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WO2017159286A1 - Charge minérale pour caoutchouc, composition de caoutchouc et pneu - Google Patents

Charge minérale pour caoutchouc, composition de caoutchouc et pneu Download PDF

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Publication number
WO2017159286A1
WO2017159286A1 PCT/JP2017/007021 JP2017007021W WO2017159286A1 WO 2017159286 A1 WO2017159286 A1 WO 2017159286A1 JP 2017007021 W JP2017007021 W JP 2017007021W WO 2017159286 A1 WO2017159286 A1 WO 2017159286A1
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WO
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Prior art keywords
titanium oxide
rubber
oxide particles
inorganic filler
rubber composition
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PCT/JP2017/007021
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English (en)
Japanese (ja)
Inventor
春奈 西本
Original Assignee
大塚化学株式会社
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Publication date
Application filed by 大塚化学株式会社 filed Critical 大塚化学株式会社
Priority to CN201780016855.5A priority Critical patent/CN108884277B/zh
Priority to JP2017531784A priority patent/JP6227849B1/ja
Publication of WO2017159286A1 publication Critical patent/WO2017159286A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B60—VEHICLES IN GENERAL
    • B60C—VEHICLE TYRES; TYRE INFLATION; TYRE CHANGING; CONNECTING VALVES TO INFLATABLE ELASTIC BODIES IN GENERAL; DEVICES OR ARRANGEMENTS RELATED TO TYRES
    • B60C1/00—Tyres characterised by the chemical composition or the physical arrangement or mixture of the composition
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L21/00—Compositions of unspecified rubbers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons

Definitions

  • the present invention relates to an inorganic filler for rubber capable of improving wet grip properties when used in a tire, a rubber composition containing the same, and a tire using the same.
  • Patent Document 1 it is known to use a rubber composition in which an inorganic filler is blended in a rubber component.
  • titanium-based materials are easy to handle, inexpensive, and highly environmentally safe, they are being studied for use in various applications. However, it is not known that sufficient wet grip properties can be obtained with a rubber composition containing a titanium-based material.
  • An object of the present invention is to provide an inorganic filler for rubber that exhibits excellent wet grip properties when used in a tire, a rubber composition containing the same, and a tire using the same.
  • the present inventor provides the following inorganic filler for rubber, rubber composition and tire.
  • Item 1 Consisting of titanium oxide particles having a heating weight loss rate of 0.4 to 10.0% by mass in a temperature range of 200 to 800 ° C. when heated from 40 ° C. to 1000 ° C. at a heating rate of 10 ° C./min. , Inorganic filler for rubber.
  • Item 2 The inorganic filler for rubber according to Item 1, wherein the titanium oxide particles have a specific surface area of 5 to 1000 m 2 / g.
  • Item 3 The inorganic filler for rubber according to Item 1 or 2, wherein the titanium oxide particles have an average particle size of 10.0 ⁇ m or less.
  • Item 5 The inorganic filler for rubber according to any one of Items 1 to 4, wherein the titanium oxide particles have an aqueous dispersion pH value of 2.0 to 11.0.
  • Item 6 The inorganic filler for rubber according to any one of Items 1 to 5, wherein a treatment layer made of a surface treatment agent is formed on the surface of the titanium oxide particles.
  • Item 7 A rubber composition comprising the rubber component and the inorganic filler for rubber according to any one of Items 1 to 6.
  • Item 8 The rubber composition according to Item 7, wherein the rubber component is a diene rubber.
  • Item 9 The rubber composition according to Item 7 or 8, wherein the compounding amount of the inorganic filler for rubber is 1 to 100 parts by mass with respect to 100 parts by mass of the rubber component.
  • Item 10 The rubber composition according to any one of Items 7 to 9, which is used for tire treads.
  • Item 11 A tire comprising the rubber composition according to any one of Items 7 to 10 in a tread portion.
  • the rubber composition containing the inorganic filler for rubber of the present invention can exhibit excellent wet grip properties when used in a tire.
