Thermoplastic elastomer composition with moderate degree of vulcanization

FIELD: polymer materials.

SUBSTANCE: thermoplastic elastomer composition contains dynamically vulcanized mixture of partially vulcanized halogenated isobutylene elastomer, polyamide, and conventionally utilized additives, wherein stretching elasticity modulus at 100% elongation for elastomer distributed in polyamide is less than 0.60 MPa and wherein halogenated elastomer is, in particular, brominated or chlorinated one. Preparation of thermoplastic elastomer composition involves dynamic vulcanization of halogenated isobutylene elastomer, polyamide, and conventionally utilized additives at temperature lower than 185°C.

EFFECT: improved durability and flexibility of composition.

11 cl, 2 tbl, 2 ex

 

The technical field

The present invention provides an improved thermoplastic elastomer composition having excellent durability and flexibility. In particular, the present invention relates to a thermoplastic elastomer composition, which comprises halogenated isobutilene elastomer, distributed in the polyamide matrix having a limited modulus of tensile elasticity of the elastomer after vulcanization, which provides excellent durability at low temperatures.

The level of technology

In EP722850B1 described low permeability thermoplastic elastomer composition which is excellent as a barrier layer for gas in the pneumatic tire. This thermoplastic composition comprises a low permeability thermoplastic matrix, such as polyamides or a mixture of polyamides, which are distributed low permeability rubber, such as the commercially available brominated copolymer of isobutene with p-methylstyrene (or BIMS). Later in the two patent applications EP 857761A1 and EP 969039A1, it was determined the ratio of the viscosity of thermoplastic matrix and dispersion of rubber as a function of the ratio of the volume fractions and independently determined that it must be close to unity in order to achieve the phase continuity in thermoplastic and the fine rubber, respectively. In EP 969039A1 was established importance for e is their thermoplastic elastomers smaller dispersion of rubber to give acceptable durability, especially when they are used as inner lining in the pneumatic tire. Also, according ERA, desired degree of vulcanization BIMS from 50 to 95%.

The essence of the invention

The essence of the present invention is to provide a thermoplastic elastomer composition having excellent durability and flexibility.

In accordance with the present invention proposed a thermoplastic elastomer composition comprising a dynamically vulcanized blend of (A) partially vulcanized halogenated isobutilene elastomer and (b) a polyamide in which the modulus of tensile elasticity at 100%elongation of the elastomer, distributed in the polyamide has a value of less than 0.60 MPa.

Description of the invention

In this description and the following claims the singular also refer to the plural object references unless the context clearly indicates otherwise.

According to the present invention improve the durability of the low permeability thermoplastic elastomers at low temperatures is achieved by adjusting the modulus of tensile elasticity at 100%elongation dispersed elastomer after vulcanization. Thus, the present invention relates to dynamically vulcanised elastomeric particles distributed in the floor of the amide matrix of thermoplastic elastomeric film, having excellent durability at low temperatures. More specifically the present invention relates to partially vulcanized thermoplastic elastomer composition for thermoplastic elastomeric film with a modulus of tensile elasticity at 100%elongation distributed elastomer after curing, suitable for use as a barrier that prevents the penetration of air, such as a layer for preventing the penetration of air into the pneumatic tire. The modulus of tensile elasticity of dispersed elastomer at 100%elongation is less than 0,60 MPa, preferably of 0.59 MPa or less, preferably of 0.58 MPa or less, of 0.57 MPa or less, preferably of 0.56 MPa or less.

The modulus of tensile elasticity at 100%elongation determined by measuring the modulation of force by AFM in accordance with the test method described in "Maria D. Ellul et al. ACS Rubber 2001, Cleveland (i.e. reference 1), and then calculating the modulus of elasticity at 100%elongation. Ellul and others Express the modulation strength in millivolts, and then must be calculated modulus of tensile elasticity at 100%elongation.

