JP7533308B2 - Manufacturing method for heat-resistant anti-vibration rubber - Google Patents
Manufacturing method for heat-resistant anti-vibration rubber Download PDFInfo
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- 229920001971 elastomer Polymers 0.000 title claims description 209
- 239000005060 rubber Substances 0.000 title claims description 209
- 238000004519 manufacturing process Methods 0.000 title claims description 24
- 238000004898 kneading Methods 0.000 claims description 125
- 239000003431 cross linking reagent Substances 0.000 claims description 67
- 239000000203 mixture Substances 0.000 claims description 49
- 238000004132 cross linking Methods 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 23
- 238000000465 moulding Methods 0.000 claims description 13
- 238000013329 compounding Methods 0.000 claims description 8
- 229920005558 epichlorohydrin rubber Polymers 0.000 claims description 6
- 229920000800 acrylic rubber Polymers 0.000 claims description 4
- 229920003244 diene elastomer Polymers 0.000 claims description 4
- 229920000058 polyacrylate Polymers 0.000 claims description 4
- 229920001973 fluoroelastomer Polymers 0.000 claims description 3
- 238000002156 mixing Methods 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 12
- 239000000463 material Substances 0.000 description 10
- 238000011156 evaluation Methods 0.000 description 9
- 239000012467 final product Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 8
- 239000000654 additive Substances 0.000 description 5
- 244000043261 Hevea brasiliensis Species 0.000 description 4
- 238000013016 damping Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 229920003049 isoprene rubber Polymers 0.000 description 4
- 229920003052 natural elastomer Polymers 0.000 description 4
- 229920001194 natural rubber Polymers 0.000 description 4
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 description 2
- -1 CO) Polymers 0.000 description 2
- PDQAZBWRQCGBEV-UHFFFAOYSA-N Ethylenethiourea Chemical compound S=C1NCCN1 PDQAZBWRQCGBEV-UHFFFAOYSA-N 0.000 description 2
- 229920000459 Nitrile rubber Polymers 0.000 description 2
- 239000005062 Polybutadiene Substances 0.000 description 2
- 229920005683 SIBR Polymers 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229920005549 butyl rubber Polymers 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229920001084 poly(chloroprene) Polymers 0.000 description 2
- 229920002857 polybutadiene Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- 239000004636 vulcanized rubber Substances 0.000 description 2
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical group C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000004606 Fillers/Extenders Substances 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000001721 transfer moulding Methods 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
- Arrangement Or Mounting Of Propulsion Units For Vehicles (AREA)
- Vibration Prevention Devices (AREA)
Description
本開示は、耐熱性防振ゴムの製造方法に関する。 This disclosure relates to a method for manufacturing heat-resistant anti-vibration rubber.
従来、車両のエンジンマウント等に用いられるゴム部材には、防振性および耐熱性が求められる。このように複数の特性を有する高機能性のゴム材料として、例えば、特許文献１には、芳香族ビニル単量体とブタジエン単量体の共重合ゴムと、ジエン系ゴムと、特定の伸展油を配合した防振ゴム用組成物が開示されており、防振性および防音性を備えると記載されている。 Conventionally, rubber members used in vehicle engine mounts and the like are required to have vibration-proofing and heat resistance. For example, Patent Document 1 discloses a highly functional rubber material with multiple properties, which is a rubber composition for vibration-proof rubber that is a blend of a copolymer rubber of an aromatic vinyl monomer and a butadiene monomer, a diene rubber, and a specific extender oil, and is described as having vibration-proofing and soundproofing properties.
また、特許文献２には、未加硫のゴム材料Ａ中に未加硫のゴム材料Ｂを均一に混錬、分散せしめた状態下において、ゴム材料Ｂの加硫を行うことによって加硫ゴム材料Ｂが形成され、そのような加硫ゴム材料Ｂの分散状態下で、未加硫のゴム材料Ａが加硫されることによって得られる防振ゴムが、低動バネ特性および高減衰特性を備えると記載されている。 Patent Document 2 also describes how unvulcanized rubber material B is uniformly mixed and dispersed in unvulcanized rubber material A, and then vulcanized rubber material B is formed by vulcanizing the rubber material B, and how the vibration-proof rubber obtained by vulcanizing unvulcanized rubber material A in such a dispersed state of vulcanized rubber material B has low dynamic spring properties and high damping properties.
防振性に優れたゴム成分や耐熱性に優れたゴム成分など、特性の異なるゴム成分には、それぞれ適した架橋剤が存在する。架橋剤が対応するゴム成分と十分に反応して架橋反応を進行させることで、架橋後のゴム成分は特性を発現させることができる。 There are cross-linking agents suitable for rubber components with different properties, such as rubber components with excellent vibration damping properties and rubber components with excellent heat resistance. When the cross-linking agent reacts sufficiently with the corresponding rubber component to advance the cross-linking reaction, the rubber component after cross-linking can express its properties.
特許文献１では、ゴム成分の混錬のタイミングや架橋剤の添加のタイミングは明確に定められていない。特許文献２では、２種類の架橋剤が段階的に添加されているものの、架橋剤の添加の前に異なるゴム成分どうしが混錬されている。このような方法では、各ゴム成分に対して、それぞれ適切な架橋剤が十分に反応しないと考えられる。 In Patent Document 1, the timing of kneading the rubber components and the timing of adding the crosslinking agent are not clearly defined. In Patent Document 2, two types of crosslinking agents are added in stages, but different rubber components are kneaded together before adding the crosslinking agents. With this method, it is thought that the appropriate crosslinking agent does not react sufficiently with each rubber component.
ここに開示する技術は、耐熱性防振ゴムの製造方法において、優れた耐熱性および防振性の両方を兼ね備える耐熱性防振ゴムを得ることが可能となる。 The technology disclosed here makes it possible to obtain heat-resistant anti-vibration rubber that has both excellent heat resistance and vibration-proofing properties through a manufacturing method for heat-resistant anti-vibration rubber.
本開示は、上記課題を解決するために、ゴム成分とそれに適した架橋剤を予め混錬した後、複数のゴム成分を混錬することにより、ゴム成分と対応する架橋剤とを十分に反応可能にすることに着目した。 In order to solve the above problem, the present disclosure focuses on pre-mixing a rubber component with a suitable cross-linking agent, and then mixing multiple rubber components to allow the rubber component and the corresponding cross-linking agent to react sufficiently.
