WO2016174863A1 - Composition de caoutchouc et procédé de production associé - Google Patents

Composition de caoutchouc et procédé de production associé Download PDF

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Publication number
WO2016174863A1
WO2016174863A1 PCT/JP2016/002179 JP2016002179W WO2016174863A1 WO 2016174863 A1 WO2016174863 A1 WO 2016174863A1 JP 2016002179 W JP2016002179 W JP 2016002179W WO 2016174863 A1 WO2016174863 A1 WO 2016174863A1
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WIPO (PCT)
Prior art keywords
rubber composition
cellulose
oil
mass
rubber
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Application number
PCT/JP2016/002179
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English (en)
Japanese (ja)
Inventor
鉄平 中山
奥野　茂樹
博之 橘
正吾 小林
大樹 土屋
Original Assignee
バンドー化学株式会社
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Application filed by バンドー化学株式会社 filed Critical バンドー化学株式会社
Priority to JP2016570905A priority Critical patent/JP6123037B2/ja
Publication of WO2016174863A1 publication Critical patent/WO2016174863A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/20—Compounding polymers with additives, e.g. colouring
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
    • C08L1/02—Cellulose; Modified cellulose
    • 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

Definitions

  • the present disclosure relates to a rubber composition and a manufacturing method thereof.
  • cellulose fine fibers are blended in a rubber composition.
  • a rubber composition For example, in Patent Document 1, after mixing water or a polar solvent dispersion of fine unicellular cellulose fibers and rubber latex, at least a part of water or solvent is removed to obtain a finely modified cellulose fiber / rubber composite. Later, it is disclosed that this is mixed with rubber to produce a rubber composition.
  • an object of the technology of the present disclosure is to provide a method for producing a rubber composition that can reduce cost and environmental load.
  • a mechanical defibrating process is performed to defibrate the hydrophobized cellulose to produce an oil dispersion of cellulosic fine fibers.
  • the method for producing a rubber composition of the present embodiment includes a step of producing an oil dispersion of hydrophobic cellulose-based fine fibers and a step of kneading the dispersion into a rubber component.
  • the hydrophobic cellulose fiber is defibrated into fine fibers using mechanical defibrating means, and a gel-like oil dispersion in which the hydrophobic cellulose-based fine fibers are dispersed in the oil is obtained. obtain. Since the cellulose fiber hydrophobized is used, it can be dispersed well in the oil.
  • Cellulose fibers are fiber materials derived from cellulose fibers composed of plant cell wall skeletal components obtained from plant fibers.
  • Examples of the raw material plant for cellulose fiber include wood, bamboo, rice (rice straw), potato, sugar cane (bagasse), aquatic plants, seaweed and the like. Of these, wood is preferred.
  • hydrophobic cellulose fibers include, but are not limited to, cellulose fibers in which some or all of the hydroxyl groups of cellulose are substituted with hydrophobic groups, cellulose fibers that have been subjected to a hydrophobic surface treatment with a surface treatment agent, and the like. Can be mentioned.
  • Examples of the hydrophobization for obtaining cellulose fibers in which some or all of the hydroxyl groups of cellulose are substituted with hydrophobic groups include esterification (acylation) (alkyl esterification, complex esterification, ⁇ -ketoesterification, etc.) , Alkylation, tosylation, epoxidation, arylation and the like. Of these, esterification is preferred. Specifically, in the esterified hydrophobized cellulose fiber, part or all of the hydroxyl groups of cellulose are formed by carboxylic acid such as acetic acid, acetic anhydride, propionic acid, butyric acid, or a halide (particularly chloride) thereof. Acylated cellulose fiber.
  • Examples of the surface treatment agent for obtaining a cellulose fiber hydrophobized and surface-treated with a surface treatment agent include a silane coupling agent.
  • non-volatile process oil or plasticizer as the oil.
