JP2019189838A - アクリルゴムの製造方法、ならびに、その製造方法により得られるアクリルゴム、ゴム組成物、及びゴム架橋物 - Google Patents
アクリルゴムの製造方法、ならびに、その製造方法により得られるアクリルゴム、ゴム組成物、及びゴム架橋物 Download PDFInfo
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- JP2019189838A JP2019189838A JP2018087820A JP2018087820A JP2019189838A JP 2019189838 A JP2019189838 A JP 2019189838A JP 2018087820 A JP2018087820 A JP 2018087820A JP 2018087820 A JP2018087820 A JP 2018087820A JP 2019189838 A JP2019189838 A JP 2019189838A
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- acrylic rubber
- rubber
- emulsion polymerization
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- acrylic
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 48
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- 239000005060 rubber Substances 0.000 title claims description 89
- 239000000203 mixture Substances 0.000 title claims description 52
- 238000000034 method Methods 0.000 title abstract description 30
- 230000008569 process Effects 0.000 title abstract description 5
- 239000000178 monomer Substances 0.000 claims abstract description 119
- 238000007720 emulsion polymerization reaction Methods 0.000 claims abstract description 86
- 229920000642 polymer Polymers 0.000 claims abstract description 68
- 238000005406 washing Methods 0.000 claims abstract description 44
- 229910052751 metal Inorganic materials 0.000 claims abstract description 33
- 239000002184 metal Substances 0.000 claims abstract description 33
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- 238000001035 drying Methods 0.000 claims abstract description 28
- 239000007788 liquid Substances 0.000 claims abstract description 28
- 125000002947 alkylene group Chemical group 0.000 claims abstract description 25
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- 238000012360 testing method Methods 0.000 description 11
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- 239000012875 nonionic emulsifier Substances 0.000 description 10
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- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 description 9
- 239000012874 anionic emulsifier Substances 0.000 description 9
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 9
- 125000003700 epoxy group Chemical group 0.000 description 9
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 9
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- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 7
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 7