具体的に、ここに開示する技術は、耐熱性防振ゴムの製造方法に係るものであり、防振性を有するゴム成分Ａおよび該ゴム成分Ａを架橋可能な架橋剤Ａ’を混錬し、防振性ゴム組成物を得る第１混錬工程と、耐熱性を有するゴム成分Ｂおよび該ゴム成分Ｂを架橋可能な架橋剤Ｂ’を混錬し、耐熱性ゴム組成物を得る第２混錬工程と、前記防振性ゴム組成物および前記耐熱性ゴム組成物を混錬し、ゴム混合物を得る第３混錬工程と、前記ゴム混合物の架橋を行う架橋成形工程と、を含むことを特徴とする。 Specifically, the technology disclosed herein relates to a method for producing heat-resistant anti-vibration rubber, and is characterized by including a first kneading step in which a rubber component A having anti-vibration properties and a crosslinking agent A' capable of crosslinking the rubber component A are kneaded to obtain an anti-vibration rubber composition, a second kneading step in which a rubber component B having heat resistance and a crosslinking agent B' capable of crosslinking the rubber component B are kneaded to obtain a heat-resistant rubber composition, a third kneading step in which the anti-vibration rubber composition and the heat-resistant rubber composition are kneaded to obtain a rubber mixture, and a crosslinking molding step in which the rubber mixture is crosslinked.
ゴム成分Ａとゴム成分Ｂは、それぞれ対応する架橋剤Ａ’，Ｂ’と予め混錬されることにより、ゴム混合物となった状態において、ゴム成分とそれに対応する架橋剤とが反応しやすい状態で分布する。そのため、架橋成形工程において、ゴム成分Ａおよび対応する架橋剤Ａ’と、ゴム成分Ｂおよび対応する架橋剤Ｂ’が十分に反応し、最終生成物においてゴム成分Ａの特性とゴム成分Ｂの特性をそれぞれ発現させることができるため、優れた耐熱性および防振性の両方を兼ね備える耐熱性防振ゴムを得ることが可能となる。 Rubber component A and rubber component B are premixed with the corresponding crosslinking agents A' and B', respectively, so that in the rubber mixture, the rubber components and the corresponding crosslinking agents are distributed in a state that makes them easy to react with each other. Therefore, in the crosslinking molding process, rubber component A and the corresponding crosslinking agent A' react sufficiently with rubber component B and the corresponding crosslinking agent B', and the characteristics of rubber component A and the characteristics of rubber component B can be expressed in the final product, respectively, making it possible to obtain a heat-resistant vibration-proof rubber that combines both excellent heat resistance and vibration-proofing properties.
なお、前記ゴム成分Ａと前記ゴム成分Ｂとの配合比率が３：７～７：３の範囲であることが好ましい。 It is preferable that the compounding ratio of the rubber component A to the rubber component B is in the range of 3:7 to 7:3.
このような配合比率の範囲であれば、最終生成物である耐熱性防振ゴムにおいて、優れた耐熱性および防振性をバランス良く兼ね備えることが可能となる。 With this blend ratio range, the final product, heat-resistant anti-vibration rubber, can have a good balance of excellent heat resistance and vibration-proofing properties.
また、前記ゴム成分Ａが、ジエン系ゴムであり、前記ゴム成分Ｂが、エピクロロヒドリンゴム、アクリルゴム、フッ素ゴムからなる群より選択される少なくとも１種であることが好ましい。 It is also preferable that the rubber component A is a diene rubber, and the rubber component B is at least one selected from the group consisting of epichlorohydrin rubber, acrylic rubber, and fluororubber.
また、前記第１混錬工程、前記第２混錬工程、および前記第３混錬工程は、６０℃以上１４０℃以下の排出温度で行われることが好ましい。 Furthermore, it is preferable that the first kneading process, the second kneading process, and the third kneading process are performed at a discharge temperature of 60°C or higher and 140°C or lower.
排出温度が６０℃以上であれば、架橋剤がゴム成分内に十分に分散され、架橋反応が進み易く、最終生成物である耐熱性防振ゴムにおいてゴム成分Ａおよびゴム成分Ｂの特性を十分に発現させることができる。排出温度が１４０℃以下であれば、架橋成形工程の前に架橋反応が起こってスコーチが発生するのを防ぐことができる。 If the discharge temperature is 60°C or higher, the crosslinking agent is sufficiently dispersed within the rubber component, the crosslinking reaction proceeds easily, and the properties of rubber component A and rubber component B can be fully expressed in the final product, heat-resistant vibration-proof rubber. If the discharge temperature is 140°C or lower, it is possible to prevent the crosslinking reaction from occurring before the crosslinking molding process, which would cause scorch.
さらに、前記第１混錬工程における混錬時間は３分以上であり、前記第２混錬工程における混錬時間は１分以上であり、前記第３混錬工程における混錬時間は１分以上であることが好ましい。また、前記第１混錬工程、前記第２混錬工程および前記第３混錬工程の混錬時間の合計が６０分以内であることが好ましい。 Furthermore, it is preferable that the kneading time in the first kneading process is 3 minutes or more, the kneading time in the second kneading process is 1 minute or more, and the kneading time in the third kneading process is 1 minute or more. It is also preferable that the total kneading time in the first kneading process, the second kneading process, and the third kneading process is 60 minutes or less.
第１混錬工程および第２混錬工程において、架橋剤がゴム成分内に十分に分散されるような混錬時間とすることにより、架橋反応がより進み易く、最終生成物である耐熱性防振ゴムにおいてゴム成分Ａおよびゴム成分Ｂの特性を十分に発現させることができる。また、第３混錬工程において、耐熱性ゴム組成物と防振性ゴム成分とがバランスよく分布するような混錬時間とすることにより、最終生成物である耐熱性防振ゴムにおいてゴム成分Ａおよびゴム成分Ｂの特性をバランスよく発現させることができる。さらに、各混錬時間の合計を６０分以内とすれば、耐熱性防振ゴムの生産性に優れる。 In the first and second kneading steps, by setting the kneading time so that the crosslinking agent is sufficiently dispersed in the rubber components, the crosslinking reaction proceeds more easily, and the properties of rubber components A and B can be fully expressed in the final product, heat-resistant anti-vibration rubber. In addition, by setting the kneading time in the third kneading step so that the heat-resistant rubber composition and the anti-vibration rubber components are distributed in a balanced manner, the properties of rubber components A and B can be fully expressed in the final product, heat-resistant anti-vibration rubber. Furthermore, if the total kneading time is within 60 minutes, the productivity of the heat-resistant anti-vibration rubber is excellent.
