, supported at a low temperature (e.g., between 40°C and 100°C), then enter the crosslinking system. All this is then mixed (productive phase) for several minutes, for example, from more than 2 to less than 15 min.

Actually the crosslinking system is preferably based on sulfur and a primary vulcanization accelerator, in particular an accelerator sulfenamides type. To this vulcanization system are added, introducing the first non-productive stage and/or at Ho�e productive stage various subsidiary known accelerators or vulcanization activators, such as zinc oxide, stearic acid, guanidine derivatives (in particular diphenylguanidine), etc. sulfur content is preferably from 0.5 to 3.0 phr, the share of the main accelerator is preferably from more than 0.5 to less than 5.0 phr.

As an accelerator (main or auxiliary) can be used any compound capable of acting as accelerator of the vulcanization of diene elastomers in the presence of sulphur, in particular accelerators thiazoline type and their derivatives, accelerators type of Turnov, dithiocarbamates of zinc. More preferably, these accelerators selected from the group consisting of a disulfide 2-mercaptobenzothiazole (abbreviated MBTS), N-cyclohexyl-2-benzothiazolesulfenamide (abbreviated as CBS), N,N-DICYCLOHEXYL-2-benzothiazolesulfenamide (abbreviated DCBS), N-tert-butyl-2-benzothiazolesulfenamide (abbreviated TBBS), N-tert-butyl-2-benzothiazolesulfenamide (abbreviated TBSI), dibenzyldithiocarbamate zinc (abbreviated ZBEC) and mixtures of these compounds. Preferably used main accelerator sulfenamides type.

The thus obtained final composition may then be rolled, for example, in the form of sheet, plate, in particular for characterization in the laboratory, or to ekstrudirovaniya, for example, to obtain rubber profile used for the manufacture of W�NY.

The invention relates to the tires and the intermediates described above for tires, rubber products in their raw state (i.e. before curing) and in the crosslinked state (i.e. after crosslinking or vulcanization).

II.7 - a Tire according to the invention

The rubber composition according to the invention can be used in different parts of the tire, in particular, in the crown, in the area of the flange and in the area of the lateral surface.

According to one preferred embodiment of the invention described above, the rubber composition can be used in the tire as a rigid elastomeric layer in at least one part of the tire.

Under elastomeric "layer" refers to any three-dimensional element from the rubber composition (or "elastomer" - these two terms are treated as synonyms) of any shape and any thickness, in particular, sheet, strip or other element of any cross section, e.g. rectangular or triangular.

First, the elastomeric layer can be used as a layer in the crown of the tire, between, on the one hand, the surface of the rolling element, i.e. the part that will be in contact with the road during rolling, and, on the other hand, the reinforcing belt of the said crown. The thickness of the elastomeric layer preferably lies in the range of from 0.5 to 10 mm, in particular in the range from 1 to 5 mm.

According to another preferred� embodiment of the invention, the rubber composition according to the invention can be used for the formation of the elastomeric layer located in the area of the bead of the tire, the radius between the layer of the carcass, the bead to the point of tilting of the layer frame.

Another preferred embodiment of the invention may be the use of the composition according to the invention for the formation of the elastomeric layer, located in the zone of the sidewall.

III - Examples of carrying out the invention

III.1 - Preparation of compositions

Conduct the following tests in the following way: in an internal mixer (final degree of filling: approximately 70% by volume), the initial temperature capacity equal to about 60°C, successively administered diene elastomer, reinforcing filler and a phenolic resin, and various other ingredients, except the vulcanization system. Then produce thermomechanical working (non-productive phase) in one stage, which lasts in total about 3-4 min, until the maximum temperature of the "fall" of 180°C.

Thus obtained mixture is extracted, cooled, and then into the mixer (finisher-homogenizer) at 30°C is injected sulfur, accelerator, sulfenamide type and polyallelic and stir it all (productive phase) for a suitable time (e.g., from more than 5 to less than 12 min.)

Then get�record thus composition is rolled into the form of plates (thickness of 2 to 3 mm) or thin sheets of rubber to measure their physical or mechanical properties, or is extruded in the form of a profile.

III.2 - Test rubber compositions

This experience illustrates the rubber composition used in the lower zones of the tire, which do not lead to the formation of formaldehyde during vulcanization and which have a stiffness at low strain, the equivalent stiffness of conventional compositions comprising a phenolic resin and HMT as a methylene donor, and also have improved fatigue strength as compared with the conventional arrangement.

For this purpose the above method were prepared with two rubber compositions, one according to the invention (identified below C. 2) and the other not according to the invention (the control composition C. 1 below) (see table 1).

The control composition C. 1 is common for the specialist composition used to obtain mixtures of the lower zones tire tourist transport; it is based on natural rubber.

