WO2009113193A1 - 回転摺動シールの製造方法及び回転摺動シール - Google Patents
回転摺動シールの製造方法及び回転摺動シール Download PDFInfo
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- WO2009113193A1 WO2009113193A1 PCT/JP2008/065736 JP2008065736W WO2009113193A1 WO 2009113193 A1 WO2009113193 A1 WO 2009113193A1 JP 2008065736 W JP2008065736 W JP 2008065736W WO 2009113193 A1 WO2009113193 A1 WO 2009113193A1
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- sliding seal
- weight
- rotary sliding
- fluororubber
- rotating
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/14—Peroxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08L27/16—Homopolymers or copolymers or vinylidene fluoride
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
- C09D175/16—Polyurethanes having carbon-to-carbon unsaturated bonds having terminal carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/10—Materials in mouldable or extrudable form for sealing or packing joints or covers
- C09K3/1006—Materials in mouldable or extrudable form for sealing or packing joints or covers characterised by the chemical nature of one of its constituents
- C09K3/1009—Fluorinated polymers, e.g. PTFE
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- 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
- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
- C08K3/013—Fillers, pigments or reinforcing additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
Definitions
- the present invention relates to a method for manufacturing a rotary slide seal and a rotary slide seal, and more particularly to a method for manufacturing a rotary slide seal and a rotary slide seal excellent in eccentric tracking.
- Patent Document 3 those using vinylidene fluoride fluororubber (FKM) as a base polymer are conventionally known from the viewpoint of heat resistance and oil resistance (Patent Documents 1 and 2).
- Patent Document 4 discloses a non-adhesive and low-friction fluororubber composition in which 2 to 10 parts by weight of zinc oxide and 1 to 5 parts by weight of magnesium oxide are blended as an acid acceptor with 100 parts by weight of a ternary fluororubber. Things are disclosed.
- This ternary fluororubber is a polyol-crosslinked fluororubber, and this ternary fluororubber alone has a poor eccentricity followability and has a drawback that it cannot be used as a rotary sliding seal.
- the object of the present invention is to reduce the torque (lower friction), improve the initial characteristics of the sealing performance (the amount of oil pump accompanying the sliding of the seal member) by reducing oil leakage, and after frictional wear has occurred Further, it is an object of the present invention to provide a method of manufacturing a rotary sliding seal and a rotary sliding seal that can suppress deterioration of the characteristics and improve the eccentric followability.
- a peroxide is added to a fluororubber polymer component comprising 95 to 40% by weight of a ternary fluororubber polymer copolymerized with perfluoroalkyl vinyl ether and 5 to 60% by weight of a liquid fluororubber polymer.
- a method for producing a rotary sliding seal is characterized in that a fluororubber composition is prepared by blending a system cross-linking agent, followed by crosslinking and molding.
- the invention according to claim 2 is that the fluororubber polymer component comprises 80 to 50% by weight of a ternary fluororubber polymer copolymerized with perfluoroalkyl vinyl ether and 20 to 50% by weight of a liquid fluororubber polymer.
- the invention according to claim 3 is characterized in that 0.5 to 10 parts by weight of the peroxide-based crosslinking agent is used as an active ingredient with respect to 100 parts by weight of the fluororubber polymer component. 2.
- the invention described in claim 4 is a rotary sliding seal obtained by the method of manufacturing a rotary sliding seal according to any one of claims 1 to 3.
- the invention according to claim 5 is the rotary sliding seal according to claim 4, wherein the TR-10 value by the following measurement method is -20 ° C or lower.
- TR-10 value In accordance with JIS K 6261, with a low-temperature elastic recovery tester, the rotary sliding seal sample was stretched by 50%, the temperature was lowered, and the glass was vitrified below the glass transition point (Tg). The temperature at which the sample is relaxed and 10% of the initial elongation is recovered is defined as a TR-10 value.