以上説明したように、本開示によれば、優れた耐熱性および防振性の両方を兼ね備える耐熱性防振ゴムを得ることが可能となる。 As described above, this disclosure makes it possible to obtain heat-resistant anti-vibration rubber that combines both excellent heat resistance and vibration damping properties.
以下、本開示を実施するための形態を説明する。以下の好ましい実施形態の説明は、本質的に例示に過ぎず、本開示、その適用物或いはその用途を制限することを意図するものではない。 The following describes the form for implementing the present disclosure. The following description of the preferred embodiment is merely exemplary in nature and is not intended to limit the present disclosure, its applications, or its uses.
＜耐熱性防振ゴムの組成＞
本実施形態に係る耐熱性防振ゴムは、防振性を有するゴム成分Ａおよびゴム成分Ａを架橋可能な架橋剤Ａ’と、耐熱性を有するゴム成分Ｂおよびゴム成分Ｂを架橋可能な架橋剤Ｂ’と、を含むものであり、防振性を有するゴム成分Ａおよび架橋剤Ａ’と、耐熱性を有するゴム成分Ｂおよび架橋剤Ｂ’とが、それぞれ予め十分に混錬された後に、混ぜ合わさされて架橋成形される。
<Composition of heat-resistant anti-vibration rubber>
The heat-resistant vibration-proof rubber of this embodiment contains a rubber component A having vibration-proof properties and a crosslinking agent A' capable of crosslinking rubber component A, and a rubber component B having heat resistance and a crosslinking agent B' capable of crosslinking rubber component B. The rubber component A and crosslinking agent A' having vibration-proof properties, and the rubber component B and crosslinking agent B' having heat resistance are each thoroughly kneaded in advance, and then mixed together and crosslinked to form the product.
ゴム成分Ａとしては、防振性に優れるジエン系ゴムを広く使用可能であり、特に制限はないが、例えば、天然ゴム（ＮＲ）、イソプレンゴム（ＩＲ）、ブタジエンゴム（ＢＲ）、スチレンブタジエンゴム（ＳＢＲ）、スチレンイソプレンブタジエンゴム（ＳＩＢＲ）、クロロプレンゴム（ＣＲ）、アクリロニトリルブタジエンゴム（ＮＢＲ）、ブチルゴム（ＩＩＲ）等が挙げられる。これらのゴム成分より１種を用いても、２種以上を組み合わせて用いてもよい。 As rubber component A, a wide variety of diene rubbers with excellent vibration-proofing properties can be used, and there are no particular restrictions. Examples include natural rubber (NR), isoprene rubber (IR), butadiene rubber (BR), styrene butadiene rubber (SBR), styrene isoprene butadiene rubber (SIBR), chloroprene rubber (CR), acrylonitrile butadiene rubber (NBR), and butyl rubber (IIR). One of these rubber components may be used, or two or more may be used in combination.
ゴム成分Ａを架橋可能な架橋剤Ａ’としては、選択されたゴム成分Ａに対応する適切な架橋剤として公知のものを広く使用可能であり、特に制限はないが、例えば、硫黄が挙げられる。 As the crosslinking agent A' capable of crosslinking the rubber component A, a wide range of known crosslinking agents suitable for the selected rubber component A can be used, and although there are no particular limitations, examples include sulfur.
ゴム成分Ｂとしては、耐熱性に優れる公知のゴム成分を広く使用可能であり、特に制限はないが、例えば、エピクロロヒドリンゴム（ＥＣＯ，ＣＯ）、アクリルゴム（ＡＣＭ，ＡＮＭ）、フッ素ゴム（ＦＫＭ，ＦＰＭ）が挙げられる。これらのゴム成分より１種を用いても、２種以上を組み合わせて用いてもよい。 As the rubber component B, a wide variety of known rubber components having excellent heat resistance can be used, and although there are no particular limitations, examples include epichlorohydrin rubber (ECO, CO), acrylic rubber (ACM, ANM), and fluororubber (FKM, FPM). One of these rubber components may be used, or two or more may be used in combination.
ゴム成分Ｂを架橋可能な架橋剤Ｂ’としては、選択されたゴム成分Ｂに対応する適切な架橋剤として公知のものを広く使用可能であり、特に制限はないが、例えば、エチレンチオウレアなどのチオウレア系架橋剤やジクミルパーオキサイドなどの過酸化物架橋剤が挙げられる。 As the crosslinking agent B' capable of crosslinking the rubber component B, a wide range of known crosslinking agents suitable for the selected rubber component B can be used, and although there are no particular limitations, examples include thiourea crosslinking agents such as ethylene thiourea and peroxide crosslinking agents such as dicumyl peroxide.
ゴム成分Ａと架橋剤Ａ’とを第１混錬工程において、また、ゴム成分Ｂと架橋剤Ｂ’とを第２混錬工程において混錬する際、ゴム成分Ａ，Ｂ、架橋剤Ａ’，Ｂ’以外の成分を添加剤として配合してもよい。例えば、ゴム成分Ａおよび架橋剤Ａ’には、促進助剤として酸化亜鉛（ＺｎＯ）やステアリン酸を添加してもよい。また例えば、ゴム成分Ｂおよび架橋剤Ｂ’には、受酸剤として酸化カルシウム（ＣａＯ）などの金属酸化物を添加してもよい。また、ゴム成分Ａおよび架橋剤Ａ’とム成分Ｂおよび架橋剤Ｂ’に共通して、カーボンブラックやシリカなどの補強剤や、シランカップリング剤、６ＰＰＤなどの老化防止剤やその他の添加剤を配合してもよい。 When rubber component A and crosslinking agent A' are mixed in the first mixing step, and rubber component B and crosslinking agent B' are mixed in the second mixing step, components other than rubber components A and B and crosslinking agents A' and B' may be mixed as additives. For example, zinc oxide (ZnO) or stearic acid may be added to rubber component A and crosslinking agent A' as an accelerating agent. For example, metal oxides such as calcium oxide (CaO) may be added to rubber component B and crosslinking agent B' as an acid acceptor. In addition, reinforcing agents such as carbon black and silica, silane coupling agents, anti-aging agents such as 6PPD, and other additives may be mixed in common to rubber component A and crosslinking agent A' and rubber component B and crosslinking agent B'.
前記ゴム成分Ａと前記ゴム成分Ｂとの配合比率は３：７～７：３の範囲であることが好ましい。このような配合比率の範囲とすることで、最終生成物である耐熱性防振ゴムにおいて優れた耐熱性および防振性をバランス良く兼ね備えることが可能となる。 The compounding ratio of the rubber component A to the rubber component B is preferably in the range of 3:7 to 7:3. By setting the compounding ratio in this range, it is possible to obtain a good balance between excellent heat resistance and vibration damping properties in the final product, which is a heat-resistant anti-vibration rubber.