  • the tire of the present invention is excellent in wet grip properties.
  • FIG. 1 is a view showing an X-ray diffraction chart of titanium oxide particles A obtained in Production Example 1 of the present invention.
  • FIG. 2 is a view showing an X-ray diffraction chart of titanium oxide particles B obtained in Production Example 2 of the present invention.
  • FIG. 3 is a view showing an X-ray diffraction chart of the titanium oxide particles C obtained in Production Example 3 of the present invention.
  • FIG. 4 is a view showing an X-ray diffraction chart of titanium oxide particles D obtained in Production Example 4 of the present invention.
  • FIG. 5 is a view showing an X-ray diffraction chart of the titanium oxide particles E obtained in Production Example 5 of the present invention.
  • FIG. 1 is a view showing an X-ray diffraction chart of titanium oxide particles A obtained in Production Example 1 of the present invention.
  • FIG. 2 is a view showing an X-ray diffraction chart of titanium oxide particles B obtained in Production Example 2 of the present invention.
  • FIG. 3 is a view
  • the inorganic filler for rubber of the present invention has a weight loss rate of 0.4 in a temperature range of 200 to 800 ° C. when heated from 40 ° C. to 1000 ° C. at a rate of temperature increase of 10 ° C./min in an inert gas stream. It consists of titanium oxide particles of ⁇ 10.0 mass%. It is considered that the titanium oxide particles of the present invention contain chemically adsorbed water and hydroxyl groups, and the chemically adsorbed water evaporates and dehydrates the hydroxyl groups in the above temperature range, and finally becomes titanium oxide.
  • the reason for specifying the heating weight reduction rate is that by evaluating the heating weight reduction rate in the temperature range, the physically adsorbed water evaporates before reaching the temperature range, and the chemically adsorbed water and hydroxyl groups of the titanium oxide particles This is because the amount of titanium oxide particles that can be evaluated and can provide excellent wet grip properties can be specified.
  • the heating weight reduction rate in the temperature range of 200 to 800 ° C. of the titanium oxide particles of the present invention is 0.4 to 10.0% by mass, preferably 1.0 to 8.0% by mass. It is more preferably from 0.5 to 7.0% by mass, even more preferably from 2.0 to 6.5% by mass, and particularly preferably from 2.3 to 6.0% by mass.
  • the shape of the titanium oxide particles of the present invention is not particularly limited, but is preferably a non-fibrous particle such as a plate shape, a spherical shape, and an indefinite shape from the viewpoint of influence on the environment.
  • the specific surface area (BET method) of the titanium oxide particles of the present invention is usually 5 to 1000 m 2 / g, preferably 10 to 500 m 2 / g, more preferably 30 to 200 m 2 / g, More preferably, it is 50 to 150 m 2 / g.
  • the average particle size of the titanium oxide particles of the present invention is usually 10.0 ⁇ m or less, preferably 0.01 to 10.0 ⁇ m, more preferably 0.1 to 10.0 ⁇ m, still more preferably.
  • the thickness is 0.1 to 5.0 ⁇ m, particularly preferably 0.5 to 2.0 ⁇ m. If the average particle size exceeds 10.0 ⁇ m, it is not preferable from the viewpoint of the fracture resistance characteristics of the rubber, and if the average particle size is too small, it is not preferable from the viewpoint of the toxicity of the fine particles.
  • the average particle size means a particle size having an integrated value of 50% in the particle size distribution determined by the laser diffraction / scattering method.
  • the titanium oxide particles of the present invention are compounds known as hydrolysates of water-soluble titanium compounds such as titanium sulfate and titanium chloride, such as “titanium oxide hydrate”, “hydrous titanium oxide”, “metatitanic acid”. And the like.
  • titanium oxide hydrate a compound having a peak pattern similar to that of anatase type titanium oxide, but unlike titanium oxide, it is a low crystalline compound.