- the initial characteristics of the torque reduction (lower friction) and the sealing performance (oil pump amount accompanying the sliding of the seal member) are improved by reducing oil leakage, and after frictional wear occurs. It is possible to provide a method of manufacturing a rotary sliding seal and a rotary sliding seal that can suppress deterioration of the characteristics and improve eccentric followability.
- the method for producing a rotary sliding seal according to the present invention comprises a fluororubber polymer component comprising 95 to 40% by weight of a ternary fluororubber polymer copolymerized with perfluoroalkyl vinyl ether and 5 to 60% by weight of a liquid fluororubber polymer.
- a fluororubber composition is prepared by blending a peroxide-based crosslinking agent, followed by crosslinking and molding.
- a ternary fluorororubber polymer copolymerized with perfluoroalkyl vinyl ether (hereinafter referred to as ternary fluororubber polymer of the present invention) is composed of perfluoroalkyl vinyl ether and one or more fluorine-containing olefins (polymer or A ternary copolymer with a copolymer) and a peroxide crosslinking type.
- fluorinated olefin examples include vinylidene fluoride, hexafluoropropylene, pentafluoropropylene, trifluoroethylene, trifluorochloroethylene, tetrafluoroethylene, vinyl fluoride, perfluoroacrylic acid ester, perfluoroalkyl acrylate, and the like. Can be mentioned.
- ternary fluororubber polymer of the present invention examples include peroxide crosslinked type vinylidene fluoride-hexafluoropropylene-perfluoroalkyl vinyl ether ternary fluororubber polymer (abbreviation: VdF / TFE / PMVE). .
- polymers can be obtained by solution polymerization, suspension polymerization or emulsion polymerization by a conventionally known method and can be obtained as commercial products (for example, GLT type, GFLT type manufactured by DuPont).
- liquid fluororubber polymer examples include a vinylidene fluoride-hexafluoropropylene copolymer, a vinylidene fluoride-hexafluoropropylene-tetrafluoroethylene copolymer, and a perfluoropropylene oxide-based copolymer. (At 100 ° C.) is preferably in the range of about 400 to 4000 cps, more preferably in the range of about 500 to 3000 cps for the purpose of solving the problems of the present invention.
- the liquid fluororubber polymer is obtained by solution polymerization, suspension polymerization or emulsion polymerization by a conventionally known method, and is available as a commercial product (for example, Diel G-101 manufactured by Daikin Industries, Ltd., Shin-Etsu). Chemical industry SIFEL series, DuPont Viton LM, etc.).
- the blending ratio of the ternary fluororubber polymer of the present invention to the liquid fluororubber polymer in the fluororubber polymer component is 95 to 40% by weight of the ternary fluororubber polymer of the present invention.
- the preferred blending ratio is 20 to 50% by weight of the liquid fluororubber polymer with respect to 80 to 50% by weight of the ternary fluororubber polymer of the present invention (the total weight of the fluororubber polymer component is 100% by weight). %).
- liquid fluororubber polymer is less than 5% by weight, the eccentricity followability cannot be improved, and it is not suitable for rotary sliding seal applications. On the other hand, when it exceeds 60% by weight, moldability such as generation of mold adhesion is deteriorated.
- an organic peroxide crosslinking agent can be preferably used as the peroxide crosslinking agent.
- the organic peroxide crosslinking agent include 2,5-dimethylhexane-2,5-dihydroperoxide, 2,5- Dimethyl-2,5-di (benzoylperoxy) hexane, tert-butyl peroxide, dicumyl peroxide, tert-butylcumyl peroxide, 1,1-di (tert-butylperoxy) -3,3,5 -Trimethylcyclohexane, 2,5-dimethyl-2,5-di (tert-butylperoxy) hexane, 2,5-dimethyl-2,5-di (tert-butylperoxy) hexyne-3, 1,3- Di (tert-butylperoxyisopropyl) benzene, tert-butylperoxybenzoate, tert-butylperoxyisoprop
- crosslinking agent a commercially available product (for example, Japanese fat product Perhexa 25B-40) can be used as it is.