架橋剤Ａ’，Ｂ’やその他の添加剤の配合量は特に制限はないが、ゴム成分Ａおよびゴム成分Ｂの配合量に対応する適切な量が配合されることが好ましい。 There are no particular restrictions on the amounts of crosslinking agents A' and B' and other additives, but it is preferable to use appropriate amounts that correspond to the amounts of rubber component A and rubber component B.
本実施形態において、ゴム成分Ａと架橋剤Ａ’およびその他任意の添加剤が混錬されたものを防振性ゴム組成物と呼び、ゴム成分Ｂと架橋剤Ｂ’およびその他任意の添加剤が混錬されたものを耐熱性ゴム組成物と呼ぶ。防振性ゴム組成物および耐熱性ゴム組成物は、ゴム成分と架橋剤とが未架橋の状態のものである。 In this embodiment, a mixture of rubber component A, crosslinking agent A', and any other additives is called an anti-vibration rubber composition, and a mixture of rubber component B, crosslinking agent B', and any other additives is called a heat-resistant rubber composition. The anti-vibration rubber composition and the heat-resistant rubber composition are in an uncrosslinked state between the rubber component and the crosslinking agent.
＜耐熱性防振ゴムの製造方法＞
図１に示すように、本実施形態に係る耐熱性防振ゴムは、防振性を有するゴム成分Ａおよびゴム成分Ａを架橋可能な架橋剤Ａ’を混錬し、防振性ゴム組成物を得る第１混錬工程（Ｓ１）と、耐熱性を有するゴム成分Ｂおよびゴム成分Ｂを架橋可能な架橋剤Ｂ’を混錬し、耐熱性ゴム組成物を得る第２混錬工程（Ｓ２）と、防振性ゴム組成物および耐熱性ゴム組成物を混錬し、ゴム混合物を得る第３混錬工程（Ｓ３）と、ゴム混合物の架橋を行う架橋成形工程（Ｓ４）と、を含む製造方法により製造される。
<Manufacturing method of heat-resistant anti-vibration rubber>
As shown in FIG. 1, the heat-resistant vibration-proof rubber of this embodiment is produced by a production method including a first kneading step (S1) of kneading a rubber component A having vibration-proof properties and a crosslinking agent A' capable of crosslinking rubber component A to obtain a vibration-proof rubber composition, a second kneading step (S2) of kneading a rubber component B having heat resistance and a crosslinking agent B' capable of crosslinking rubber component B to obtain a heat-resistant rubber composition, a third kneading step (S3) of kneading the vibration-proof rubber composition and the heat-resistant rubber composition to obtain a rubber mixture, and a crosslinking molding step (S4) of crosslinking the rubber mixture.
第１混錬工程（Ｓ１）と第２混錬工程（Ｓ２）と第３混錬工程（Ｓ３）は、ゴム材料を製造するために用いられる一般的な混錬方法を用いることが可能であり、例えば、混錬機として、バンバリーミキサー、ニーダー、ミキシングロール等が挙げられる。 The first kneading step (S1), the second kneading step (S2), and the third kneading step (S3) can be performed using a general kneading method used to manufacture rubber materials, and examples of kneading machines include a Banbury mixer, a kneader, and a mixing roll.
防振性を有するゴム成分Ａおよびゴム成分Ａを架橋可能な架橋剤Ａ’を混錬し、防振性ゴム組成物を得る第１混錬工程（Ｓ１）では、混錬時間は３～５０分が好ましい。３分より短い場合、ゴム成分Ａに対する架橋剤Ａ’の分散が不十分となり、最終生成物である耐熱性防振ゴムにおいて、防振性能が十分に発現しない。また、５０分を超えると生産性の観点から好ましくない。 In the first kneading step (S1) in which rubber component A having vibration-proof properties and crosslinking agent A' capable of crosslinking rubber component A are kneaded to obtain a vibration-proof rubber composition, the kneading time is preferably 3 to 50 minutes. If it is shorter than 3 minutes, the crosslinking agent A' is not sufficiently dispersed in rubber component A, and the final product, heat-resistant vibration-proof rubber, does not fully exhibit vibration-proofing properties. Moreover, if it exceeds 50 minutes, it is not preferable from the viewpoint of productivity.
耐熱性を有するゴム成分Ｂおよびゴム成分Ｂを架橋可能な架橋剤Ｂ’を混錬し、耐熱性ゴム組成物を得る第２混錬工程（Ｓ２）では、混錬時間は１～４０分が好ましい。１分より短い場合、ゴム成分Ｂに対する架橋剤Ｂ’の分散が不十分となり、最終生成物である耐熱性防振ゴムにおいて、耐熱性能が十分に発現しない。また、４０分を超えると生産性の観点から好ましくない。 In the second kneading step (S2) in which a heat-resistant rubber component B and a crosslinking agent B' capable of crosslinking rubber component B are kneaded to obtain a heat-resistant rubber composition, the kneading time is preferably 1 to 40 minutes. If it is shorter than 1 minute, the crosslinking agent B' is not sufficiently dispersed in the rubber component B, and the heat-resistant performance is not fully expressed in the final product, the heat-resistant vibration-proof rubber. Moreover, if it exceeds 40 minutes, it is not preferable from the viewpoint of productivity.
防振性ゴム組成物および耐熱性ゴム組成物を混錬し、ゴム混合物を得る第３混錬工程（Ｓ３）では、混錬時間は１～４０分が好ましい。１分より短い場合、防振性ゴム組成物および耐熱性ゴム組成物が偏って分布してしまうことにより、高い防振性および耐熱性を発現することができない。また、４０分を超えると生産性の観点から好ましくない。 In the third kneading step (S3) in which the anti-vibration rubber composition and the heat-resistant rubber composition are kneaded to obtain a rubber mixture, the kneading time is preferably 1 to 40 minutes. If it is shorter than 1 minute, the anti-vibration rubber composition and the heat-resistant rubber composition will be unevenly distributed, making it impossible to achieve high vibration-proofing and heat resistance. Furthermore, if it exceeds 40 minutes, it is not preferable from the viewpoint of productivity.
第１混錬工程（Ｓ１）、第２混錬工程（Ｓ２）および第３混錬工程（Ｓ３）の混錬時間の合計は、生産性の観点から６０分以内であることが好ましい。 From the viewpoint of productivity, it is preferable that the total mixing time of the first mixing step (S1), the second mixing step (S2) and the third mixing step (S3) is within 60 minutes.