  • “low crystallinity” is different from an amorphous compound having no specific peak in X-ray diffraction, and is different from a crystalline compound having a sharp peak, and shows an intermediate peak.
  • the full width at half maximum of the maximum peak is 0.10 ° or more.
  • the full width at half maximum is preferably 0.10 ° to 2.00 °, more preferably 0.45 ° to 1.80 °.
  • the titanium oxide particles of the present invention can be obtained, for example, by hydrolysis of a titanium sulfate solution, and titanium oxide particles obtained in the production process of “sulfuric acid method titanium oxide” can also be used.
  • “Sulfuric acid method titanium oxide” is a method of obtaining titanium oxide by dissolving raw ore of titanium oxide in sulfuric acid and purifying it, and firing the purified product. Usually, titanium ore, ilmenite ore, natural Rutile or the like can be dissolved by heating in concentrated sulfuric acid to obtain a titanium sulfate solution.
  • Titanium oxide particles obtained by hydrolysis of titanium sulfate may contain a large amount of sulfuric acid in the production process as impurities, which may cause deterioration of rubber components and equipment used. Therefore, it is preferable to disperse the titanium oxide particles in water, wash the sulfuric acid content by adding alkali, filter the solid content, dry, and pass through to obtain the titanium oxide particles of the present invention. .
  • the concentration of the dispersion and the amount of alkali added in the washing are not particularly limited as long as the dispersion of the titanium oxide particles is stable, and can be appropriately selected from a wide range.
  • the alkali include sodium hydroxide, potassium hydroxide, and ammonia. Two or more alkalis may be used in combination as required.
  • titanium ions are said to be complex compounds bonded to water molecules and form chain or network bonds as hydrolysis proceeds. This compound grows until it becomes colloidal, and finally precipitates to obtain titanium oxide particles. For this reason, titanium oxide particles obtained by hydrolysis of titanium sulfate have a large specific surface area, have many hydroxyl groups and chemically adsorbed water, and are considered to provide excellent wet grip properties. Further, since the titanium oxide particles have more hydroxyl groups than titanium oxide, it is considered that the titanium oxide particles become a low crystalline compound unlike titanium oxide.
  • the titanium oxide particles of the present invention may be used after being fired for the purpose of evaporating excess chemically adsorbed water or the like so as not to change the structure due to heat in the production and processing of the rubber composition. .
  • the calcination temperature is preferably 800 ° C. or less, and more preferably 500 ° C. or less. Since the intended firing effect may not be obtained when the firing temperature is low, the firing temperature is preferably 200 ° C. or higher.
  • the calcination time is 2 to 8 hours because crystallization may progress and transfer to titanium oxide may occur if the calcination time is long, and the intended calcination effect may not be obtained if the calcination time is short. It is preferable.
  • the aqueous dispersion pH value of the titanium oxide particles of the present invention is preferably 2.0 to 11.0, more preferably 4.0 to 8.0. If the water dispersion pH value is less than 2.0, a large amount of sulfuric acid is contained, which may cause deterioration of rubber components and equipment used. On the other hand, if the water dispersion pH value is larger than 11.0, the alkali content increases, and there is a risk of deterioration of the rubber component or equipment used.
  • a treatment layer made of a surface treatment agent is formed on the surface of the titanium oxide particles for the purpose of improving dispersibility and improving adhesion with a rubber component.
  • the surface treatment agent include coupling agents such as a titanium coupling agent and a silane coupling agent.
  • a silane coupling agent is preferable.
  • silane coupling agents include sulfide, polysulfide, thioester, thiol, olefin, epoxy, amino, and alkyl silane coupling agents, which may be used alone. Alternatively, two or more kinds may be mixed and used.