- peroxide-based crosslinking agent a commercially available master batch containing a raw rubber component and a crosslinking agent may be used.
- the content of the peroxide-based crosslinking agent is preferably in the range of 0.5 to 10 parts by weight as an active ingredient per 100 parts by weight of the fluororubber polymer component. This is because, as a characteristic of the rotary sliding seal which is a cross-linked body obtained, the friction can be lowered while improving the low-temperature property, and the eccentric followability can be improved.
- a crosslinking accelerator (auxiliary) that can be used in the peroxide-based crosslinking system
- a metal oxide typified by zinc oxide, triallyl isocyanurate, or the like is used.
- a fatty acid typified by stearic acid or a silica-based reinforcing agent is blended, triethanolamine, diethylene glycol and the like can be mentioned.
- the content of the crosslinking accelerator is preferably in the range of 0.1 to 10 parts by weight, more preferably in the range of 0.2 to 5 parts by weight per 100 parts by weight of the fluororubber polymer component.
- reinforcing agents such as carbon black and carbon fibers; hydrotalcite (Mg 6 Al 2 (OH) 16 CO 3 ), calcium carbonate, magnesium carbonate, water Fillers such as aluminum oxide, magnesium hydroxide, aluminum silicate, magnesium silicate, calcium silicate, potassium titanate, titanium oxide, barium sulfate, aluminum borate, glass fiber, aramid fiber, diatomaceous earth, wollastonite; wax, Processing aids such as metal soap and carnauba wax; acid acceptors such as calcium hydroxide, magnesium oxide and zinc oxide; anti-aging agents; thermoplastic resins; common in the rubber industry such as clay and other fibrous fillers Crosslinking agents used in the present invention and crosslinking accelerators Optionally be added within a range that does not impair the effect.
- hydrotalcite Mg 6 Al 2 (OH) 16 CO 3
- Fillers such as aluminum oxide, magnesium hydroxide, aluminum silicate, magnesium silicate, calcium silicate, potassium titanate, titanium oxide, barium sulfate, aluminum borate, glass fiber
- calcium hydroxide can be preferably used for appropriately adjusting the crosslinking density, and is preferable for reducing the friction coefficient of the crosslinked fluororubber and obtaining a low rebound resilience. Further, foaming hardly occurs during molding. This is desirable from the point of view. In order to obtain a low rebound resilience of the crosslinked fluororubber, a low friction coefficient and a low adhesive strength, it is also preferable to use magnesium oxide.
- a predetermined amount of each of the above components is kneaded with a closed kneader such as an intermix, kneader, banbury mixer, or a general kneader for rubber such as an open roll.
- a closed kneader such as an intermix, kneader, banbury mixer, or a general kneader for rubber such as an open roll.
- a solvent or the like dispersed with a stirrer or the like.
- Rotating and sliding seals can be obtained by pressing, heating and vulcanizing the fluororubber composition prepared as described above to form a crosslinked product (vulcanized product).
- the fluorororubber composition prepared as described above is usually used in an injection molding machine, a compression molding machine, a vulcanizing press machine, an oven, or the like, usually at a temperature of 140 ° C. to 230 ° C. for 1 to 120 ° C.
- a temperature of 140 ° C. to 230 ° C. for 1 to 120 ° C. By heating for about a minute (primary vulcanization), it is possible to form a rotary sliding seal which is crosslinked (vulcanized) and is a fluororubber crosslinked product (vulcanized product).
- Primary vulcanization is a process of crosslinking to such an extent that a shape can be maintained in order to form a certain shape (preliminary molding). In the case of a complicated shape, it can be molded by a mold. Further, primary vulcanization is possible even in an oven such as air heating.
- secondary vulcanization may be performed as necessary.
- a normal method may be used, but it is preferable to perform heat treatment at a temperature range of 200 ° C. to 300 ° C. for 1 to 20 hours, for example.
- the rotary sliding seal of the present invention is excellent in low temperature properties.