第１混錬工程、第２混錬工程、および第３混錬工程は、６０℃以上１４０℃以下の排出温度で行われることが好ましい。排出温度が６０℃以上であれば、架橋剤がゴム成分内に十分に分散され、架橋反応が進み易く、最終生成物である耐熱性防振ゴムにおいてゴム成分Ａおよびゴム成分Ｂの特性を十分に発現させることができる。また、排出温度が１４０℃以下であれば、架橋成形工程の前に架橋反応が起こるのを防ぐことができる。 The first kneading step, the second kneading step, and the third kneading step are preferably performed at a discharge temperature of 60°C or more and 140°C or less. If the discharge temperature is 60°C or more, the crosslinking agent is sufficiently dispersed in the rubber component, the crosslinking reaction is easily promoted, and the properties of rubber component A and rubber component B can be fully expressed in the final product, the heat-resistant vibration-proof rubber. In addition, if the discharge temperature is 140°C or less, the crosslinking reaction can be prevented from occurring before the crosslinking molding step.
ゴム混合物の架橋を行う架橋成形工程（Ｓ４）では、ゴム混合物を金型に注入し、熱および圧力を加えることにより、製品形状にするとともに架橋反応を行う。この架橋成形工程（Ｓ４）は、一般的にゴム材料の架橋成形で用いられる方法を使用することが可能であり、加硫成形機として、例えば、圧縮成型機、射出成型機、トランスファー成形機、スチーム缶機、その他、赤外線やマイクロウェーブを用いるものを使用することができる。 In the crosslinking molding process (S4) where the rubber mixture is crosslinked, the rubber mixture is injected into a mold and heat and pressure are applied to form the product shape and to carry out the crosslinking reaction. This crosslinking molding process (S4) can use a method generally used in the crosslinking molding of rubber materials, and the vulcanization molding machine can be, for example, a compression molding machine, an injection molding machine, a transfer molding machine, a steam can machine, or other machines that use infrared rays or microwaves.
以下に実施例を挙げて本実施形態をさらに具体的に説明する。 The following examples will explain this embodiment in more detail.
＜実施例１～７および比較例１～７＞
下記表１および表２に示す質量部数の各成分を用いて、耐熱性防振ゴムを製造した。
<Examples 1 to 7 and Comparative Examples 1 to 7>
Heat-resistant anti-vibration rubber was produced using the components in the amounts by mass shown in Tables 1 and 2 below.
実施例１～７および比較例２～７では、ゴム成分Ａと架橋剤Ａ’、ゴム成分Ｂと架橋剤Ｂ’をそれぞれ「事前混錬」する本実施形態の製造方法によって製造した。この製造方法において、第１混錬工程（Ｓ１）は１００℃，７分間、第２混錬工程（Ｓ２）は１００℃，５分間、第３混錬工程（Ｓ３）は１００℃，５分間の条件で混錬した。また、１７０℃，１０分間の条件で架橋成形をおこなった。 In Examples 1 to 7 and Comparative Examples 2 to 7, the rubber components A and crosslinking agent A', and the rubber components B and crosslinking agent B' were each "pre-mixed" by the manufacturing method of this embodiment. In this manufacturing method, the first kneading step (S1) was performed at 100°C for 7 minutes, the second kneading step (S2) was performed at 100°C for 5 minutes, and the third kneading step (S3) was performed at 100°C for 5 minutes. In addition, crosslinking molding was performed at 170°C for 10 minutes.
比較例１は従来の「同時混錬」の製造方法によって製造した。比較例１では、まず防振性のゴム成分Ａと耐熱性のゴム成分Ｂとを１５０℃，７分間混錬し、その混合ゴム成分にフィラー等を加えて１４０℃，５分間さらに混錬し、最後に架橋剤Ａ’およびＢ’を添加して９０℃，３分間混錬した。また、１７０℃，１０分間の条件で架橋成形をおこなった。 Comparative Example 1 was produced using the conventional "simultaneous mixing" manufacturing method. In Comparative Example 1, vibration-proof rubber component A and heat-resistant rubber component B were first mixed at 150°C for 7 minutes, then fillers and other materials were added to the mixed rubber components and further mixed at 140°C for 5 minutes, and finally crosslinking agents A' and B' were added and mixed at 90°C for 3 minutes. Crosslinking molding was also performed at 170°C for 10 minutes.
＜評価方法＞
得られた耐熱性防振ゴムは以下の方法によりその特性を評価した。
<Evaluation method>
The properties of the heat-resistant vibration-isolating rubber thus obtained were evaluated by the following methods.
[防振性について]
製造した耐熱性防振ゴムについて、動的粘弾性測定装置（アイティー計測制御社製、ＤＶＡ－２００）を用い、引張モードで振動数１Ｈｚ及び１００Ｈｚ、振幅０．５％、温度２３℃の条件で、動倍率(１００Ｈｚの貯蔵弾性率/１Ｈｚの貯蔵弾性率)を測定した。表１および表２において便宜上、動倍率の逆数をとり、実施例１を基準値１００として、９０以上であれば防振性に優れると判断した。
[Vibration-proofing]
The heat-resistant vibration-proof rubber thus produced was measured for dynamic magnification (storage modulus at 100 Hz/storage modulus at 1 Hz) using a dynamic viscoelasticity measuring device (DVA-200, manufactured by IT Measurement & Control Co., Ltd.) in tension mode under conditions of frequencies of 1 Hz and 100 Hz, amplitude of 0.5%, and temperature of 23° C. In Tables 1 and 2, for the sake of convenience, the reciprocal of the dynamic magnification was taken, and Example 1 was set as the reference value of 100, and values of 90 or more were judged to be excellent in vibration-proofing.
[耐熱性について]
製造した耐熱性防振ゴムについて、ＪＩＳ Ｋ６２５７に準拠して、１００℃で２０００時間の熱処理前後の硬度を新東工業社製の硬度計を用いて測定した。熱処理前後の硬度の変化率について、実施例１を基準値１００として、９０～１１０の範囲内であれば耐熱性に優れると判断した。
[Heat resistance]
The hardness of the produced heat-resistant vibration-proof rubber was measured before and after heat treatment at 100°C for 2000 hours in accordance with JIS K6257 using a hardness tester manufactured by Shinto Kogyo Co., Ltd. The rate of change in hardness before and after heat treatment was determined to be excellent in heat resistance if it was within the range of 90 to 110, with Example 1 being set as the reference value of 100.