The modulation strength is used in conjunction with AFM mode "obstuctive". First Carteret topology of the sample, using mode "obstuctive". When modulation forces the tip of the cantilever about the will escaut set of 50 nm from the surface, certain obstukivanii. Then, the cantilever oscillates in the mode indentation at the resonant frequency of the bimorph ˜10 kHz. When scanning at a constant amplitude drive for implemented using bimorph piezoelectric modulation power set at 500 mV and measure the RMS amplitude response of the cantilever. Carried out using a bimorph piezoelectric modulation strength is modulated displacement relative to the holder tip. However, if you do not know the input amplitude at the tip (known only to the amplitude modulation for the bimorph), to calculate the mechanical module of the sample from the amplitude response is impossible. Instead, for comparison, the hardness of the rubber in different samples measure the relative difference in RMS amplitude response between the rubber and the nylon in the specified pattern.

Determination of modulus of tensile elasticity of the amplitude of the AFM modulation strength is as follows. Although the following example is for nylon and BIMS, the person skilled in the art will understand that this procedure can be used with other thermoplastics and elastomers. Preparing a single mixture of nylon and BIMS (commercially available brominated copolymer of isobutylene and para-methylstyrene) with a fully vulcanized BIMS (by saturating the vulcanizing agent and a great time of vulcanization) with the same mixture of NYLO the a and BIMS, but without vulcanizing agents (vulcanization = 0%). Exploring these two mixtures using AFM mode modulation strength, establish a correlation between the degree of vulcanization and the amplitude of the AFM modulation strength (in mV) on the assumption of a linear correlation. Since the moduli of elasticity tensile BIMS as a function of the state of vulcanization are known, the amplitude modulation of the force can therefore be recalculated on the modulus of elasticity at 100%elongation BIMS-rubber. In the examples of periodic and non-periodic modules of elasticity in tension were averaged to obtain a final modulus of tensile elasticity at 100%elongation.

The ability to stretch and tensile test described here is based on JIS K6251 "test Method for tensile strength of vulcanized rubber".

Thermoplastic elastomer composition is a mixture of halogenated isobutilene elastomer and polyamide, which is subjected to dynamic vulcanization, where the polyamide is present in an amount of 5 to 75 mass parts, more preferably from 10 to 75 mass parts, and the elastomer is present in an amount of from 95 to 25 mass parts, more preferably from 90 to 25 mass parts.

The term "dynamic vulcanization" is used here to refer to the process of vulcanization, in which the structural polymer resin and capable of vulcanization of the elastomer vulcanized under conditions of high shear. The result is capable of vulcanization of the elastomer at the same time stitched and distributed in the form of fine particles "microgel" inside the matrix structural polymer resin.

Dynamic vulcanization is effected by mixing the components at a temperature equal to or higher than the temperature of vulcanization of the elastomer, equipment such as rolls, Banbury mixers®, continuous mixers, agitators or mixing extruders type, such as twin-screw extruders. The unique feature of dynamically cured compositions is that, notwithstanding the fact that the elastomeric component may be fully cured, the compositions can be processed and reprocessed by conventional methods of processing of rubber, such as extrusion, injection molding, extrusion, etc. Cropping or allowances can be collected and recycled again.

In a preferred embodiment, halogenated isobutilene elastomeric component includes a copolymer of isobutylene and para-alkylthiol, such as described in European patent application 0344021, where the elastomer is a brominated copolymers of isobutylene and para-methylstyrene containing from 5 to 12 wt.% para-methylstyrene, from 0.3 to 1.8 mol.% the brominated para-methylstyrene, and having visco is th Mooney (1+4) from 30 to 65 at 125° C, measured according to ASTM D 1646-99. The copolymers preferably have an essentially uniform distribution of the composition. Preferred alkyl groups for pair-alkylthiophenes component include alkyl groups containing from 1 to 5 carbon atoms, primary halogenated, secondary halogenated having from 1 to 5 carbon atoms, and mixtures thereof. The preferred copolymer contains isobutylene and para-methylsterol.

Suitable halogenated isobutilene elastomeric components include copolymers (such as brominated copolymers of isobutylene and para-methylstyrene) with srednekamennogo molecular weight Mn of at least about 25,000, preferably at least 50,000, preferably at least approximately 75,000, preferably at least about 100,000, preferably at least approximately 150,000. The copolymers may also be relevant srednevekovoi molecular weight (Mw) to srednekamennogo molecular weight (Mn), i.e., Mw/Mn, less than about 6, preferably less than about 4, more preferably less than about 2.5, most preferably less than approximately a 2.0. In another embodiment, suitable halogenated isobutilene elastomeric components include copolymers (such as brominated copolymers of isobutylene with para-methylstyrene)having a viscosity on the moon is (1+4) at 125° C (measured according to ASTM D 1646-99) 25 or more, preferably 30 or more, more preferably 40 or more.