- 150000002148 esters Chemical class 0.000 description 7
- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 description 7
- 229910052938 sodium sulfate Inorganic materials 0.000 description 7
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- 238000003756 stirring Methods 0.000 description 7
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- 125000005843 halogen group Chemical group 0.000 description 6
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 description 6
- 239000003921 oil Substances 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 5
- 125000005907 alkyl ester group Chemical group 0.000 description 5
- 238000007654 immersion Methods 0.000 description 5
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 5
- 235000019341 magnesium sulphate Nutrition 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
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- 229920005989 resin Polymers 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- GAODDBNJCKQQDY-UHFFFAOYSA-N 2-methyl-4,6-bis(octylsulfanylmethyl)phenol Chemical compound CCCCCCCCSCC1=CC(C)=C(O)C(CSCCCCCCCC)=C1 GAODDBNJCKQQDY-UHFFFAOYSA-N 0.000 description 4
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 4
- CHJJGSNFBQVOTG-UHFFFAOYSA-N N-methyl-guanidine Natural products CNC(N)=N CHJJGSNFBQVOTG-UHFFFAOYSA-N 0.000 description 4
- 150000001412 amines Chemical class 0.000 description 4
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 4
- DKVNPHBNOWQYFE-UHFFFAOYSA-N carbamodithioic acid Chemical compound NC(S)=S DKVNPHBNOWQYFE-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 150000001990 dicarboxylic acid derivatives Chemical class 0.000 description 4
- SWSQBOPZIKWTGO-UHFFFAOYSA-N dimethylaminoamidine Natural products CN(C)C(N)=N SWSQBOPZIKWTGO-UHFFFAOYSA-N 0.000 description 4
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- 229910052717 sulfur Inorganic materials 0.000 description 4
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- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 description 1
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- OAHWWXAJFXEIPX-UHFFFAOYSA-M tributyl(octadecyl)azanium;bromide Chemical compound [Br-].CCCCCCCCCCCCCCCCCC[N+](CCCC)(CCCC)CCCC OAHWWXAJFXEIPX-UHFFFAOYSA-M 0.000 description 1
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 description 1
- ABVVEAHYODGCLZ-UHFFFAOYSA-N tridecan-1-amine Chemical compound CCCCCCCCCCCCCN ABVVEAHYODGCLZ-UHFFFAOYSA-N 0.000 description 1