  • sulfide-based silane coupling agents include bis (3-triethoxysilylpropyl) tetrasulfide, bis (3-trimethoxysilylpropyl) tetrasulfide, bis (3-methyldimethoxysilylpropyl) tetrasulfide, and bis ( 2-triethoxysilylethyl) tetrasulfide, bis (3-triethoxysilylpropyl) disulfide, bis (3-trimethoxysilylpropyl) disulfide, bis (3-methyldimethoxysilylpropyl) disulfide, bis (2-triethoxysilyl) Ethyl) disulfide, bis (3-triethoxysilylpropyl) trisulfide, bis (3-trimethoxysilylpropyl) trisulfide, bis (3-methyldimethoxysilylpropyl) trisulfide, bis (2- Triethoxy
  • thioester-based silane coupling agents include 3-hexanoylthiopropyltriethoxysilane, 3-octanoylthiopropyltriethoxysilane, 3-decanoylthiopropyltriethoxysilane, and 3-lauroylthiopropyltriethoxysilane.
  • thiol-based silane coupling agent examples include 3-mercaptopropyltrimethoxysilane, 3-mercaptopropyltriethoxysilane, 3-mercaptopropylmethyldimethoxysilane, and the like.
  • olefin-based silane coupling agents include dimethoxymethylvinylsilane, vinyltrimethoxysilane, dimethylethoxyvinylsilane, diethoxymethylvinylsilane, triethoxyvinylsilane, vinyltris (2-methoxyethoxy) silane, allyltrimethoxysilane, allyltri Ethoxysilane, p-styryltrimethoxysilane, 3- (methoxydimethoxydimethylsilyl) propyl acrylate, 3- (trimethoxysilyl) propyl acrylate, 3- [dimethoxy (methyl) silyl] propyl methacrylate, 3- (trimethoxysilyl) Propyl methacrylate, 3- [dimethoxy (methyl) silyl] propyl methacrylate, 3- (triethoxysilyl) propyl methacrylate, 3- [tris (to Methylsiloxy) silane
  • epoxy-based silane coupling agents include 3-glycidyloxypropyl (dimethoxy) methylsilane, 3-glycidyloxypropyltrimethoxysilane, diethoxy (3-glycidyloxypropyl) methylsilane, and triethoxy (3-glycidyloxypropyl) silane. 2- (3,4-epoxycyclohexyl) ethyltrimethoxysilane and the like.
  • amino silane coupling agents examples include N-2- (aminoethyl) -3-aminopropylmethyldimethoxysilane, N-2- (aminoethyl) -3-aminopropyltrimethoxysilane, and 3-aminopropyl. Trimethoxysilane, 3-aminopropyltriethoxysilane, 3-ethoxysilyl-N- (1,3-dimethylbutylidene) propylamine, N-phenyl-3-aminopropyltrimethoxysilane, N- (vinylbenzyl)- Examples include 2-aminoethyl-3-aminopropyltrimethoxysilane. Of these, 3-aminopropyltriethoxysilane is preferred.
  • alkyl-based silane coupling agents include methyltrimethoxysilane, dimethyldimethoxysilane, trimethylmethoxysilane, methyltriethoxysilane, ethyltrimethoxysilane, n-propyltrimethoxysilane, isobutyltrimethoxysilane, and isobutyltriethoxy.
  • Examples include silane, n-hexyltrimethoxysilane, n-hexyltriethoxysilane, cyclohexylmethyldimethoxysilane, n-octyltriethoxysilane, and n-decyltrimethoxysilane.
  • bis (3-triethoxysilylpropyl) tetrasulfide can be particularly preferably used.
  • a known surface treatment method can be used as a method for forming a treatment layer comprising a surface treatment agent on the surface of the titanium oxide particles.
  • a solvent that promotes hydrolysis for example, water, alcohol, or these
  • the surface treatment agent is dissolved in a mixed solvent) as a solution, and the solution is sprayed onto the titanate compound particles, or the integral blend method in which the titanate compound particles and the surface treatment agent are blended with the rubber component.
  • the amount of the surface treatment agent when the surface treatment agent is treated on the surface of the titanate compound particles of the present invention is not particularly limited, but in the case of a wet method, the surface treatment agent is 0 with respect to 100 parts by mass of the titanate compound particles.