  • specific examples include paraffin oil, naphthenic oil, aroma oil, and ether / ester oil. Since volatile oil volatilizes due to temperature rise during processing, there are problems such as a change in the concentration of cellulose fibers in the oil and the need to recover and treat the volatilized oil. Therefore, it is preferable to use a non-volatile oil that does not cause such a problem.
  • the viscosity of the oil is preferably 25 cSt (centistokes) or more, more preferably 100 cSt or more, still more preferably 200 cSt or more, and particularly preferably 300 cSt or more, from the viewpoint of dispersibility of cellulose fibers, workability of dispersion preparation, and the like. Moreover, it is preferably 600 cSt or less, more preferably 550 cSt or less, still more preferably 500 cSt or less, and particularly preferably 450 cSt or less. In addition, the viscosity said here is the value measured according to JISK2283 at 40 degreeC.
  • the mechanical defibrating means used in the present embodiment is not particularly limited, and examples thereof include a jet mill, a two-roll mill, a mixer, a jet mixer, and a ball mill. Among these, it is preferable to use a jet mill.
  • the hydrophobic cellulose fiber is preferably contained in the oil dispersion in an amount of 10% by mass or more, more preferably 20% by mass or more, and preferably 50% by mass or less, more preferably 40% by mass or less. Yes.
  • the oil dispersion when preparing a rubber composition by kneading the oil dispersion with the rubber component, it becomes easy to set the blending amount of the oil and the cellulosic fine fibers within an appropriate range, and an oil dispersion that is easy to handle is obtained. be able to.
  • the hydrophobic cellulose-based fine fiber is preferably 0.5 parts by mass or more, more preferably 1 part by mass or more, further preferably 5 parts by mass or more, and preferably 40 parts by mass with respect to 100 parts by mass of the rubber component.
  • it is determined such that it is more preferably 30 parts by mass or less, and still more preferably 20 parts by mass or less.
  • the rubber component and the hydrophobized cellulose fine fiber are kneaded, and a compounding agent such as a reinforcing material, a processing aid, and a crosslinking agent is added and kneaded to obtain an uncrosslinked rubber composition part.
  • a compounding agent such as a reinforcing material, a processing aid, and a crosslinking agent is added and kneaded to obtain an uncrosslinked rubber composition part.
  • a general kneader such as a kneader or a Banbury mixer can be used.
  • Examples of rubber components include ethylene- ⁇ -olefin elastomers such as natural rubber (NR), ethylene / propylene copolymer (EPR), ethylene / propylene / diene terpolymer (EPDM), ethylene / octene copolymer, and ethylene / butene copolymer; Examples include chloroprene rubber (CR); chlorosulfonated polyethylene rubber (CSM); hydrogenated acrylonitrile rubber (H-NBR). The rubber component is preferably one or more of these blend rubbers.
  • NR natural rubber
  • EPR ethylene / propylene copolymer
  • EPDM ethylene / propylene / diene terpolymer
  • H-NBR hydrogenated acrylonitrile rubber
  • rubber compounding agents examples include reinforcing materials, oils, vulcanization acceleration aids, processing aids, crosslinking agents, and vulcanization accelerators.
  • carbon black for example, channel black; furnace black such as SAF, ISAF, N-339, HAF, N-351, MAF, FEF, SRF, GPF, ECF, N-234; FT, MT, etc. Thermal black; acetylene black and the like.
  • Silica is also mentioned as the reinforcing material. It is preferable that a reinforcing material is 1 type, or 2 or more types among these.
  • the content of the reinforcing material is preferably 5 parts by mass or more, more preferably 10 parts by mass or more, and preferably 50 parts by mass or less, more preferably 40 parts by mass with respect to 100 parts by mass of the rubber component of the rubber composition. It is below mass parts.
  • Oils include, for example, petroleum-based softeners, mineral oils such as paraffin wax, castor oil, cottonseed oil, linseed oil, rapeseed oil, soybean oil, palm oil, palm oil, fall raw oil, wax, rosin, pine And vegetable oils such as oil.