実施例１と比較例１によれば、同じ組成であるにも関わらず、混錬方法の違いにより、防振性および耐熱性のいずれにおいても実施例１が比較例１よりも優れていた。実施例１では、図２のように、ゴム成分Ａには対応する架橋剤Ａ’が分散されており、ゴム成分Ｂには対応する架橋剤Ｂ’分散しており、それぞれ架橋反応が進行しやすい分布になっていると推測される。比較例１では、図３のように、ゴム成分と対応する架橋剤とがランダムに分布していると推測され、このような分布が防振性および耐熱性がいずれも不十分となった原因であると考えられる。 According to Example 1 and Comparative Example 1, despite the same composition, Example 1 was superior to Comparative Example 1 in both vibration-proofing and heat resistance due to the difference in the kneading method. In Example 1, as shown in Figure 2, the corresponding crosslinking agent A' is dispersed in the rubber component A, and the corresponding crosslinking agent B' is dispersed in the rubber component B, and it is presumed that the distribution is such that the crosslinking reaction can easily proceed. In Comparative Example 1, as shown in Figure 3, it is presumed that the rubber component and the corresponding crosslinking agent are randomly distributed, and this distribution is thought to be the cause of the insufficient vibration-proofing and heat resistance.
ゴム成分Ａとして天然ゴム（ＮＲ）、ゴム成分Ｂとして二元系のエピクロロヒドリンゴム（ＥＣＯ）を用いた実施例１～３および比較例２，３では、ゴム成分Ａとゴム成分Ｂとの配合比率が３：７～７：３の範囲であるときに、防振性および耐熱性に優れ、特性バランスの取れた耐熱性防振ゴムが得られた。ゴム成分Ａとしてイソプレンゴム（ＩＲ）、ゴム成分Ｂとしてアクリルゴム（ＡＣＭ）を用いた場合（実施例４～６および比較例３，４）も同様に、ゴム成分Ａとゴム成分Ｂとの配合比率は３：７～７：３の範囲であるときに優れた結果が得られており、ゴム成分の種類に関わらず、防振性のゴム成分Ａと耐熱性のゴム成分Ｂとの組み合わせがこのような配合比率であれば、バランスの取れた高い防振性および耐熱性の耐熱性防振ゴムが得られると考えられる。 In Examples 1 to 3 and Comparative Examples 2 and 3, in which natural rubber (NR) was used as rubber component A and binary epichlorohydrin rubber (ECO) was used as rubber component B, heat-resistant vibration-proof rubber with excellent vibration-proofing and heat resistance and well-balanced properties was obtained when the compounding ratio of rubber component A to rubber component B was in the range of 3:7 to 7:3. Similarly, when isoprene rubber (IR) was used as rubber component A and acrylic rubber (ACM) was used as rubber component B (Examples 4 to 6 and Comparative Examples 3 and 4), excellent results were obtained when the compounding ratio of rubber component A to rubber component B was in the range of 3:7 to 7:3. It is believed that, regardless of the type of rubber component, if the combination of vibration-proof rubber component A and heat-resistant rubber component B is in such a compounding ratio, a heat-resistant vibration-proof rubber with balanced high vibration-proofing and heat resistance can be obtained.
また、実施例１～６ではゴム成分Ｂの架橋剤Ｂ’としてエチレンチオウレアを用いているが、異なる架橋剤（ジクミルパーオキサイド）を用いた実施例７においても優れた防振性および耐熱性が得られたため、架橋剤の種類は限定されないと考えられる。 In addition, in Examples 1 to 6, ethylene thiourea was used as the crosslinking agent B' for rubber component B, but excellent vibration-proofing and heat resistance were also obtained in Example 7, which used a different crosslinking agent (dicumyl peroxide), so it is believed that the type of crosslinking agent is not limited.
比較例６は、耐熱性のゴム成分Ｂに対応する架橋剤Ｂ’が含まれない組成であり、得られた耐熱性防振ゴムでは耐熱性が低下していた。また、比較例７は、防振性のゴム成分Ａに対応する架橋剤Ａ’が含まれない組成であり、得られた耐熱性防振ゴムでは防振性が低下していた。この結果から防振性のゴム成分Ａには対応する架橋剤Ａ’を、耐熱性のゴム成分Ｂには対応する架橋剤Ｂ’をそれぞれ配合する必要があると考えられる。 Comparative Example 6 is a composition that does not contain crosslinking agent B' corresponding to heat-resistant rubber component B, and the heat-resistant anti-vibration rubber obtained had reduced heat resistance. Comparative Example 7 is a composition that does not contain crosslinking agent A' corresponding to vibration-resistant rubber component A, and the heat-resistant anti-vibration rubber obtained had reduced vibration resistance. From these results, it is considered necessary to compound the corresponding crosslinking agent A' with the vibration-resistant rubber component A, and the corresponding crosslinking agent B' with the heat-resistant rubber component B.
＜実施例１における製造条件の検討＞
次に、各混錬工程における混錬時間と混錬温度の検討を行い、高い防振性および耐熱性を発現することが可能な製造条件を検討した。
<Study of manufacturing conditions in Example 1>
Next, the mixing time and temperature in each mixing step were examined to determine the manufacturing conditions that would enable the development of high vibration-proofing properties and heat resistance.
まず、実施例１の組成について検討した。第１混錬工程（Ｓ１）は１００℃，７分間、第２混錬工程（Ｓ２）は１００℃，５分間、第３混錬工程（Ｓ３）は１００℃，５分間の条件を検討１－１とし、この条件を基準として、混錬時間と混錬温度の検討をおこなった。なお、架橋成形はいずれの検討においても１７０℃，１０分間でおこなった。検討結果を表３に示す。 First, the composition of Example 1 was studied. The conditions for the first kneading step (S1) at 100°C for 7 minutes, the second kneading step (S2) at 100°C for 5 minutes, and the third kneading step (S3) at 100°C for 5 minutes were designated as Study 1-1, and the kneading time and temperature were studied based on these conditions. In addition, crosslinking molding was performed at 170°C for 10 minutes in all studies. The results of the study are shown in Table 3.