  • the solution of the surface treatment agent may be sprayed so as to be 1 to 20% by mass.
  • the surface treatment agent is added to the rubber component so that the surface treatment agent is 1 to 50 parts by mass, preferably 10 to 40 parts by mass with respect to 100 parts by mass of the titanate compound particles. That's fine.
  • the rubber composition of the present invention is a rubber composition obtained by blending the above-mentioned inorganic filler for rubber with a rubber component.
  • the rubber component used in the rubber composition of the present invention is not particularly limited, but a diene rubber is preferably used from the viewpoint of excellent strength.
  • the diene rubber include natural rubber (NR), isoprene rubber (IR), styrene butadiene rubber (SBR), butadiene rubber (BR), butyl rubber (IIR), ethylene propylene diene rubber (EPDM), acrylonitrile butadiene rubber ( NBR), rubbers such as styrene isoprene butadiene rubber (SIBR), chloroprene rubber (CR), and modified rubbers of these, and rubber components containing one or more of these are preferred. From the viewpoint of a balance between low rolling resistance and high wet grip properties, it is particularly preferable to use styrene butadiene rubber (SBR, which may be modified).
  • SBR styrene butadiene rubber
  • the blending amount of the inorganic filler in the rubber composition of the present invention is preferably 1 to 100 parts by weight, more preferably 5 to 70 parts by weight, with respect to 100 parts by weight of the rubber component. More preferably, it is 40 mass parts. By setting it within this range, it is possible to obtain even better wet grip properties.
  • carbon black silica (white carbon), calcium carbonate (CaCO 3 ), alumina (Al 2 O 3 ), alumina hydrate (Al 2 O 3 .H) are used as reinforcing fillers.
  • reinforcing fillers can be used alone or in combination of two or more, and among these, carbon black and silica can be suitably used.
  • the total amount of the reinforcing filler is preferably 5 to 200 parts by mass, and more preferably 30 to 100 parts by mass with respect to 100 parts by mass of the rubber component.
  • the surface of the reinforcing filler may be organically treated in order to improve the affinity with the rubber component.
  • rubber chemicals usually used in the rubber industry can be appropriately blended.
  • softeners such as process oil
  • vulcanizing agents such as sulfur, vulcanization accelerators, vulcanization acceleration aids, anti-aging agents, stearic acid, zinc white (zinc oxide), scorch inhibitors, ozone inhibitors, processing Auxiliaries, waxes, resins, foaming agents, stearic acid, vulcanization retarders, and the like can be blended within the range of blending amounts that are usually used, if necessary.
  • the rubber composition of the present invention is obtained by kneading using an open kneader such as a roll or a kneading machine such as a closed kneader such as a Banbury mixer, and is vulcanized after molding to It can be applied to rubber products.
  • the rubber composition of the present invention can be used for tire treads, under treads, carcass, sidewalls, bead parts, etc., particularly for tire applications, and among these, excellent wet grip properties can be exhibited. It is preferably used as a tire tread rubber.
  • the tire of the present invention is characterized in that the rubber composition of the present invention is used in the tread portion, and thereby has excellent wet grip properties.
  • the tire of the present invention there is no particular limitation on the points other than using the rubber composition of the present invention in the tread portion, and the tire composition can be appropriately configured according to a conventional method.
  • Titanium oxide particles A 100 g of titanium oxide particles 1 (water content 50%, average particle size 2.5 ⁇ m) obtained in the production process of sulfuric acid method titanium oxide was dispersed in 10 L of deionized water to obtain a dispersion. A 48 mass% potassium hydroxide aqueous solution was added to the obtained dispersion so that the pH of the dispersion was 7, and the mixture was stirred. After stirring, the solid was collected by filtration, dried and sieved to obtain titanium oxide particles A.
  • the average particle diameter of the obtained titanium oxide particles A was measured with a laser diffraction particle size distribution analyzer (SALD-2100, manufactured by Shimadzu Corporation), and the specific surface area was measured according to JIS Z8830. It was shown in 1.