Preferred brominated copolymers of isobutylene and para-methylstyrene include copolymers containing from 5 to 12 wt.% para-methylstyrene, from 0.3 to 1.8 mol.% the brominated para-methylstyrene and having a Mooney viscosity (1+4) from 30 to 65 at 125°C (measured according to ASTM D 1646-99).

Halogenated isobutilene elastomer component (A) according to the present invention can be obtained from isobutylene and from about 0.5 to 25 wt.%, preferably from about 2 to 20 wt.% (from the total number of comonomers) n-alkylthiol, preferably p-methylstyrene, followed by halogenoalkanes. Halogen (such as Br and/or Cl, preferably Br) is preferably less than about 10 wt.%, more preferably from about 0.1 to about 7 wt.% from the total amount of copolymer.

The copolymerization can be carried out in a known manner as described, for example, in European patent application EP-34402/A, published on November 29, 1989, and halogenoalkane can be carried out in a known manner, as described, for example, in U.S. patent No. 4548995.

Halogenated isobutilene elastomer preferably has srednekamennogo molecular massfor less than the least about 25,000, more preferably at least about 100,000, and srednevekovoi molecular weightto srednekamennogo molecular massiepreferably less than about 10, more preferably less than about 8.

Polyamides suitable for use in the present invention are thermoplastic polyamides (nylonase)containing crystalline or resinous, high molecular weight solid polymers including copolymers and ternary copolymers having recurring amide units within the polymer chain. The polyamides can be obtained by polymerization of one or more Epsilon-lactams, such as caprolactam, pyrrolidone, laurinlactam and aminoundecanoic lactam, or amino acid, or by condensation of dibasic acids and diamines. Suitable nylony as fibre-forming species, and is suitable for casting. Examples of such polyamides are polycaprolactam (nylon 6), polyarylate (nylon 12), polyhexamethylenediamine (nylon 6,6), polyhexamethylenediamine (nylon 6,9), polyhexamethyleneguanidine (nylon 6,10), polyhexamethylenediamine (nylon 6 IP), and the condensation product of 11-aminoundecanoic acid (nylon 11). Can also be used nylon 6 (N6), nylon 11 (N11), nylon 12 (N12), sprinklers shall dimensional nylon 6/66 (N6/66), nylon 6,10 (N610), nylon 4,6, nylon MXD6, nylon 6,9, and nylon 6,12 (N612). Can also apply their copolymers and their mixtures. Additional examples of satisfactory polyamides (especially having a softening point below 275° (C) described in Kirk-Othmer in Encyclopedia of Chemical Technology, v. 10, page 919, and Encyclopedia of Polymer Science and Technology, Vol.10, pages 392-414. In the practice of the present invention can be used commercially available thermoplastic polyamides, preferably linear crystalline polyamides with a softening point or melting point 160-230°C.

In addition, the present invention relates to a method for producing a thermoplastic elastomer composition that includes dynamic vulcanization halogenated isobutilene elastomer, polyamide and traditionally used additives at a temperature of less than 185°C.

Besides the already mentioned main components of the elastomeric composition according to the present invention may contain a vulcanization agent or crosslinking, the accelerator of vulcanization or crosslinking, various types of oils, a stabilizer, a reinforcing filler, plasticizer, softening agent, or other various additives usually incorporated into the main rubber. Compounds are mixed and vulcanized conventional methods, to obtain a composition, which can then be used for vulcanization or crosslinking. Quantity is of such additives added may be the same as a number, usually dobavlialsea still, unless it is contrary to the aim of the present invention.

Hereinafter the present invention will be illustrated, but in no way limited by the following examples.