- the TR-10 value (low temperature property) by the following measurement method is ⁇ 20 ° C. or lower, preferably ⁇ 25 ° C. or lower.
- TR-10 value The measurement method of TR-10 value is as follows. In accordance with JIS K 6261, with a low-temperature elastic recovery tester, the rotary sliding seal sample was stretched 50%, the temperature was lowered, and the glass was vitrified below the glass transition point (Tg). The temperature at which the sample is relaxed and 10% of the initial elongation is recovered is defined as a TR-10 value.
- the rotary sliding seal of the present invention is excellent in that the torque increase rate is small. Specifically, the rate of torque increase by the following measurement method and the following calculation method is 45% or less, preferably 41% or less.
- the torque measurement method and the torque increase rate calculation method are as follows.
- a new rotating sliding seal molded with an inner diameter of 85 mm, an outer diameter of 105 mm, and a width of 13 mm, and a worn product in which a paper file is wound around the rotating shaft and the seal lip of the rotating sliding seal is forcibly worn with a target of 300 ⁇ m of wear.
- Each rotary sliding seal was set on a rotary testing machine, and a rotational test was conducted under conditions of a test temperature of 100 ° C. and a rotational speed of 2000 rpm with the lubricating oil sealed at the center of the shaft.
- the torque related to the seal during the rotation test was measured with the load cell, and the torque increase rate was determined by the following equation.
- Torque increase rate (wear sliding torque-new sliding torque) / new sliding torque
- the rotary sliding seal of the present invention is excellent in pump amount.
- the pump amount decrease rate by the following measurement method is 37% or less, preferably 35% or less.
- the pump amount measurement method and the pump amount reduction rate calculation method are as follows.
- a new rotating sliding seal molded with an inner diameter of 85 mm, an outer diameter of 105 mm, and a width of 13 mm, and a worn product in which a paper file is wound around the rotating shaft and the seal lip of the rotating sliding seal is forcibly worn with a target of 300 ⁇ m of wear.
- For each of the rotating and sliding seals set the rotating tester and seal the lubricating oil at the center of the shaft, and perform a rotation test under the conditions of a test temperature of 100 ° C and a rotation speed of 2000 rpm.
- the rotary sliding seal of the present invention is excellent in eccentricity tracking.
- the ratio of the amount of shaft eccentricity (oil leakage eccentricity / tightening allowance) in which oil leakage occurs with respect to the tightening allowance obtained by the following measurement method is 0.45 or more, preferably 0.60 or more.
- Example 1 Composition ingredients and amount> 1.
- Fluorororubber polymer component -Vinylidene fluoride-hexafluoropropylene-perfluoroalkyl vinyl ether ternary fluororubber polymer (peroxide crosslinking system); (“Viton GLT-600S” manufactured by DuPont Dow Elastomer Co., Ltd.) ⁇ ⁇ ⁇ 80 parts by weight ⁇ Liquid fluororubber polymer; ("Diel G-101" manufactured by Daikin Industries) 20 parts by weight filler; Diatomaceous earth (“Radiolite # 3000” manufactured by Hayashi Kasei Co., Ltd.) 15 parts by weight Wollastonite (“NYAD400” manufactured by NYCO; aspect ratio 5) 35 parts by weight Carbon black; (“N990” manufactured by Cancarb) 2 parts by weight Processing aid; carnauba wax (melting point 860 ° C) (“VPA No.
- Vulcanizing component ⁇ Peroxide-based crosslinking agent; 2,5-dimethylhexane-2,5-dihydroperoxide (Nippon Yushi Co., Ltd. “Perhexa 25B-40”) 2 parts by weight ⁇ Crosslinking aid: triallyl isocyanurate; (Nippon Kasei Co., Ltd. “TAIC WH60”) 2 parts by weight Acid acceptor; ⁇ Calcium hydroxide (“Caldic # 2000” manufactured by Omi Chemical Co., Ltd.) 3 parts by weight Magnesium oxide (“MgO # 150” manufactured by Kyowa Chemical Industry Co., Ltd.) 6 parts by weight
- Rubber hardness Hs measured with a type A durometer in accordance with JIS K6253.