得られた耐熱性防振ゴムの防振性および耐熱性は上記の方法を用いて評価した。また、生産性についての評価は、第１混錬工程（Ｓ１）、第２混錬工程（Ｓ２）および第３混錬工程（Ｓ３）の合計の混錬時間が３０分以内であれば◎、６０分以内であれば〇、６０分を超える場合は×とした。防振性、耐熱性および生産性を合わせた判定は、防振性の判定値が９０より低い場合、耐熱性の判定値が９０～１１０の範囲外である場合、または、合計混錬時間が６０分を超える場合の少なくとも１つに該当すれば×とし、防振性、耐熱性および生産性の全てにおいて満足する結果が得られた検討条件を〇とした。 The vibration-proofing and heat resistance of the obtained heat-resistant vibration-proof rubber were evaluated using the above method. In addition, the evaluation of productivity was as follows: if the total kneading time of the first kneading step (S1), the second kneading step (S2), and the third kneading step (S3) was 30 minutes or less, it was rated as ◎; if it was 60 minutes or less, it was rated as 〇; if it exceeded 60 minutes, it was rated as ×. The combined evaluation of vibration-proofing, heat resistance, and productivity was rated as × if at least one of the following conditions was met: if the vibration-proofing evaluation value was lower than 90, if the heat resistance evaluation value was outside the range of 90 to 110, or if the total kneading time exceeded 60 minutes, the evaluation was rated as 〇 if the conditions under consideration gave satisfactory results in terms of vibration-proofing, heat resistance, and productivity.
検討１－２から１－５では、第１混錬工程（Ｓ１）の混錬時間を変えて検討した。第１混錬工程（Ｓ１）の混錬時間を２分間とした検討１－２では、防振性の評価において良い結果が得られなかった。第１混錬工程（Ｓ１）において、防振性のゴム成分Ａに対応する架橋剤Ａ’が十分に分散されなかったためであると考えられる。よって、第１混錬工程（Ｓ１）の混錬時間は、３分以上が好ましい。また、生産性の観点から５０分以内が好ましい。 In Studies 1-2 to 1-5, the kneading time of the first kneading step (S1) was changed. In Study 1-2, where the kneading time of the first kneading step (S1) was set to 2 minutes, good results were not obtained in the evaluation of vibration-proofing. This is thought to be because the crosslinking agent A', which corresponds to the vibration-proof rubber component A, was not sufficiently dispersed in the first kneading step (S1). Therefore, the kneading time of the first kneading step (S1) is preferably 3 minutes or more. Also, from the viewpoint of productivity, it is preferably 50 minutes or less.
検討１－６から１－９では、第２混錬工程（Ｓ２）の混錬時間を変えて検討した。第２混錬工程（Ｓ２）の混錬時間を０．５分とした検討１－６では、耐熱性の評価において良い結果が得られなかった。これは、第２混錬工程（Ｓ２）において、耐熱性のゴム成分Ｂに対応する架橋剤Ｂ’が十分に分散されなかったためであると考えられる。このような検討１－６の製造条件では、ゴム成分と架橋剤は図４のように分布していると推測される。第２混錬工程（Ｓ２）の混錬時間は１分以上が好ましく、また、生産性の観点から４０分以内が好ましい。 In Studies 1-6 to 1-9, the kneading time of the second kneading step (S2) was changed. In Study 1-6, where the kneading time of the second kneading step (S2) was set to 0.5 minutes, good results were not obtained in the evaluation of heat resistance. This is thought to be because the crosslinking agent B' corresponding to the heat-resistant rubber component B was not sufficiently dispersed in the second kneading step (S2). Under the manufacturing conditions of Study 1-6, it is presumed that the rubber component and the crosslinking agent are distributed as shown in Figure 4. The kneading time of the second kneading step (S2) is preferably 1 minute or more, and from the viewpoint of productivity, it is preferably 40 minutes or less.
検討１－１０から１－１３では、第３混錬工程（Ｓ３）の混錬時間を変えて検討した。第３混錬工程（Ｓ３）の混錬時間を０．５分とした検討１－１０では、防振性および耐熱性の評価において良い結果が得られなかった。これは、第３混錬工程（Ｓ３）において、防振性ゴム組成物と耐熱性ゴム組成物とが十分に分散されなかったためであると考えられる。このような検討１－１０の製造条件では、ゴム成分は図５のように分布していると推測される。第３混錬工程（Ｓ３）の混錬時間は１分以上が好ましく、また、生産性の観点から４０分以内が好ましい。 In Studies 1-10 to 1-13, the kneading time of the third kneading step (S3) was changed. In Study 1-10, in which the kneading time of the third kneading step (S3) was set to 0.5 minutes, good results were not obtained in the evaluation of vibration-proofing and heat resistance. This is thought to be because the vibration-proof rubber composition and the heat-resistant rubber composition were not sufficiently dispersed in the third kneading step (S3). Under the manufacturing conditions of Study 1-10, it is presumed that the rubber components are distributed as shown in Figure 5. The kneading time of the third kneading step (S3) is preferably 1 minute or more, and from the viewpoint of productivity, it is preferably 40 minutes or less.
検討１－１４および１－１５では、第１混錬工程（Ｓ１）、第２混錬工程（Ｓ２）および第３混錬工程（Ｓ３）の合計の混錬時間を変えて検討した。各混錬工程を最低限の混錬時間とし、合計時間を５分間とした検討１－１４では、防振性、耐熱性および生産性に優れた結果であった。各混錬工程を上限の混錬時間とし、混錬の合計時間を１３０分間とした検討１－１５では、防振性および耐熱性は高いが生産性が悪いため×とした。 In Studies 1-14 and 1-15, the total kneading time for the first kneading step (S1), the second kneading step (S2), and the third kneading step (S3) was changed and examined. In Study 1-14, in which each kneading step was set to the minimum kneading time and the total time was set to 5 minutes, the results were excellent in terms of vibration-proofing, heat resistance, and productivity. In Study 1-15, in which each kneading step was set to the maximum kneading time and the total kneading time was set to 130 minutes, the vibration-proofing and heat resistance were high but the productivity was poor, so it was rated as x.
検討１－１６から１－１９では、第１混錬工程（Ｓ１）、第２混錬工程（Ｓ２）および第３混錬工程（Ｓ３）における各排出温度を変えて検討した。排出温度を５０℃とした検討１－１６では、防振性および耐熱性が低かった。５０℃では、架橋剤がゴム成分へ十分に分散されないと考えられる。排出温度を１５０℃とした検討１－１９では、混錬中にスコーチが発生してしまうため、耐熱性防振ゴムを製造することができなかった。よって、第１混錬工程、第２混錬工程、および第３混錬工程は、６０℃以上１４０℃以下の排出温度で行われることが好ましい。 In Studies 1-16 to 1-19, the discharge temperatures in the first kneading step (S1), the second kneading step (S2), and the third kneading step (S3) were changed. In Study 1-16, where the discharge temperature was 50°C, the vibration-proofing and heat resistance were low. It is believed that at 50°C, the crosslinking agent is not sufficiently dispersed in the rubber components. In Study 1-19, where the discharge temperature was 150°C, scorching occurred during kneading, so it was not possible to produce heat-resistant vibration-proof rubber. Therefore, it is preferable that the first kneading step, the second kneading step, and the third kneading step are performed at a discharge temperature of 60°C or higher and 140°C or lower.