Procedure Tapping Phase and AFM modulated power were as follows. All samples were analyzed no later than 8 hours after freezing, to avoid relaxation of the samples. After freezing, the samples were cooled to -150°and cut with a diamond knife in a freezing microtome Reichert. Then they were kept in a desiccator in a stream of dry nitrogen gas to warm to room temperature without condensation. Finally subjected to freezing, the samples were mounted in a miniature steel holders for AFM analysis. AFM measurements were carried out in air by scanning probe microscope NanoScope Dimension 3000 (Digital instruments)using a rectangular silicon cantilever. Ratio operating point maintained at a level equal to or less than 0.5, whereas the contact operating point was chosen in the usual manner to provide a repulsive contacts with a positive phase shift. The cantilever operating at its resonant frequency or a little smaller.

For components used in the examples used the following commercially available products:

1. Component of the polymer resin

Niall is n: nylon 11 (BESN, ATOFINA) and nylon 6/66 (V, UBE) at a mass ratio of approximately three to two.

2. The elastomeric component

BIMS: commercially available brominated copolymer of isobutylene and para-methylstyrene, sold under the trademark EXXPRO 89-4 company ExxonMobil Chemical Company, with a Mooney viscosity of about 45 containing approximately 5 wt.% para-methylstyrene and about 0.75 mol.% bromine ZnO: zinc oxide, vulcanizing substance St-acid: stearic acid, curing substance ZnSt: zinc stearate, vulcanizing agent.

3. Supplements

The plasticizer is N-butylbenzenesulfonamide Antioxidant Irganox 1098, Tinuvin 622LD and Cul.

Examples 1-2 and comparative example 1

Three films produced by extrusion blow, with the same composition shown in table 1 were mixed in a twin-screw extruder at a temperature of mixture 230°C. Then extrusion blow received three films having the same composition as that shown in table 1, at the temperature of extrusion 250°for examples 1, 2 and comparative example 1, using the same blow molding die plate. The tires of examples 1 and 2 were produced at 180°C. the Tire of comparative example 1 was produced at 185°C. the Degree of vulcanization Ehkrga 89-4 thermoplastic elastomeric films are shown in table 2. The film was subjected to production test tires in Canada during the winter season, when temperatures may ACTIGALL -20° C and below.

Table 1

The composition of the cast film
MaterialRPG (parts per 100 parts of BIMS)
BIMS100
ZnO0,15
St-acid0,6
ZnSt0,3
Nylon68
The plasticizer21
Antioxidant0,5

The state of vulcanization was measured using AFM mode modulation strength. For examples was measured by the amplitude of the modulation strength (FMA). In example 1, the FMA was equal to the 5.25 nm in example 2 FMA equal 5,23 nm in comparative example 1, the FMA was $ 6.1 nm. This method was described in the above reference 1.

Table 2
Example 1Comparative example 1Example 2
The modulus of tensile elasticity at 100%elongation [MPa]DurabilityThe modulus of tensile elasticity at 100%elongation [MPa]]DurabilityThe modulus of tensile elasticity at 100%UDL is in [MPa]] Durability
Temperature vulcanization180°185°180°
Periodic0,56OK0,587NG0,529OK
Nonperiodic0,514OK0,611NG0,541OK
Average0,5370,6020,535
NG: there was cracking.

According to the test method references 1 degree of vulcanization of the elastomer, distributed in thermoplastic elastomer composition was proportional to the oscillation amplitude of the cantilever in AFM measurements in the modulation mode power. This means that the higher the modulus of tensile elasticity at 100%elongation of the elastomer gives greater the amplitude of the cantilever oscillation.

The effect of inventions

Examples 1 and 2 and comparative example 1 were tested in the same environment testing (i.e. in Canada). As shown in table 2, if the modulus of tensile elasticity at 100%elongation of less than 0,60 MPa, tire cracking does not occur. The investigator is about, the present invention demonstrates that by reducing the modulus of tensile elasticity at 100%elongation to a value of less than 0.60 MPa can be obtained desirable characteristics and can be improved durability of the tire in thermoplastic elastomer film obtained by extrusion-blow process, to improve the durability at low temperatures.

All described here documents introduced by reference, including all documents by priority and/or test methods. As is evident from the preceding General description and specific embodiments, although there have been illustrated and described variants of the invention may be made by different modifications not departing from the essence and scope of the invention. Accordingly, it is understood that the invention is not restricted by them.