- SWZDQOUHBYYPJD-UHFFFAOYSA-N tridodecylamine Chemical compound CCCCCCCCCCCCN(CCCCCCCCCCCC)CCCCCCCCCCCC SWZDQOUHBYYPJD-UHFFFAOYSA-N 0.000 description 1
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 description 1
- FBBATURSCRIBHN-UHFFFAOYSA-N triethoxy-[3-(3-triethoxysilylpropyldisulfanyl)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCSSCCC[Si](OCC)(OCC)OCC FBBATURSCRIBHN-UHFFFAOYSA-N 0.000 description 1
- VTHOKNTVYKTUPI-UHFFFAOYSA-N triethoxy-[3-(3-triethoxysilylpropyltetrasulfanyl)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCSSSSCCC[Si](OCC)(OCC)OCC VTHOKNTVYKTUPI-UHFFFAOYSA-N 0.000 description 1
- KLFNHRIZTXWZHT-UHFFFAOYSA-N triethoxy-[3-(3-triethoxysilylpropyltrisulfanyl)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCSSSCCC[Si](OCC)(OCC)OCC KLFNHRIZTXWZHT-UHFFFAOYSA-N 0.000 description 1
- RKBCYCFRFCNLTO-UHFFFAOYSA-N triisopropylamine Chemical compound CC(C)N(C(C)C)C(C)C RKBCYCFRFCNLTO-UHFFFAOYSA-N 0.000 description 1
- QPPXVBLDIDEHBA-UHFFFAOYSA-N trimethoxy(3-nitropropyl)silane Chemical compound CO[Si](OC)(OC)CCC[N+]([O-])=O QPPXVBLDIDEHBA-UHFFFAOYSA-N 0.000 description 1
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
- YQMWDQQWGKVOSQ-UHFFFAOYSA-N trinitrooxystannyl nitrate Chemical compound [Sn+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YQMWDQQWGKVOSQ-UHFFFAOYSA-N 0.000 description 1
- YFTHZRPMJXBUME-UHFFFAOYSA-N tripropylamine Chemical compound CCCN(CCC)CCC YFTHZRPMJXBUME-UHFFFAOYSA-N 0.000 description 1
- WXAZIUYTQHYBFW-UHFFFAOYSA-N tris(4-methylphenyl)phosphane Chemical compound C1=CC(C)=CC=C1P(C=1C=CC(C)=CC=1)C1=CC=C(C)C=C1 WXAZIUYTQHYBFW-UHFFFAOYSA-N 0.000 description 1
- NCPXQVVMIXIKTN-UHFFFAOYSA-N trisodium;phosphite Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])[O-] NCPXQVVMIXIKTN-UHFFFAOYSA-N 0.000 description 1
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 235000014692 zinc oxide Nutrition 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- NEYNBSGIXOOZGZ-UHFFFAOYSA-L zinc;butoxymethanedithioate Chemical compound [Zn+2].CCCCOC([S-])=S.CCCCOC([S-])=S NEYNBSGIXOOZGZ-UHFFFAOYSA-L 0.000 description 1
- VSWBCXJHSLMWFY-UHFFFAOYSA-L zinc;n,n-dihexylcarbamodithioate Chemical compound [Zn+2].CCCCCCN(C([S-])=S)CCCCCC.CCCCCCN(C([S-])=S)CCCCCC VSWBCXJHSLMWFY-UHFFFAOYSA-L 0.000 description 1
- JGSUMMPGKPITGK-UHFFFAOYSA-L zinc;n,n-dipentylcarbamodithioate Chemical compound [Zn+2].CCCCCN(C([S-])=S)CCCCC.CCCCCN(C([S-])=S)CCCCC JGSUMMPGKPITGK-UHFFFAOYSA-L 0.000 description 1