検討１－２０から１－２３では、第１混錬工程（Ｓ１）、第２混錬工程（Ｓ２）および第３混錬工程（Ｓ３）における各排出温度と混錬の合計時間を検討した。排出温度が１４０℃の場合であって、合計混錬時間が５分のとき（検討１－２２）は、防振性、耐熱性および生産性に優れた結果であったが、合計混錬時間が１３０分の場合は、混錬中にスコーチが発生してしまうため、耐熱性防振ゴムを製造することができなかった。よって、優れた防振性および耐熱性を備え、高い生産性で耐熱性防振ゴムを得るには、排出温度および混錬時間を最適な範囲で製造することが好ましい。 In Studies 1-20 to 1-23, the discharge temperatures and total kneading times in the first kneading step (S1), the second kneading step (S2), and the third kneading step (S3) were examined. When the discharge temperature was 140°C and the total kneading time was 5 minutes (Study 1-22), the results were excellent in vibration-proofing, heat resistance, and productivity, but when the total kneading time was 130 minutes, scorching occurred during kneading, making it impossible to produce heat-resistant vibration-proof rubber. Therefore, in order to obtain heat-resistant vibration-proof rubber with excellent vibration-proofing and heat resistance and high productivity, it is preferable to produce it with the discharge temperature and kneading time in the optimal range.
＜実施例４における製造条件の検討＞
次に、防振性のゴム成分Ａの配合割合が耐熱性のゴム成分Ａよりも高い実施例４の組成においても製造条件を検討した。第１混錬工程（Ｓ１）は１００℃，７分間、第２混錬工程（Ｓ２）は１００℃，５分間、第３混錬工程（Ｓ３）は１００℃，５分間の条件を検討４－１とし、この条件を基準として、上記検討１－１から１－２３と同様の条件検討をおこない、検討４－１から４－２３の検討結果を得た。結果を表４に示す。
<Study of manufacturing conditions in Example 4>
Next, the manufacturing conditions were also examined for the composition of Example 4, in which the blending ratio of the vibration-proof rubber component A was higher than that of the heat-resistant rubber component A. The conditions of the first kneading step (S1) at 100°C for 7 minutes, the second kneading step (S2) at 100°C for 5 minutes, and the third kneading step (S3) at 100°C for 5 minutes were designated as Study 4-1, and based on these conditions, the same condition studies as those of Studies 1-1 to 1-23 above were conducted, and the results of Studies 4-1 to 4-23 were obtained. The results are shown in Table 4.
＜実施例５における製造条件の検討＞
次に、防振性のゴム成分Ａの配合割合が耐熱性のゴム成分Ａよりも低い実施例４の組成においても、製造条件を検討した。第１混錬工程（Ｓ１）は１００℃，７分間、第２混錬工程（Ｓ２）は１００℃，５分間、第３混錬工程（Ｓ３）は１００℃，５分間の条件を検討５－１とし、この条件を基準として、上記検討１－１から１－２３と同様の条件検討をおこない、検討５－１から５－２３の検討結果を得た。結果を表４に示す。
<Study of manufacturing conditions in Example 5>
Next, the manufacturing conditions were also examined for the composition of Example 4, in which the blending ratio of the vibration-proof rubber component A was lower than that of the heat-resistant rubber component A. The conditions of the first kneading step (S1) at 100°C for 7 minutes, the second kneading step (S2) at 100°C for 5 minutes, and the third kneading step (S3) at 100°C for 5 minutes were designated as Study 5-1, and based on these conditions, the same condition studies as those of Studies 1-1 to 1-23 above were conducted, and the results of Studies 5-1 to 5-23 were obtained. The results are shown in Table 4.
検討４－２から４－２３の結果および検討５－２から５－２３の結果は、検討１－１から１－２３の結果とほぼ同様であった。よって、実施例１の組成における製造条件が、ゴム成分の配合比率の異なる組成において適用可能であると考えられる。 The results of Studies 4-2 to 4-23 and Studies 5-2 to 5-23 were almost the same as those of Studies 1-1 to 1-23. Therefore, it is considered that the manufacturing conditions for the composition of Example 1 can be applied to compositions with different rubber component compounding ratios.
Claims (5)
耐熱性を有するゴム成分Ｂおよび該ゴム成分Ｂを架橋可能な架橋剤Ｂ’を混錬し、耐熱性ゴム組成物を得る第２混錬工程と、
前記防振性ゴム組成物および前記耐熱性ゴム組成物を混錬し、ゴム混合物を得る第３混錬工程と、
前記ゴム混合物の架橋を行う架橋成形工程と、を含むことを特徴とする耐熱性防振ゴムの製造方法。 a first kneading step of kneading a rubber component A having vibration-proof properties and a crosslinking agent A' capable of crosslinking the rubber component A to obtain a vibration-proof rubber composition;
a second kneading step of kneading a heat-resistant rubber component B and a crosslinking agent B' capable of crosslinking the rubber component B to obtain a heat-resistant rubber composition;
a third kneading step of kneading the vibration-proof rubber composition and the heat-resistant rubber composition to obtain a rubber mixture;
and a crosslinking molding step of crosslinking the rubber mixture.
前記ゴム成分Ｂが、エピクロロヒドリンゴム、アクリルゴム、フッ素ゴムからなる群より選択される少なくとも１種であることを特徴とする請求項１または２に記載の耐熱性防振ゴムの製造方法。 The rubber component A is a diene rubber,
3. The method for producing a heat-resistant vibration-proof rubber according to claim 1, wherein the rubber component B is at least one selected from the group consisting of epichlorohydrin rubber, acrylic rubber, and fluororubber.
前記第２混錬工程における混錬時間は１分以上であり、
前記第３混錬工程における混錬時間は１分以上であり、
前記第１混錬工程、前記第２混錬工程および前記第３混錬工程の混錬時間の合計は６０分以内であることを特徴とする請求項１から４のいずれか１項に記載の耐熱性防振ゴムの製造方法。 The kneading time in the first kneading step is 3 minutes or more,
The kneading time in the second kneading step is 1 minute or more,
The kneading time in the third kneading step is 1 minute or more,
5. The method for producing a heat-resistant vibration-proof rubber according to claim 1, wherein a total kneading time for the first kneading step, the second kneading step, and the third kneading step is within 60 minutes.
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