1. Thermoplastic elastomer (TPE) composition comprising a dynamically vulcanized blend of partially vulcanized halogenated isobutilene elastomer, polyamide and traditionally used additives, in which the modulus of tensile elasticity at 100% elongation for distributed in the polyamide elastomer is less than 0.60 MPa, and where the halogenated elastomer is a commercially available brominated or chlorinated elastomer.

2. TPE composition according to claim 1, characterized in that the elastomer contains bromine the integration of a copolymer of isobutylene and parallelsthe.

3. TPE composition according to claim 1 or 2, characterized in that the elastomer contains a copolymer of partially vulcanized, brominated isobutylene and parameterstyle.

4. TPE composition according to claim 1 or 2, characterized in that the polyamide contains one or more polymers of nylon 6, nylon 6,6, nylon 11, nylon 6,9, nylon 12, nylon 6,10, nylon 6,12, nylon 4,6, nylon MXD6, nylon 6/66.

5. TPE composition according to claim 1 or 2, characterized in that the polyamide has a softening point of from 160 to 230°C.

6. TPE composition according to claim 1 or 2, characterized in that the polyamide is present in the TPE compositions an amount of 5 to 75 parts by weight, and the elastomer is present in an amount of from 95 to 25 parts by weight of

7. TPE composition according to claim 1 or 2, characterized in that the elastomer has srednekamennogo molecular weight equal to at least 50000.

8. TPE composition according to claim 1 or 2, characterized in that the elastomer has Mw/Mnless than 6.

9. TPE composition according to claim 1 or 2, characterized in that the elastomer has a Mooney viscosity (1+4) at 125°C (measured according to ASTM D 1646-99) 25 or more.

10. TPE composition according to claim 1 or 2, characterized in that the elastomer is a brominated copolymers of isobutylene and parameterstyle containing from 5 to 12 wt.% parameterstyle, from 0.3 to 1.8 mol.% the brominated parameterstyle, and the Mooney viscosity (1+4) is from 30 to 65 at 125°With (and who intend ASTM D 1646-99).

11. A method of obtaining a thermoplastic elastomer (TPE) composition according to any one of claims 1 to 10, with a dynamic vulcanization halogenated isobutilene elastomer, polyamide and traditionally used additives at a temperature of less than 185°and the modulus of tensile elasticity at 100% elongation for distributed in the polyamide partially cured halogenated elastomer is less than 0.60 MPa.



 

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FIELD: polymer mixtures and rubber industry.

SUBSTANCE: low-permeable elastomer composition useful in manufacturing pneumatic diaphragm such as inside shell of tire comprises elastomer, filler, stratified clay, polybutene softener having molecular mass 400 to 10000, and curing agent. Elastomer can be random copolymer including unit derived from C4-C7-isomonoolefin and can be selected from halogenated isobutylene/p-methylstyrene copolymer, star-shaped butyl rubber, halogenated butyl rubber, and their combinations. Composition as a whole forms nanocomposite. Prior to be mixed with copolymer, clay may optionally be subjected to additional stratification treatment.

EFFECT: improved pneumatic diaphragm properties of composition and improved processability thereof.

13 cl, 19 tbl, 44 ex

FIELD: rubber industry; automotive industry; production of the sealing layer at manufacture of the tubeless tires and the pneumatic constructions.

SUBSTANCE: the invention is pertaining to rubber industry and the automotive industry and is dealt with production of the sealing layer at manufacture of the tubeless tires and the pneumatic constructions. The rubber mixture contains the isoprene rubber, the filled chlorbutyl rubber produced by interaction at comixing of the butyl rubber and the hlorinated hydrocarbon of the common formulaСnН(2n+2)С1х, where n = 10-30, х = 7-24, at the temperature of 80-150°С at the presence of the colloid silicon dioxide introduced into the mixture in the process of their comixing, brimstone, the sulfonamide accelerant, the stearic acid, zinc oxide, the high-pressure polyethylene, the engineering carbon, the alkylphenolamide resin. The technical result of the invention consists in the increased protection of the rubber mixture from the possible premature vulcanization in the processes of its preparation and reprocessing.

EFFECT: the invention ensures the increased protection of the rubber mixture from the possible premature vulcanization in the processes of its preparation and reprocessing.

2 tbl, 1 ex

FIELD: polymer materials.