- Tensile strength Tb (MPa) compliant with JIS K-6251.
- Elongation Eb (%) Conforms to JIS K6251 (measured at 23 ⁇ 3 ° C.).
- TR-10 value Low temperature property
- Torque increase rate (wear sliding torque-new sliding torque) / new sliding torque
- the pump amount reduction rate was determined by the following measurement method, and the results are shown in Table 1.
- a new rotating sliding seal molded with an inner diameter of 85 mm, an outer diameter of 105 mm, and a width of 13 mm, and a worn product in which a paper file is wound around the rotating shaft and the seal lip of the rotating sliding seal is forcibly worn with a target of 300 ⁇ m of wear.
- Each rotary sliding seal is set in a rotary testing machine, and with a lubricating oil (Toyota genuine castle oil SM class 10W-30) sealed at the shaft center, a rotational test is performed at a test temperature of 100 ° C. and a rotational speed of 2000 rpm. Then, a certain amount of oil was supplied to the seal lip portion of the new and worn rotary sliding seals, and the time from the oil supply to the end of suction was measured.
- a lubricating oil Toyota genuine castle oil SM class 10W-30
- a fixed amount of oil is supplied to the seal lip portion 2 with a syringe or the like in a state where the rotary sliding seal 1 is normally attached (oil is sucked into the lip), and the oil is supplied.
- 3 is a garter spring
- 4 is an oil film
- 5 is a contact width.
- the ratio of the shaft eccentricity at which oil leakage occurs with respect to the tightening allowance (oil leakage eccentricity / tightening allowance) is obtained, and when this ratio is 0.60 or more, ⁇ , 0.45 to less than 0.60 is ⁇ ,. A value less than 30 to less than 0.45 is indicated by ⁇ and a value less than 0.30 is indicated by ⁇ .
- Example 2 In Example 1, the evaluation was performed in the same manner except that the amounts of the peroxide-based crosslinking agent and the crosslinking aid were each increased to 2.5 parts by weight to increase the crosslinking density. The results are shown in Table 1.
- Example 3 In Example 1, it evaluated similarly except having changed the compounding ratio of ternary fluororubber polymer and liquid fluororubber polymer as shown in Table 1. The results are shown in Table 1.
- Example 4 In Example 1, the blending ratio of the ternary fluororubber polymer and the liquid fluororubber polymer was changed as shown in Table 1, and the amounts of the peroxide crosslinker and the crosslinking aid were increased to 3.6 parts by weight, respectively. And evaluated in the same manner except that the crosslink density was increased. The results are shown in Table 1.
- Example 1 Comparative Example 1 In Example 1, the evaluation was made in the same manner except that only a binary fluororubber polymer having the following composition was used and the crosslinking agent and the crosslinking assistant were changed as follows. The results are shown in Table 1.
- Example 2 Comparative Example 2 In Example 1, the evaluation was made in the same manner except that the liquid fluororubber polymer in the fluororubber polymer component was not used and the ternary fluororubber polymer was changed to 100 parts by weight. The results are shown in Table 1.
- Comparative Example 3 Evaluation was made in the same manner as in Example 1 except that the blending ratio of the ternary fluororubber polymer and the liquid fluororubber polymer in the fluororubber polymer component was changed as shown in Table 1. The results are shown in Table 1.
- Example 4 the blending ratio of the ternary fluororubber polymer and the liquid fluororubber polymer in the fluororubber polymer component is changed as shown in Table 1, and the amounts of the peroxide crosslinker and the crosslinking aid are set to 3. Evaluation was made in the same manner except that the crosslinking density was increased by increasing the amount to 6 parts by weight. The results are shown in Table 1.