- KMNUDJAXRXUZQS-UHFFFAOYSA-L zinc;n-ethyl-n-phenylcarbamodithioate Chemical compound [Zn+2].CCN(C([S-])=S)C1=CC=CC=C1.CCN(C([S-])=S)C1=CC=CC=C1 KMNUDJAXRXUZQS-UHFFFAOYSA-L 0.000 description 1
- SZNCKQHFYDCMLZ-UHFFFAOYSA-L zinc;propan-2-yloxymethanedithioate Chemical compound [Zn+2].CC(C)OC([S-])=S.CC(C)OC([S-])=S SZNCKQHFYDCMLZ-UHFFFAOYSA-L 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
Description
本発明者らは、更に、本発明のアクリルゴムと架橋剤を含むゴム組成物において、特定の配合剤を配合することにより、貯蔵安定性、ならびに、架橋した時の耐水性及び耐圧縮永久歪み性が高度に高められることを見出した。
本発明者らは、これらの知見に基づき本発明を完成するに至ったものである。
本発明のアクリルゴムの製造方法において、前記重合開始剤が、過酸化物と、硫酸第一鉄と、アスコルビン酸及び/またはアスコルビン酸塩との組み合わせであることが好ましい。
本発明のアクリルゴムの製造方法において、乳化重合前の単量体乳化液中及び/または乳化重合後の前記乳化重合液中に、前記アルキレンオキシド重合体を添加することで、凝固時に、前記乳化重合液中に、前記アルキレンオキシド重合体を存在させることが好ましい。
本発明のアクリルゴムの製造方法において、前記アルキレンオキシド重合体の重量平均分子量(Mw)が、10,000〜6,000,000の範囲であることが好ましい。
本発明のアクリルゴムの製造方法において、前記乳化重合液と前記金属硫酸塩との接触が、前記乳化重合液に前記金属硫酸塩を添加するか、前記乳化重合液を前記金属硫酸の溶液または分散液に投入するかいずれかの方法であることが好ましい。
本発明のアクリルゴムの製造方法において、前記洗浄工程の洗浄が、酸洗浄を含むものであることが好ましい。
本発明のアクリルゴムにおいて、単量体組成が、(メタ)アクリル酸エステル単量体単位50〜99.9重量%、架橋性単量体単位0.01〜20重量%及び共重合可能な他の単量体単位0〜50重量%であることが好ましい。
本発明のアクリルゴムにおいて、前記架橋性単量体単位が、カルボキシル基含有単量体単位であることが好ましい。
本発明のアクリルゴムにおいて、ムーニー粘度(ML1+4、100℃)が、10〜150の範囲であることが好ましい。
本発明のゴム組成物において、更に、架橋促進剤、充填剤及びシランカップリングとからなる群から選ばれる少なくとも1種の配合剤を配合してなることが好ましい。
また、本発明によれば、上記ゴム組成物を架橋してなるゴム架橋物が提供される。
本発明のアクリルゴムの製造方法は、(メタ)アクリル酸エステルを主成分とする単量体を乳化剤の存在下に重合触媒を用いて乳化重合し乳化重合液を得る乳化重合工程と、前記乳化重合液をアルキレンオキシド重合体の存在下で金属硫酸塩と接触させて凝固し含水クラムを得る凝固工程と、前記含水クラムに対して洗浄する洗浄工程と、洗浄した前記含水クラムを乾燥する乾燥工程と備えることを特徴とする。
本発明で使用される単量体は、(メタ)アクリル酸エステルを主成分とすることが特徴である。主成分である(メタ)アクリル酸エステルとしては、格別な限定はなく、例えば(メタ)アクリル酸アルキルエステル、(メタ)アクリル酸アルコキシアルキルエステルなどを挙げることができる。
本発明の製造方法における乳化重合工程は、上記(メタ)アクリレートを主成分とする単量体を乳化剤の存在下に重合触媒を用いて乳化重合し乳化重合液を得ることを特徴とする。
ノニオン性乳化剤としては、特に限定されず、例えば、ポリオキシエチレンドデシルエーテルなどのポリオキシアルキレンアルキルエーテル;ポリオキシエチレンノニルフェニルエーテルなどのポリオキシアルキレンアルキルフェニルエーテル;ポリオキシエチレンステアリン酸エステルなどのポリオキシアルキレン脂肪酸エステル;ポリオキシエチレンソルビタンアルキルエステル;ポリオキシエチレン/ポリプロピレンオキシド共重合体などのオキシアルキレンの共重合体;などを挙げることができる。これらの中でも、ポリオキシアルキレンアルキルエーテル、ポリオキシアルキレンアルキルフェニルエーテルなどが好ましく、特にポリオキシエチレンアルキルエーテル、ポリオキシエチレンアルキルフェニルエーテルが好ましい。ノニオン性乳化剤の重量平均分子量は、格別な限定はないが、通常300〜50,000、好ましくは500〜30,000、より好ましくは1,000〜15,000の範囲である。これらのノニオン性乳化剤は、それぞれ単独で、あるいは2種以上を組み合わせて用いることができる。
本発明の製造方法における乳化重合工程においては、乳化重合により得られた、凝固前の乳化重合液に必要に応じて各種配合剤を添加し、生成するアクリルゴム重合体中に均一分散することができる。添加する配合剤としては、ゴム用配合剤であれば格別な限定はないが、例えば、老化防止剤が好適なものとして挙げられる。
本発明の製造方法における凝固工程は、上記乳化重合液をアルキレンオキシド重合体存在下で金属硫酸塩と接触させて凝固し含水クラムを得ることを特徴とする。
本発明の製造方法における洗浄工程は、上記凝固工程において得られた含水クラムに対して洗浄を行うものである。
本発明の乾燥工程は、上記洗浄工程において洗浄を行った含水クラムに対し乾燥を行うものである。
本発明によれば、上記製造方法により、本発明のアクリルゴムを得ることができる。
かくして得られる本発明のアクリルゴムは、製造時に釜汚れが発生せず、高いポリマー回収率にて製造することができることに加え、貯蔵安定性に優れるものであり、さらには、ゴム架橋物にしたときの耐水性及び耐圧縮永久歪み性に優れるものである。