SUBSTANCE: invention relates to elevated-viscosity thermoplastic halogenated elastomer compositions and to a process for preparing the same. Composition according to invention contains thermoplastic polymer, at least one isoolefin copolymer comprising unit derived from halomethylstyrene, and at least one hindered amine or phosphine compound having the respective structure R1R2 R3N or R1R2R3P wherein R1 is H or C-1-C6-alkyl, R2 is C1-C30-alkyl and R3 is C4-C30-alkyl and further wherein R3 represents alkyl higher than R-1. A process for preparing elevated-viscosity thermoplastic composition consists in mixing thermoplastic polymer, at least one isoolefin copolymer comprising unit derived from halomethylstyrene, and at least one hindered amine or phosphine compound to obtain thermoplastic elastomer compositions, including dynamically cured ones, containing more finely dispersed elastomer.

EFFECT: improved mechanical properties.

4 cl, 10 tbl

Rubber composition // 2254348

FIELD: rubber industry.

SUBSTANCE: invention concerns a method for grafting polymers based on conjugated diene monomers to brominated butyl rubbers and using thus obtained grafted copolymers in rubber compositions, which, after vulcanization, acquire improved physical characteristics. Grafting procedure comprises mixing solid brominated butyl rubber with solid polymers based on conjugated diene monomer including some quantity of bonds C-S-(S)n-C with n being an integer equal from 1 to 7. Mixing is conducted at temperature above 50 over a period of time long enough to complete the grafting. Rubber composition containing above grafted polymer optionally includes one or more curing agents. Cured rubber composition is intended for manufacturing tracks.

EFFECT: increased shock-absorbing capacity of products.

14 cl, 5 dwg, 5 tbl, 3 ex

FIELD: plastic, rubber, chemical, petrochemical, paint-vehicle, air and other industrials.

SUBSTANCE: halogenated or halosulfonated 4-methylpentene-1 (co)polymer is obtained in tetrachloroethane or chlorobenzene solution and contains chemically coupled chlorine and/or bromine, or chlorine and sulfur, or bromine and sulfur, or simultaneously chlorine, bromine and sulfur in form of groups -SO2Cl and -SO2Br, wherein content of chlorine and/or bromine and sulfur is 1-73 mass % and 0,2-4,0 mass %, respectively. Also disclosed are polymer, elastomer composition, binding agent and articles based on halogenated and halosulfonated 4-methylpentene-1 (co)polymer.

EFFECT: butene-1 (co)polymer, article and composition therefrom with increased controlling strength, elasticity, fire-retarding, as well as controlling flow point, percent elongation, etc.

FIELD: plastic, rubber, chemical, petrochemical, paint-vehicle, air and other industrials.

SUBSTANCE: halogenated or halosulfonated butene-1 (co)polymer is obtained in tetrachloroethane or chlorobenzene solution and contains chemically coupled chlorine and/or bromine, or chlorine and sulfur, or bromine and sulfur, or simultaneously chlorine, bromine and sulfur in form of groups -SO2Cl and -SO2Br, wherein content of chlorine and/or bromine and sulfur is 1-73 mass % and 0,2-4,0 mass %, respectively. Also disclosed are polymer, elastomer composition, binding agent and articles based on halogenated and halosulfonated butene-1 (co)polymer.

EFFECT: butene-1 (co)polymer, article and composition therefrom with increased controlling strength, elasticity, fire-retarding, as well as controlling flow point, percent elongation, etc.

9 cl, 19 tbl, 6 dwg

FIELD: chemistry of polymers.

SUBSTANCE: invention relates to preparing shock-resistant antifreeze polypropylene compositions. The shock-resistant antifreeze composition comprises the following components, wt.-%: isotactic polypropylene, 77.0-85.7; elastomer, 14.0-18.0, wherein poly-1-octene with the intrinsic viscosity value in the range from 4.0 to 12.0 dl/g is used; thermostabilizing agent, 0.1-0.5, and special additives, the balance. Shock-resistant antifreeze polypropylene composition is characterized by improved melt fluidity indices that providing the improved processing capacity. Invention can be used in automobile manufacture, building and light industry for production of articles of technical designation exploited at reduced temperatures.

EFFECT: improved and valuable technical properties of composition.

2 tbl, 7 ex

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