A composition according to the invention C. 2 contains 2-hydroxybenzene-1,3,5-tricarballylic instead HMT contained in the composition C. 1, and has the same number of aldehyde groups, which is entered by the hardener HMT composition C. 1.

The composition (in phr, i.e., weight parts per hundred parts of rubber) and their mechanical properties are summarized in the attached tables 1 and 2.

Note first that the composition C. 2 according to the invention has a rigidity of bobbin and hi� (MA10), almost equivalent at low strain stiffness of the control composition and also the equivalent elongation at break (AR).

However, it is established that the fatigue strength of the composition C. 2 according to the invention is much improved in comparison with the control composition C. 1, which is equivalent to improve the life of the tire containing such a composition.

In conclusion, the results of this experience show that the use of 2-hydroxybenzene-1,3,5-tricarballylic instead of HMT in the rubber compositions according to the invention allows to obtain a rubber composition, the characteristics of the rigidity of which at low strain identical to those produced for traditional control compositions, but with a significant improvement in fatigue strength compared to the same compositions without the formation of formaldehyde during the cross-linking composition.

Table 1
ComponentC. 1C. 2
NR(1)100100
Carbon black (2)7575
Phenol-formaldehyde resin (3)4 4
ZnO4(4)88
Stearic acid (5)0,650,65
6PPD (6)1,41,4
HMT (7)1,6-
Polyallelic (8)-4,1
CPT (9)0,30,3
Insoluble sulfur 20N (10)6,56,5
TBBS (11)0,670,67
(1) Natural rubber;
(2) Carbon black N326 (designation according to ASTM D-1765);
(3) phenol-formaldehyde Novolac resin ("Peracit 4536K" from Perstorp);
(4) zinc Oxide (industrial grade - the company Umicore);
(5) stearin ("Pristerene 4931" from the company Uniqema);
(6) N-1,3-dimethylbutyl-N-phenylpropanolamine (Santoflex 6-PPD from the company Flexsys);
(7) Hexamethylenetetramine (from Degussa);
(8) 2-hydroxybenzene-1,3,5-tricarballylic (from the company Maybridge),
(9) Cyclohexylthio�phthalimide (PVI);
(10) Insoluble sulfur 80%;
(11) N-tert-butyl-2-benzothiazolesulfenamide (from the company Flexsys).

Table 2
Composition No.C. 1C. 2
MA102724,5
AR224221
Durability (fatigue)100123

1. Rubber composition for tires or semi-finished products for tyres, based on at least:
- one diene elastomer,
- one reinforcing filler,
- one crosslinking system,
- one phenolic resin,
- one polyallelic in which the proportion of phenolic resin is between 2 and 15 phr and share polyallelic is between 1 and 20 phr.

2. The rubber composition according to claim 1 in which the elastomer is selected from the group consisting of natural rubber, synthetic polyisoprenes, polybutadienes, copolymers of butadiene, copolymers of isoprene and mixtures of these elastomers.

3. The rubber composition according to claim 1, in which polyallelic contains at least 2 aldehyde groups.

4. KAU�okowa composition according to claim 1, in which the proportion of polyallelic is between 1 and 15 phr.

5. The rubber composition according to claim 1, in which polyallelic is 2-hydroxybenzene-1,3,5-tricarballylic.

6. The rubber composition according to claim 1, in which the reinforcing filler includes carbon black and/or silica.

7. The tire containing the rubber composition according to any one of claims.1-6.

8. The finished rubber product containing rubber composition according to any one of claims.1-6.

9. Prefabricated rubber product containing rubber composition according to any one of claims.1-6.

10. A method of producing a rubber composition according to any one of claims.1-6, characterized in that it comprises the following steps:
- enter in a diene elastomer during a first stage called non-productive, reinforcing filler, a phenolic resin and polyallelic, stirring it all thermomechanically until a maximum temperature between 110°C and 190°C;
- cooling the combined mixture to a temperature below 100°C;
- subsequent input at the second stage, called productive stitching system;
- mixing obtained to a maximum temperature below 110°C.

11. A method of producing a rubber composition according to any one of claims.1-6, characterized in that it comprises the following steps:
- enter in a diene elastomer during a first stage called non-productive, reinforcing filler, RA�masiva all this thermomechanically until a maximum temperature, located between 110°C and 190°C;
- cooling the combined mixture to a temperature below 100°C;
- subsequent input at the second stage, called productive, crosslinking systems, phenolic resin and polyallelic;
- mixing obtained to a maximum temperature below 110°C.

12. A method of producing a rubber composition according to any one of claims.1-6, characterized in that it comprises the following steps:
- enter in a diene elastomer during a first stage called non-productive, reinforcing filler and a phenolic resin, stirring it all thermomechanically until a maximum temperature between 110°C and 190°C;
- cooling the combined mixture to a temperature below 100°C;
- subsequent input at the second stage, called productive stitching system and polyallelic;
- mixing obtained to a maximum temperature below 110°C.



 

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