  • the heating weight reduction rate of the obtained titanium oxide particles A in the temperature range of 200 to 800 ° C. was 10 ° C./min under a nitrogen stream of 200 ml / min using 10 mg of sample TG-DTA manufactured by Seiko Instruments Inc.
  • the weight loss rate in the temperature range of 200 to 800 ° C. was calculated from the results, and the results are shown in Table 1.
  • FIGS. 1-10. The measurement was performed using an X-ray diffraction measurement apparatus (Rigaku Corporation, Ultimate IV), and the half width of the peak corresponding to the crystal plane (101) of titanium oxide in the range of 2 ⁇ 20 ° to 30 ° is shown in Table 1. It was.
  • the aqueous dispersion pH value of the obtained titanium oxide particles A was determined by immersing a pH meter (manufactured by HORIBA, Castany Lab pH meter F-21) in the dispersion after stirring for 10 minutes at a 1% by mass slurry concentration of the titanium oxide particles A.
  • the stable pH value after stirring for 3 minutes is shown in Table 1.
  • Table 1 shows the average particle diameter, specific surface area, heating weight loss rate in the temperature range of 200 to 800 ° C., and water dispersion pH value of the obtained titanium oxide particles B.
  • X-ray diffraction charts of the titanium oxide particles B are shown in FIG. 2 and FIG.
  • Table 1 shows the average particle diameter, specific surface area, heating weight loss rate in the temperature range of 200 to 800 ° C., and water dispersion pH value of the obtained titanium oxide particles C.
  • X-ray diffraction charts of the titanium oxide particles C are shown in FIG. 3 and FIG.
  • Table 1 shows the average particle diameter, specific surface area, heating weight reduction rate in the temperature range of 200 to 800 ° C., and water dispersion pH value of the obtained titanium oxide particles D.
  • X-ray diffraction charts of the titanium oxide particles D are shown in FIG. 4 and FIG.
  • Titanium oxide particles E Titanium oxide particles A obtained in Production Example 1 were baked at 800 ° C. for 6 hours to obtain titanium oxide particles E.
  • Table 1 shows the average particle diameter, specific surface area, rate of weight loss by heating in the temperature range of 200 to 800 ° C., and water dispersion pH value of the obtained titanium oxide particles E.
  • X-ray diffraction charts of the titanium oxide particles E are shown in FIG. 5 and FIG.
  • Titanium oxide particles F 100 g of titanium oxide particles 2 (water content 50%, average particle size 1.1 ⁇ m) obtained in the production process of sulfuric acid method titanium oxide was dispersed in 10 L of deionized water to obtain a dispersion. A 48 mass% potassium hydroxide aqueous solution was added to the obtained dispersion so that the pH of the dispersion was 7, and the mixture was stirred. After stirring, the solid was collected by filtration, dried and sieved to obtain titanium oxide particles F.
  • Table 1 shows the average particle diameter, specific surface area, heating weight loss rate in the temperature range of 200 to 800 ° C., and water dispersion pH value of the obtained titanium oxide particles F.
  • Table 1 shows the full width at half maximum of the titanium oxide particles F.
  • Table 1 shows the average particle diameter, specific surface area, heating weight loss rate in the temperature range of 200 to 800 ° C., and water dispersion pH value of the obtained titanium oxide particles G.
  • the full width at half maximum of the titanium oxide particles G is shown in Table 1.
  • Titanium oxide particles H 100 g of titanium oxide particles 2 (water content 50%, average particle size 1.1 ⁇ m) obtained in the production process of sulfuric acid method titanium oxide was dispersed in 10 L of deionized water to obtain a dispersion. A 48 mass% potassium hydroxide aqueous solution was added to the obtained dispersion so that the pH of the dispersion was 4, and the mixture was stirred. After stirring, the solid was collected by filtration, dried, sieved, and calcined at 500 ° C. for 6 hours to obtain titanium oxide particles H.