特に、上記製造方法により得られる、本発明のアクリルゴムによれば、製造時に釜汚れが発生せず、高いポリマー回収率にて製造することができ、しかも、貯蔵安定性に優れ、架橋した時の耐水性及び耐圧縮永久歪み性に優れるものである。ここで、アクリルゴムなどのゴムの分野においては、重合により得られたゴムの溶液あるいは分散液から、固形状のゴムを得る際に凝固を行うのが通常であり、本発明者等の知見によると、凝固時の状態により、得られるアクリルゴムの特性が大きく変化するものである。
本発明のゴム組成物は、上記アクリルゴムを含むゴム成分と架橋剤とを含むことを特徴とする。ゴム成分中における、本発明のアクリルゴムの含有量は、使用目的に応じて選択されればよく、例えば、通常30重量%以上、好ましくは50重量%以上、より好ましくは70重量%以上であり、特に好ましくは100重量%である。
その他のゴムとしては、本発明のアクリルゴム以外のアクリルゴム、天然ゴム、ポリブタジエンゴム、ポリイソプレンゴム、スチレン−ブタジエンゴム、アクリロニトリル−ブタジエンゴム、シリコンゴム、フッ素ゴム、オレフィン系エラストマー、スチレン系エラストマー、塩化ビニル系エラストマー、ポリエステル系エラストマー、ポリアミド系エラストマー、ポリウレタン系エラストマー、ポリシロキサン系エラストマーなどを挙げることができる。
これらの老化防止剤は、それぞれ単独で、あるいは2種以上を組み合わせて用いることができる。なお、上述したように、老化防止剤は、凝固を行う前の乳化重合液に予め含有させておくことができる。
本発明のゴム架橋物は、上記ゴム組成物を架橋してなるものである。
本発明のゴム架橋物は、本発明のアゴム組成物を用い、所望の形状に対応した成形機、たとえば、押出機、射出成形機、圧縮機、およびロールなどにより成形を行い、加熱することにより架橋反応を行い、ゴム架橋物として形状を固定化することにより製造することができる。この場合においては、予め成形した後に架橋しても、成形と同時に架橋を行ってもよい。成形温度は、通常10〜200℃、好ましくは25〜150℃である。架橋温度は、通常100〜250℃、好ましくは130〜220℃、より好ましくは150〜200℃であり、架橋時間は、通常0.1分〜10時間、好ましくは1分〜5時間である。加熱方法としては、プレス加熱、蒸気加熱、オーブン加熱、および熱風加熱などのゴムの架橋に用いられる方法を適宜選択すればよい。
各種の物性及び特性については、以下の方法に従って評価した。
アクリルゴムのムーニー粘度(ポリマームーニー)をJIS K6300に従って測定した。
重合後の乳化重合液中のゴム固形分に対する、重合により得られた乾燥後の固形状のアクリルゴムの重量の比率を求め、以下の基準で評価した。
◎:100%
○:95%超、100%未満
△:90%超、95%以下
×:70%超、90%以下
××:70%以下
釜汚れは、凝固後の凝固槽を観察し、下記の基準で判断した。
◎:凝固槽および撹拌翼に汚れが無い
○:凝固槽および撹拌翼わずかに汚れが見られる
×:槽全体に白色の付着物がついている
××:槽全体に厚い白色の付着物があり、洗浄も困難
ゴム組成物を、縦15cm、横15cm、深さ0.2cmの金型に入れ、プレス圧10MPaで加圧しながら170℃で20分間プレスすることにより一次架橋し、次いで、得られた一次架橋物を、ギヤー式オーブンにて、さらに170℃、4時間の条件で加熱して二次架橋させることにより、シート状のゴム架橋物を得た。そして、得られたシート状のゴム架橋物から、3cm×2cm×0.2cmの試験片に切り取り、JIS K6258に準拠して、得られた試験片を温度80℃に調整した蒸留水中に70時間浸漬させる浸漬試験を行い、浸漬前後の試験片の体積変化率を下記式にしたがって、測定した。浸漬前後の体積変化率が小さいほど、水に対する膨潤が抑制されており、耐水性に優れると判断できる。
浸漬前後の体積変化率(%)=(浸漬後の試験片の体積−浸漬前の試験片の体積)÷浸漬前の試験片の体積×100
ゴム組成物を、金型を用いて、温度170℃で20分間プレスすることにより一次架橋し、直径29mm、高さ12.7mmの円柱型の一次架橋物を得て、次いで、得られた一次架橋物を、ギヤー式オーブンにて、さらに170℃、4時間の条件で加熱して二次架橋させることにより、円柱状のゴム架橋物を得た。そして、得られたゴム架橋物を用いて、JIS K6262に従い、ゴム架橋物を25%圧縮させた状態で、175℃の環境下に70時間置いた後、圧縮永久歪み率を測定した。この値が小さいほど、耐圧縮永久歪み性に優れる。
アクリルゴム組成物について、JIS K6300に従い、125℃の測定条件下でムーニースコーチの測定を行い、ムーニースコーチ時間t5(分)、ムーニースコーチ時間t35(分)、およびムーニー粘度(ML1+4、100℃)の最低値Vminを測定した。本測定においては、ムーニー粘度が、Vminから5M上昇した時間をt5とし、ムーニー粘度が、Vminから35M上昇した時間をt35とした。t5及びt35は値が大きいほど加硫にかかる時間がかかることを意味し、ゴム組成物の貯蔵安定性に優れ、加硫促進効果が抑えられている(良好に制御されている)と判断できる。Vminは値が低いほどゴム組成物の初期加硫が少ないことを意味し、貯蔵安定性に優れると判断できる。
ホモミキサーを備えた混合容器に、純水46.294部、アクリル酸エチル49.3部、アクリル酸n−ブチル49.3部、フマル酸モノn−ブチル1.4部、アニオン性乳化剤としてのラウリル硫酸ナトリウム(商品名「エマール 2FG」、花王社製)0.567部、およびノニオン性乳化剤としてのポリオキシエチレンドデシルエーテル(商品名「エマルゲン 105」、重量平均分子量:約1500、花王社製)1.4部を仕込み、攪拌することで、単量体乳化液を得た。