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Abstract
Description
〔TR-10値〕
JIS K 6261に準拠し、低温弾性回復試験機で、回転摺動シールサンプルを50%伸長し、温度を下げ、ガラス転移点(Tg)以下でガラス化させた後、徐々に温度を上げて前記サンプルの歪みを緩和させ、初期伸長に対して10%回復した温度をTR-10値とする。
2:シールリップ部
3:ガータスプリング
4:油膜
5:接触幅
<回転摺動シールの製造方法>
本発明に係る回転摺動シールの製造方法は、パーフルオロアルキルビニルエーテルを共重合した3元系フッ素ゴムポリマー95~40重量%と、液状フッ素ゴムポリマー5~60重量%とからなるフッ素ゴムポリマー成分に、過酸化物系架橋剤を配合してフッ素ゴム組成物を調製し、次いで、架橋、成形することを特徴とする。
上記のようにして製造された本発明の回転摺動シールは、以下の特性を有する。
<配合成分と配合量>
1.フッ素ゴムポリマー成分;
・フッ化ビニリデン-ヘキサフルオロプロピレン-パーフルオロアルキルビニルエーテル3元系フッ素ゴムポリマー(過酸化物架橋系);
(デュポン・ダウ・エラストマー社製「バイトンGLT-600S」) ・・・80重量部
・液状フッ素ゴムポリマー;
(ダイキン工業社製「Diel G-101」) ・・・20重量部
2.充填剤;
・珪藻土(林化成社製「ラヂオライト#3000」) ・・・15重量部
・ウォラストナイト(NYCO社製「NYAD400」;アスペクト比5) ・・・35重量部
3.カーボンブラック;
(Cancarb社製「N990」) ・・・2重量部
4.加工助剤;カルナバワックス(融点860℃)
(デュポン・ダウ・エラストマー社製「VPA No.2」) ・・・2重量部
5.加硫成分
・過酸化物系架橋剤;
2,5-ジメチルヘキサン-2,5-ジヒドロペルオキシド(日本油脂製品「パーヘキサ25B-40」) ・・・2重量部
・架橋助剤:トリアリルイソシアヌレート;
(日本化成社製「TAIC WH60」) ・・・2重量部
6.受酸剤;
・水酸化カルシウム(近江化学工業社製「Caldic#2000」) ・・・3重量部
・酸化マグネシウム(協和化学工業社製「MgO#150」) ・・・6重量部
以上の各配合成分(加硫成分を除く)をニーダーに投入して20分混練した後、オープンロールにて加硫成分を投入することで組成物を調製した。
上記組成物(加硫成分を除く)を用いて6インチミキシングロールにより厚さ2mmの未加硫ゴムシートを作製し、これに180℃×60分のプレス加硫の後、200℃×24時間のオーブン加硫を施して、常態物性評価用のシート状のゴム試験片を得た。
び伸びEb(%)を評価した。評価結果を表1に示す。
ゴム硬度Hs;JIS K6253に準拠し、タイプAデュロメーターで測定した。
引張り強さTb(MPa);JIS K-6251に準拠。
伸びEb(%);JIS K6251に準拠(23±3℃にて測定)。
JIS K 6261に準拠し、低温弾性回復試験機で、回転摺動シールサンプルを50%伸長し、温度を下げ、ガラス転移点(Tg)以下でガラス化させた後、徐々に温度を上げて前記サンプルの歪みを緩和させ、初期伸長に対して10%回復した温度をTR-10値とする。結果を表1に示す。
下記測定法によりトルク上昇率を求め、その結果を表1に示す。
内径85mm、外径105mm、幅13mmに成形した新品回転摺動シールと、回転軸に紙ヤスリを巻きつけて、摩耗量300μm狙いで、前記回転摺動シールのシールリップを強制摩耗させた摩耗品回転摺動シールの各々について、回転試験機にセットし、潤滑油(トヨタ純正キャッスルオイルSM級10W-30)を軸中心で密封した状態で、試験温度100℃,回転数2000rpmの条件で回転試験を行い、回転摺動シールに取付けられたロードセルで回転試験時のシールに係るトルクを各々測定し、トルク上昇率を以下の式で求めた。
下記測定法により、ポンプ量低下率を求め、その結果を表1に示す。
内径85mm、外径105mm、幅13mmに成形した新品回転摺動シールと、回転軸に紙ヤスリを巻きつけて、摩耗量300μm狙いで、前記回転摺動シールのシールリップを強制摩耗させた摩耗品回転摺動シールの各々について、回転試験機にセットし、潤滑油(トヨタ純正キャッスルオイルSM級10W-30)を軸中心で密封した状態で、試験温度100℃,回転数2000rpmの条件で回転試験を行い、新品と摩耗品の回転摺動シールのシールリップ部に一定量のオイルを供給し、オイルの供給から吸込み終了までの時間を測定した。