  • Table 1 shows the average particle diameter, specific surface area, rate of weight loss by heating in the temperature range of 200 to 800 ° C., and water dispersion pH value of the obtained titanium oxide particles H.
  • the full width at half maximum of the titanium oxide particles H is shown in Table 1.
  • Table 1 also shows the specific surface area, average particle diameter, half-value width, and heating weight loss rate in the temperature range of 200 to 800 ° C. of titanium oxide (anatase) particles used in Comparative Example 1 described below.
  • Examples 1 to 13 and Comparative Examples 1 and 2 The ingredients listed in Table 2, excluding the vulcanization accelerator and sulfur, were kneaded for 3 to 5 minutes in a 1.5 L closed mixer, and the master batch released when the temperature reached 140 to 170 ° C was listed in Table 2.
  • a vulcanization accelerator and sulfur were added at a ratio and kneaded with a 10-inch open roll to obtain a composition.
  • This composition was press vulcanized in a mold at 150 ° C. for 40 minutes to prepare a test sample of the desired rubber composition.
  • Examples 1 to 13 using the titanium oxide particles A to H in the present invention showed excellent wet grip properties as compared with Comparative Examples 1 and 2.
  • Examples 1 to 3 and 11 to 13 using titanium oxide particles A to C and F to H have better wet grip properties than Examples 4 and 5 using titanium oxide particles D and E. Show.
  • Examples 11 to 13 using the titanium oxide particles F to H having a small average particle diameter are the same as those in Example 1 using the titanium oxide particles A having a large average particle diameter and aluminum hydroxide. Compared with the comparative example 2 used, the outstanding abrasion resistance was shown. Moreover, it turns out from the comparison with Example 11 and Example 12 and 13 that the abrasion resistance which was further excellent is shown by using a titanium oxide particle with a small specific surface area.

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Abstract

La présente invention vise à fournir une charge minérale pour caoutchouc, qui présente d'excellentes performances d'adhérence à l'état humide lorsqu'elle est utilisée dans un pneu, une composition de caoutchouc qui contient la charge minérale, et un pneu qui utilise la composition de caoutchouc. L'invention concerne une charge minérale pour caoutchouc, la charge comprenant des particules d'oxyde de titane qui ont un rapport de perte de poids de 0,4 à 10,0 % en masse à l'intérieur de la plage de température de 200 à 800 °C lorsqu'elle est chauffée de 40 °C à 1 000 °C à une vitesse d'élévation de température de 10 °C/min. De préférence, la surface spécifique des particules d'oxyde de titane est de 5 à 1 000 m2/g, le diamètre moyen de particule des particules d'oxyde de titane est de 10,0 µm ou moins, la valeur de demi-largeur d'un pic dans la plage 2θ = 20 à 30° est de 0,10° ou plus dans une analyse de diffraction des rayons X des particules d'oxyde de titane, la valeur de pH sous forme dispersée dans l'eau des particules d'oxyde de titane est de 2,0 à 11,0, et une couche de traitement comprenant un agent de traitement de surface est formée sur la surface des particules d'oxyde de titane.
PCT/JP2017/007021 2016-03-15 2017-02-24 Charge minérale pour caoutchouc, composition de caoutchouc et pneu WO2017159286A1 (fr)

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CN201780016855.5A CN108884277B (zh) 2016-03-15 2017-02-24 橡胶用无机填充材料、橡胶组合物和轮胎
JP2017531784A JP6227849B1 (ja) 2016-03-15 2017-02-24 ゴム用無機充填材、ゴム組成物及びタイヤ

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JPS63307119A (ja) * 1987-05-30 1988-12-14 チオクサイド　グループ　ピーエルシー 粒子状物質
JPH06279618A (ja) * 1993-03-25 1994-10-04 Ishihara Sangyo Kaisha Ltd 棒状微粒子導電性酸化チタンおよびその製造方法
JPH10139434A (ja) * 1996-11-13 1998-05-26 Teika Corp 紡錘状二酸化チタンの製造方法
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