  • the oil is preferably one or more of these.
  • the oil content is, for example, 5 to 15 parts by mass with respect to 100 parts by mass of the rubber component of the rubber composition.
  • processing aids include stearic acid, polyethylene wax, and fatty acid metal salts.
  • the processing aid may be composed of a single species or a plurality of species.
  • the content of the processing aid is, for example, 0.1 to 3 parts by mass with respect to 100 parts by mass of the rubber component of the rubber composition.
  • the vulcanization acceleration aid examples include metal oxides such as zinc oxide (zinc white) and magnesium oxide, metal carbonates, fatty acids and derivatives thereof.
  • the vulcanization acceleration aid is preferably one or more.
  • the content of the vulcanization acceleration aid is, for example, 5 to 15 parts by mass with respect to 100 parts by mass of the rubber component of the rubber composition.
  • crosslinking agent examples include organic peroxides and sulfur.
  • an organic peroxide may be blended, sulfur may be blended, or both of them may be used in combination.
  • the amount of the crosslinking agent is, for example, 1 to 5 parts by mass with respect to 100 parts by mass of the rubber component of the rubber composition.
  • sulfur the compounding amount is 100 parts by mass of the rubber component of the rubber composition. For example, 1 to 5 parts by mass.
  • vulcanization accelerator examples include thiazole type (eg MBT, MBTS etc.), thiuram type (eg TT, TRA etc.), sulfenamide type (eg CZ etc.), dithiocarbamate type (eg BZ-P etc.) And the like. It is preferable that a vulcanization accelerator is 1 type, or 2 or more types among these. The content of the vulcanization accelerator is, for example, 2 to 5 parts by mass with respect to 100 parts by mass of the rubber component of the rubber composition.
  • the lower limit of the fiber diameter distribution is preferably 10 nm or more, and more preferably 20 nm or more, in order to ensure that the hydrophobic cellulose-based fine fiber exhibits its effect.
  • An upper limit becomes like this.
  • Preferably it is 1 micrometer or less, More preferably, it is 700 nm or less, More preferably, it is 500 nm or less.
  • the fiber diameter distribution range of the hydrophobized cellulose-based fine fibers is preferably 20 nm to 1 ⁇ m, more preferably 20 to 700 mm, and more preferably 20 to 500 nm. More preferably.
  • the fiber diameter distribution of the hydrophobized cellulose-based fine fibers is determined by freezing and pulverizing a sample of the rubber composition, then observing the cross section with a transmission electron microscope (TEM), and arbitrarily selecting 50 cellulose-based fine fibers. It is calculated
  • the average fiber diameter of the cellulosic fine fibers is obtained as the number average of the fiber diameters of 50 arbitrarily selected cellulosic fine fibers.
  • the uncrosslinked rubber composition obtained by the kneading process is molded and crosslinked by a normal molding and crosslinking process, whereby a crosslinked rubber composition is obtained.
  • the rubber composition can be produced with reduced cost and environmental load.
  • organic solvents when cellulose is defibrated in an organic solvent, most of the organic solvent is volatile, so there is a risk of ignition during kneading and the like, and a decrease in weight is also considered.
  • organic solvents since organic solvents generally have low viscosity, if the affinity with fibers is low, liquid leakage may occur from the gaps of the rotor during kneading, which may cause mechanical contamination and failure.
  • organic solvents since organic solvents generally have a lower molecular weight than oil, it is considered that bleeding from rubber is likely to occur.
  • a press for example, a press, a vulcanizer, a continuous vulcanizer, or the like may be used, or a special crosslinking group that is crosslinked by high-frequency crosslinking, radiation crosslinking, or electron beam crosslinking may be used.
  • the molding crosslinking conditions such as temperature, pressure, and time are appropriately set based on the composition of the filler-containing uncrosslinked rubber, the required quality of the rubber molded product, and the like.