軸を任意に所定量偏心させた回転試験機に、上記の回転摺動シールサンプル(軸偏心なしの状態でのシールリップの締め代は1mmの設定)をセットし、試験温度100℃、回転数2000rpmで回転試験を行い、油の漏れの有無を目視で観察した。回転試験機の軸偏心量を徐々に増大させていき、油漏れが生じる軸偏心量を求めた。
以下の評価基準に従って評価し、その結果を表1に示す。
実施例1において、過酸化物系架橋剤と架橋助剤の量を各々2.5重量部に増加させ、架橋密度を上昇させた以外は同様にして評価した。その結果を表1に示す。
実施例1において、3元系フッ素ゴムポリマーと液状フッ素ゴムポリマーの配合比を表1のように変化させた以外は同様にして評価した。その結果を表1に示す。
実施例1において、3元系フッ素ゴムポリマーと液状フッ素ゴムポリマーの配合比を表1のように変化させ、さらに過酸化物系架橋剤と架橋助剤の量を各々3.6重量部に増加させ、架橋密度を上昇させた以外は同様にして評価した。その結果を表1に示す。
実施例1において、以下の組成の2元系フッ素ゴムポリマーのみを用い、更に架橋剤及び架橋助剤を以下のように代えた以外は同様にして評価した。その結果を表1に示す。
1.2元系フッ素ゴムポリマー;
フッ化ビニリデン-ヘキサフルオロプロピレン2元系フッ素ゴムポリマー;
(デュポン・ダウ・エラストマー社製「バイトンA500」;ポリオール加硫系、ムーニー粘度ML1+10(121℃)45) ・・・100重量部
2.加硫成分;
・ビスフェノールAF
(デュポン・ダウ・エラストマー社製「キュラティブVC#30」;ジヒドロキシ芳香族化合物50%、バイトンE45:50%のマスターバッチ) ・・・2.5重量部
・加硫促進剤
(デュポン・ダウ・エラストマー社製「キュラティブVC#20」;有機ホスホニウム塩:33%、バイトンE45:67%のマスターバッチ) ・・・1.2重量部
実施例1において、フッ素ゴムポリマー成分中の液状フッ素ゴムポリマーを用いずに、3元系フッ素ゴムポリマーを100重量部とした以外は同様にして評価した。その結果を表1に示す。
実施例1において、フッ素ゴムポリマー成分中の3元系フッ素ゴムポリマーと液状フッ素ゴムポリマーの配合比を表1のように代えた以外は同様にして評価した。その結果を表1に示す。
実施例1において、フッ素ゴムポリマー成分中の3元系フッ素ゴムポリマーと液状フッ素ゴムポリマーの配合比を表1のように代え、さらに過酸化物系架橋剤と架橋助剤の量を各々3.6重量部に増加させ、架橋密度を上昇させた以外は同様にして評価した。その結果を表1に示す。
Claims (5)
- パーフルオロアルキルビニルエーテルを共重合した3元系フッ素ゴムポリマー95~40重量%と、液状フッ素ゴムポリマー5~60重量%とからなるフッ素ゴムポリマー成分に、過酸化物系架橋剤を配合してフッ素ゴム組成物を調製し、次いで、架橋、成形することを特徴とする回転摺動シールの製造方法。
- 前記フッ素ゴムポリマー成分が、パーフルオロアルキルビニルエーテルを共重合した3元系フッ素ゴムポリマー80~50重量%と、液状フッ素ゴムポリマー20~50重量%とからなることを特徴とする請求項1記載の回転摺動シールの製造方法。
- 前記過酸化物系架橋剤を、前記フッ素ゴムポリマー成分100重量部に対して、有効成分として0.5~10重量部使用することを特徴とする請求項1又は2記載の回転摺動シールの製造方法。
- 請求項1~3の何れかに記載の回転摺動シールの製造方法によって得られる回転摺動シール。
- 下記測定法によるTR-10値が、-20℃以下である請求項4記載の回転摺動シール。
〔TR-10値〕
JIS K 6261に準拠し、低温弾性回復試験機で、回転摺動シールサンプルを50%伸長し、温度を下げ、ガラス転移点(Tg)以下でガラス化させた後、徐々に温度を上げて前記サンプルの歪みを緩和させ、初期伸長に対して10%回復した温度をTR-10値とする。
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US12/673,068 US20110291365A1 (en) | 2008-03-11 | 2008-09-02 | Method for producing rotary shaft seal and rotary shaft seal |
EP08873244A EP2251393A1 (en) | 2008-03-11 | 2008-09-02 | Process for producing rotating/sliding seal and rotating/sliding seal |