得られたゴム組成物を用いて、耐水性を測定し、それらの結果を表1に示した。
凝固剤としての硫酸ナトリウム3.3部を硫酸マグネシウム3.3部に変更した以外は、実施例1と同様にして、固形状のアクリルゴム(A2)を得た。
老化防止剤としての3−(3,5−ジ−tert−ブチル−4−ヒドロキシフェニル)プロピオン酸ステアリル0.3部を2,4−ビス[(オクチルチオ)メチル]−6−メチルフェノール(商品名「Irganox 1520L」、BASF社製)0.3部に変更した以外は、実施例1と同様にして、固形状のアクリルゴム(A3)を得た。
水洗回数を4回から2回に変更した以外は、実施例3と同様にして、固形状のアクリルゴム(A4)を得た。
水洗回数を4回から1回に変更した以外は、実施例3と同様にして、固形状のアクリルゴム(A5)を得た。
エチレンオキシド重合体の添加タイミングを、単量体乳化液を調製するタイミングに変更するとともに、エチレンオキシド重合体の添加量を乳化重合液を製造する際に用いた仕込みの単量体の合計100部に対して0.039部とした以外は、実施例1と同様にして、固形状のアクリルゴム(A6)を得た。
凝固操作を行う際に用いるエチレンオキシド重合体0.011部を使用しない以外は、実施例3と同様にして、固形状のアクリルゴム(B1)を得た。
アニオン性界面活性剤としてのラウリル硫酸ナトリウムの使用量を0.567部から0.709部に、ノニオン性界面活性剤としてのポリオキシエチレンドデシルエーテルの使用量を1.4部から1.82部に、それぞれ変更した以外は、比較例1と同様にして、固形状のアクリルゴム(B2)を得た。
水洗回数を4回から1回に変更した以外は、比較例2と同様にして、固形状のアクリルゴム(B3)を得た。
凝固操作を行う際に用いる凝固剤としての硫酸ナトリウムの使用量を3.3部から10部に変更した以外は、比較例1と同様にして、固形状のアクリルゴム(B4)を得た。
水洗回数を4回から1回に変更した以外は、比較例4と同様にして、固形状のアクリルゴム(B5)を得た。
(※2)老化防止剤2は、2,4−ビス[(オクチルチオ)メチル]−6−メチルフェノール
(※3)ポリエチレンオキシド重合体は、ポリエチレングリコール
(※A)単量体乳化液作製のための配合剤の添加量は、仕込み単量体100部に対する配合量で示した。
(※B)凝固前の乳化重合液に添加した配合剤の添加量は、乳化重合液100部に対する配合量で示した。
(※C)凝固工程で使用した凝固剤の添加量は、乳化重合液に、老化防止剤、ポリエチレンオキシド、および/または滑剤を添加することにより得られた混合液100部に対する配合量で示した。
表1より、初期の洗浄回数を4回(実施例3)、2回(実施例4)、1回(実施例5)では、前記比較例(比較例2と比較例3、比較例4と比較例5)と同様に洗浄回数による耐水性への影響があるが、実施例3〜5の方が比較例2〜5よりもその影響は小さいことがわかる。これは、実施例ではエチレンオキシド重合体による耐水性改善効果が洗浄前にもあることによると思われる。
実施例1〜6で得られたゴム組成物を用いて、圧縮永久歪み試験、及びムーニースコーチ試験を行い、それらの結果を表2に示した。
Claims (13)
- (メタ)アクリル酸エステルを主成分とする単量体を乳化剤の存在下に重合触媒を用いて乳化重合し乳化重合液を得る乳化重合工程と、
前記乳化重合液をアルキレンオキシド重合体の存在下で金属硫酸塩と接触させ凝固し含水クラムを得る凝固工程と、
前記含水クラムに対して洗浄する洗浄工程と、
洗浄した前記含水クラムを乾燥する乾燥工程と、
を備えるアクリルゴムの製造方法。 - 前記重合開始剤が、過酸化物と、硫酸第一鉄と、アスコルビン酸及び/またはアスコルビン酸塩との組み合わせである請求項1記載のアクリルゴムの製造方法。
- 乳化重合前の単量体乳化液中及び/または乳化重合後の前記乳化重合液中に、前記アルキレンオキシド重合体を添加することで、凝固時に、前記乳化重合液中に、前記アルキレンオキシド重合体を存在させる請求項1または2記載のアクリルゴムの製造方法。
- 前記アルキレンオキシド重合体の重量平均分子量(Mw)が、10,000〜6,000,000の範囲である請求項1〜3のいずれかに記載のアクリルゴムの製造方法。
- 前記乳化重合液と前記金属硫酸塩との接触が、前記乳化重合液に前記金属硫酸塩を添加するか、前記乳化重合液を前記金属硫酸の溶液または分散液に投入するかいずれかの方法である請求項1〜4のいずれかに記載のアクリルゴムの製造方法。
- 前記洗浄工程の洗浄が、酸洗浄を含むものである請求項1〜5のいずれかに記載のアクリルゴムの製造方法。
- 請求項1〜6のいずれかに記載の製造方法で製造されるアクリルゴム。
- 単量体組成が、(メタ)アクリル酸エステル単量体単位50〜99.9重量%、架橋性単量体単位0.01〜20重量%及び共重合可能な他の単量体単位0〜49.99重量%である請求項7記載のアクリルゴム。
- 前記架橋性単量体単位が、カルボキシル基含有単量体単位である請求項8記載のアクリルゴム。
- ムーニー粘度(ML1+4、100℃)が、10〜150の範囲である請求項7〜9いずれかに記載のアクリルゴム。
- 請求項7〜10のいずれかに記載のアクリルゴムを含むゴム成分と架橋剤とを含んでなるゴム組成物。
- 更に、架橋促進剤、充填剤及びシランカップリング剤とからなる群から選ばれる少なくとも1種の配合剤を配合してなる請求項11記載のゴム組成物。
- 請求項11または12記載のゴム組成物を架橋してなるゴム架橋物。
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