  • the polymer molecules contained in the uncrosslinked rubber composition are crosslinked with a crosslinking agent to form a network structure. Thereby, a crosslinked rubber composition is obtained.
  • cellulose dispersions 1 to 8 were prepared.
  • the degree of dispersion varies, and there are liquid forms, but here all are referred to as dispersions.
  • the individual dispersions are also listed in Table 1.
  • the above-mentioned powdered cellulose was dispersed in paraffin oil (manufactured by Idemitsu Kosan Co., Ltd., trade name: Diana Fresia P22) to prepare a dispersion having a cellulose fiber concentration of 50% by mass. Using two rolls, powdered cellulose was fibrillated into cellulose fine fibers to obtain a gel-like oil dispersion in which hydrophobic cellulose fine fibers were dispersed in oil.
  • paraffin oil manufactured by Idemitsu Kosan Co., Ltd., trade name: Diana Fresia P22
  • Dispersion 2 was produced in the same manner as Dispersion 1, except that a mixer was used as a means for defibrating powdered cellulose.
  • Dispersion 3 was produced in the same manner as Dispersion 1, except that a jet mill was used as a means for defibrating powdered cellulose.
  • Dispersion 4 Dispersed in the same manner as Dispersion 1 except that a ball mill (pot mill rotating table: manufactured by Nippon Ceramic Science Co., Ltd., trade name BALL MILL ANZ-51S, zirconia balls: YTZ-5) was used as a means for defibrating powdered cellulose. Body 4 was produced.
  • a ball mill pot mill rotating table: manufactured by Nippon Ceramic Science Co., Ltd., trade name BALL MILL ANZ-51S, zirconia balls: YTZ-5
  • BALL MILL ANZ-51S zirconia balls
  • Dispersion 5 Powdered cellulose was dispersed in toluene to prepare a dispersion having a cellulose fiber concentration of 50% by mass. Using a high-pressure homogenizer, the dispersions were collided with each other to pulverize the powdered cellulose into cellulose fine fibers to obtain a dispersion in which the cellulose fine fibers were dispersed in toluene. The dispersion was designated as Dispersion 5.
  • Dispersion 6 A dispersion liquid (cellulose fine fiber concentration: 10% by mass) in which cellulose fiber (trade name: BiNFi-s cellulose Wma-10010), which has been defibrated, is dispersed in water is prepared, and dispersion 6 is prepared. It was.
  • Dispersion 7 similar to dispersion 6 was mixed with a solution in which styrene-butadiene (SBR) latex (manufactured by JSR, trade name: JSR 2108) was dissolved.
  • SBR styrene-butadiene
  • Dispersion 8 similar to dispersion 6 was mixed with a solution in which chlorosulfonated polyethylene (CSM) latex (trade name: Sepolex CSM, manufactured by Sumitomo Seika) was dissolved to obtain dispersion 8.
  • CSM chlorosulfonated polyethylene
  • Example 1 Natural rubber (manufactured by ALMA, natural rubber from Malaysia, trade name: SMR CV60) was masticated, and then dispersion 1 was added and kneaded. The amount of dispersion 1 introduced was such that the content of fine cellulose fibers was 10 parts by mass with respect to 100 parts by mass of natural rubber.
  • Example 2 An uncrosslinked rubber composition of Example 2 was produced in the same manner as Example 1 except that Dispersion 2 was used.
  • Example 3 An uncrosslinked rubber composition of Example 3 was produced in the same manner as Example 1 except that Dispersion 3 was used.
  • Example 4 An uncrosslinked rubber composition of Example 4 was produced in the same manner as Example 1 except that Dispersion 4 was used.
  • Example 5 An uncrosslinked rubber composition of Example 5 was produced in the same manner as in Example 1 except that EPDM (trade name: EP33, manufactured by JSR Corporation) was used as the rubber component.
  • EPDM trade name: EP33, manufactured by JSR Corporation
  • Example 6 An uncrosslinked rubber composition of Example 6 was prepared in the same manner as in Example 1 except that EPDM was used as the rubber component and Dispersion 2 was used.