CN200880103957A CN101784632A (zh) | 2008-03-11 | 2008-09-02 | 旋转滑动密封件的制造方法及旋转滑动密封件 |
JP2010502689A JP5131347B2 (ja) | 2008-03-11 | 2008-09-02 | 回転摺動シールの製造方法及び回転摺動シール |
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JP5209280B2 (ja) * | 2007-11-20 | 2013-06-12 | 株式会社ジェイテクト | 密封装置 |
EP2251393A1 (en) * | 2008-03-11 | 2010-11-17 | NOK Corporation | Process for producing rotating/sliding seal and rotating/sliding seal |
US9074116B2 (en) * | 2009-09-14 | 2015-07-07 | Nok Corporation | Fluororubber composition |
KR102015862B1 (ko) * | 2012-08-10 | 2019-08-29 | 에누오케 가부시키가이샤 | 불소 고무 조성물 |
JP6183447B2 (ja) * | 2013-02-18 | 2017-08-23 | イーグル工業株式会社 | ウォーターポンプ用リップシール |
US10294345B2 (en) | 2014-05-08 | 2019-05-21 | Nok Corporation | Ethylene-acrylic rubber composition, ethylene-acrylic rubber, rubber metal composite, and bonded piston sealing |
US20220025166A1 (en) * | 2018-12-06 | 2022-01-27 | Arkema Inc. | Fluoro-thermoplastic elastomer blends |
KR102546066B1 (ko) * | 2022-12-07 | 2023-06-28 | 유한회사 부산프로펠러공사 | 선박용 수중 메커니컬 씰 밀봉용 고무 튜브 제조방법 및 이에 의해 제조된 고무 튜브 |
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- 2008-09-02 EP EP08873244A patent/EP2251393A1/en not_active Withdrawn
- 2008-09-02 US US12/673,068 patent/US20110291365A1/en not_active Abandoned
- 2008-09-02 JP JP2010502689A patent/JP5131347B2/ja not_active Expired - Fee Related
- 2008-09-02 KR KR1020107005259A patent/KR20100121591A/ko not_active Application Discontinuation
- 2008-09-02 WO PCT/JP2008/065736 patent/WO2009113193A1/ja active Application Filing
- 2008-09-02 CN CN200880103957A patent/CN101784632A/zh active Pending
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CN101784632A (zh) | 2010-07-21 |
EP2251393A1 (en) | 2010-11-17 |
JPWO2009113193A1 (ja) | 2011-07-21 |
US20110291365A1 (en) | 2011-12-01 |
KR20100121591A (ko) | 2010-11-18 |
JP5131347B2 (ja) | 2013-01-30 |
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