  • Example 7 An uncrosslinked rubber composition of Example 7 was prepared in the same manner as in Example 1 except that EPDM was used as the rubber component and Dispersion 3 was used.
  • Example 8 An uncrosslinked rubber composition of Example 8 was prepared in the same manner as in Example 1 except that EPDM was used as the rubber component and Dispersion 4 was used.
  • Example 1 the same amount of the same compounding agent as in Example 1 (70 parts by mass of reinforcing material GPF carbon black, 3 parts by mass of zinc oxide as a vulcanization accelerator, 3 parts by mass of stearic acid as a processing aid, and crosslinking 4 parts by mass of sulfur as an agent and 2 parts by mass of a thiuram vulcanization accelerator were added and kneaded to prepare an uncrosslinked rubber composition of Comparative Example 1.
  • Comparative Example 2 Similarly to Comparative Example 1, after the dispersion 6 was put into natural rubber and kneaded, each compounding agent was added and further kneaded. Thereafter, drying under reduced pressure was performed to remove moisture derived from the dispersion 6, and an uncrosslinked rubber composition of Comparative Example 2 was produced.
  • Comparative Example 3 An uncrosslinked rubber composition of Comparative Example 3 was produced in the same manner as Comparative Example 1 except that Dispersion 7 was used.
  • Comparative Example 4 An uncrosslinked rubber composition of Comparative Example 4 was produced in the same manner as Comparative Example 1 except that Dispersion 8 was used.
  • Comparative Example 5 An uncrosslinked rubber composition of Comparative Example 5 was produced in the same manner as Comparative Example 1 except that EPDM was used as the rubber component.
  • Comparative Example 6 An uncrosslinked rubber composition of Comparative Example 6 was produced in the same manner as Comparative Example 1 except that EPDM was used as the rubber component and Dispersion 6 was used.
  • Comparative Example 7 An uncrosslinked rubber composition of Comparative Example 7 was produced in the same manner as Comparative Example 1 except that EPDM was used as the rubber component and Dispersion 7 was used.
  • Comparative Example 8 An uncrosslinked rubber composition of Comparative Example 8 was prepared in the same manner as Comparative Example 1 except that EPDM was used as the rubber component and Dispersion 8 was used.
  • a plasticizer may be used.
  • trade names DOA and DBP manufactured by Taoka Chemical Co., Ltd., trade names DOP manufactured by JNC Corporation, trade names DOS manufactured by Shin Nippon Rika Co., Ltd., and the like may be used.
  • the technique of the present disclosure is useful as a method for producing a rubber composition.

Abstract

Le procédé de production de composition de caoutchouc de la présente invention comprend une étape de production d'une dispersion huileuse de fibres fines de cellulose par mélange de fibres de cellulose rendues hydrophobes dans une huile et, après cela, par desserrage des fibres de cellulose rendues hydrophobes par mise en œuvre d'un traitement de desserrage mécanique. En outre, le procédé de production de la composition de caoutchouc comprend une étape de malaxage de la dispersion huileuse des fibres fines de cellulose avec un caoutchouc.
PCT/JP2016/002179 2015-04-28 2016-04-26 Composition de caoutchouc et procédé de production associé WO2016174863A1 (fr)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2017165956A (ja) * 2016-03-15 2017-09-21 株式会社服部商店 修飾セルロースナノファイバーの製造方法
JP2018119081A (ja) * 2017-01-26 2018-08-02 バンドー化学株式会社 ゴム組成物の製造方法及びそれを含む伝動ベルトの製造方法
JP2019178195A (ja) * 2018-03-30 2019-10-17 豊田合成株式会社 ゴム組成物の製造方法
JP2020012069A (ja) * 2018-07-19 2020-01-23 住友ゴム工業株式会社 分散体、製造方法、ゴム組成物及び空気入りタイヤ
CN111087707A (zh) * 2019-12-11 2020-05-01 太仓荣南密封件科技有限公司 一种琥珀酸酐改性ncc增强橡胶及其制备方法
JP2020196843A (ja) * 2019-06-05 2020-12-10 住友ゴム工業株式会社 ゴム組成物及び空気入りタイヤ
JP7007782B1 (ja) * 2021-04-28 2022-02-10 Ｃａｅｔｕｓ Ｔｅｃｈｎｏｌｏｇｙ株式会社 親水性多糖高分子を含有する粉末の水分散液の製造方法
JP7007781B1 (ja) * 2021-04-28 2022-02-10 Ｃａｅｔｕｓ Ｔｅｃｈｎｏｌｏｇｙ株式会社 水分散装置
WO2022230210A1 (fr) * 2021-04-28 2022-11-03 Ｃａｅｔｕｓ Ｔｅｃｈｎｏｌｏｇｙ株式会社 Dispositif de dispersion d'eau et dispersion aqueuse de polymère de polysaccharide hydrophile
WO2022230209A1 (fr) * 2021-04-28 2022-11-03 Ｃａｅｔｕｓ Ｔｅｃｈｎｏｌｏｇｙ株式会社 Procédé de fabrication d'une dispersion aqueuse de poudre contenant un polymère de polysaccharide hydrophile, et dispersion aqueuse de polymère de polysaccharide hydrophile

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JP2009084564A (ja) * 2007-09-10 2009-04-23 Sumitomo Rubber Ind Ltd 加硫ゴム組成物、空気入りタイヤおよびこれらの製造方法
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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2017165956A (ja) * 2016-03-15 2017-09-21 株式会社服部商店 修飾セルロースナノファイバーの製造方法
JP2018119081A (ja) * 2017-01-26 2018-08-02 バンドー化学株式会社 ゴム組成物の製造方法及びそれを含む伝動ベルトの製造方法
JP2019178195A (ja) * 2018-03-30 2019-10-17 豊田合成株式会社 ゴム組成物の製造方法
JP2020012069A (ja) * 2018-07-19 2020-01-23 住友ゴム工業株式会社 分散体、製造方法、ゴム組成物及び空気入りタイヤ
JP7243060B2 (ja) 2018-07-19 2023-03-22 住友ゴム工業株式会社 分散体、製造方法、ゴム組成物及び空気入りタイヤ
JP2020196843A (ja) * 2019-06-05 2020-12-10 住友ゴム工業株式会社 ゴム組成物及び空気入りタイヤ
JP7342431B2 (ja) 2019-06-05 2023-09-12 住友ゴム工業株式会社 ゴム組成物及び空気入りタイヤ
CN111087707A (zh) * 2019-12-11 2020-05-01 太仓荣南密封件科技有限公司 一种琥珀酸酐改性ncc增强橡胶及其制备方法
JP7007782B1 (ja) * 2021-04-28 2022-02-10 Ｃａｅｔｕｓ Ｔｅｃｈｎｏｌｏｇｙ株式会社 親水性多糖高分子を含有する粉末の水分散液の製造方法
JP7007781B1 (ja) * 2021-04-28 2022-02-10 Ｃａｅｔｕｓ Ｔｅｃｈｎｏｌｏｇｙ株式会社 水分散装置
WO2022230210A1 (fr) * 2021-04-28 2022-11-03 Ｃａｅｔｕｓ Ｔｅｃｈｎｏｌｏｇｙ株式会社 Dispositif de dispersion d'eau et dispersion aqueuse de polymère de polysaccharide hydrophile
WO2022230209A1 (fr) * 2021-04-28 2022-11-03 Ｃａｅｔｕｓ Ｔｅｃｈｎｏｌｏｇｙ株式会社 Procédé de fabrication d'une dispersion aqueuse de poudre contenant un polymère de polysaccharide hydrophile, et dispersion aqueuse de polymère de polysaccharide hydrophile

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