CN114773762B - 一种含有丙烯酸酯官能团乙丙橡胶及其制备方法 - Google Patents
一种含有丙烯酸酯官能团乙丙橡胶及其制备方法 Download PDFInfo
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- CN114773762B CN114773762B CN202111428887.0A CN202111428887A CN114773762B CN 114773762 B CN114773762 B CN 114773762B CN 202111428887 A CN202111428887 A CN 202111428887A CN 114773762 B CN114773762 B CN 114773762B
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- 229920000181 Ethylene propylene rubber Polymers 0.000 title claims abstract description 60
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- 238000002360 preparation method Methods 0.000 title claims abstract description 13
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- 238000002156 mixing Methods 0.000 claims abstract description 48
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 24
- 239000006229 carbon black Substances 0.000 claims abstract description 22
- 239000003607 modifier Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000004073 vulcanization Methods 0.000 claims abstract description 14
- 239000003999 initiator Substances 0.000 claims abstract description 12
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- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 11
- 230000003712 anti-aging effect Effects 0.000 claims abstract description 11
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 11
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000008117 stearic acid Substances 0.000 claims abstract description 11
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 8
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- 239000004014 plasticizer Substances 0.000 claims abstract description 7
- 150000001875 compounds Chemical class 0.000 claims abstract description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 20
- 238000007599 discharging Methods 0.000 claims description 20
- -1 12-dodecanol ester Chemical class 0.000 claims description 11
- 238000001125 extrusion Methods 0.000 claims description 10
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 claims description 10
- 239000011787 zinc oxide Substances 0.000 claims description 10
- 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 claims description 9
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 9
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 9
- KOMNUTZXSVSERR-UHFFFAOYSA-N 1,3,5-tris(prop-2-enyl)-1,3,5-triazinane-2,4,6-trione Chemical compound C=CCN1C(=O)N(CC=C)C(=O)N(CC=C)C1=O KOMNUTZXSVSERR-UHFFFAOYSA-N 0.000 claims description 8
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 7
- 239000002656 Distearyl thiodipropionate Substances 0.000 claims description 7
- PWWSSIYVTQUJQQ-UHFFFAOYSA-N distearyl thiodipropionate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCCCCCCCC PWWSSIYVTQUJQQ-UHFFFAOYSA-N 0.000 claims description 7
- 235000019305 distearyl thiodipropionate Nutrition 0.000 claims description 7
- DEQZTKGFXNUBJL-UHFFFAOYSA-N n-(1,3-benzothiazol-2-ylsulfanyl)cyclohexanamine Chemical compound C1CCCCC1NSC1=NC2=CC=CC=C2S1 DEQZTKGFXNUBJL-UHFFFAOYSA-N 0.000 claims description 7
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 claims description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 5
- OKKRPWIIYQTPQF-UHFFFAOYSA-N Trimethylolpropane trimethacrylate Chemical compound CC(=C)C(=O)OCC(CC)(COC(=O)C(C)=C)COC(=O)C(C)=C OKKRPWIIYQTPQF-UHFFFAOYSA-N 0.000 claims description 5
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- 239000011593 sulfur Substances 0.000 claims description 5
- 229910052717 sulfur Inorganic materials 0.000 claims description 5
- OWRCNXZUPFZXOS-UHFFFAOYSA-N 1,3-diphenylguanidine Chemical compound C=1C=CC=CC=1NC(=N)NC1=CC=CC=C1 OWRCNXZUPFZXOS-UHFFFAOYSA-N 0.000 claims description 4
- IPJGAEWUPXWFPL-UHFFFAOYSA-N 1-[3-(2,5-dioxopyrrol-1-yl)phenyl]pyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C1=CC=CC(N2C(C=CC2=O)=O)=C1 IPJGAEWUPXWFPL-UHFFFAOYSA-N 0.000 claims description 4
- WFUGQJXVXHBTEM-UHFFFAOYSA-N 2-hydroperoxy-2-(2-hydroperoxybutan-2-ylperoxy)butane Chemical compound CCC(C)(OO)OOC(C)(CC)OO WFUGQJXVXHBTEM-UHFFFAOYSA-N 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000292 calcium oxide Substances 0.000 claims description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 4
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 4
- 239000008116 calcium stearate Substances 0.000 claims description 4
- 235000013539 calcium stearate Nutrition 0.000 claims description 4
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 4
- CVUNPKSKGHPMSY-UHFFFAOYSA-N ethyl 2-chloroprop-2-enoate Chemical compound CCOC(=O)C(Cl)=C CVUNPKSKGHPMSY-UHFFFAOYSA-N 0.000 claims description 4
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Chemical compound CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 claims description 4
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 4
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- XSQHUYDRSDBCHN-UHFFFAOYSA-N 2,3-dimethyl-2-propan-2-ylbutanenitrile Chemical compound CC(C)C(C)(C#N)C(C)C XSQHUYDRSDBCHN-UHFFFAOYSA-N 0.000 claims description 3
- DMWVYCCGCQPJEA-UHFFFAOYSA-N 2,5-bis(tert-butylperoxy)-2,5-dimethylhexane Chemical compound CC(C)(C)OOC(C)(C)CCC(C)(C)OOC(C)(C)C DMWVYCCGCQPJEA-UHFFFAOYSA-N 0.000 claims description 3
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 3
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 3
- CEGOLXSVJUTHNZ-UHFFFAOYSA-K aluminium tristearate Chemical compound [Al+3].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CEGOLXSVJUTHNZ-UHFFFAOYSA-K 0.000 claims description 3
- 229940063655 aluminum stearate Drugs 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
- 239000000178 monomer Substances 0.000 claims description 3
- 239000010690 paraffinic oil Substances 0.000 claims description 3
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 claims description 3
- MYWOJODOMFBVCB-UHFFFAOYSA-N 1,2,6-trimethylphenanthrene Chemical compound CC1=CC=C2C3=CC(C)=CC=C3C=CC2=C1C MYWOJODOMFBVCB-UHFFFAOYSA-N 0.000 claims description 2
- KMWIPXLIKIAZMT-UHFFFAOYSA-N 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanehydrazide Chemical compound CC(C)(C)C1=CC(CCC(=O)NN)=CC(C(C)(C)C)=C1O KMWIPXLIKIAZMT-UHFFFAOYSA-N 0.000 claims description 2
- JTHZUSWLNCPZLX-UHFFFAOYSA-N 6-fluoro-3-methyl-2h-indazole Chemical compound FC1=CC=C2C(C)=NNC2=C1 JTHZUSWLNCPZLX-UHFFFAOYSA-N 0.000 claims description 2
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 2
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- ANBFRLKBEIFNQU-UHFFFAOYSA-M potassium;octadecanoate Chemical compound [K+].CCCCCCCCCCCCCCCCCC([O-])=O ANBFRLKBEIFNQU-UHFFFAOYSA-M 0.000 claims description 2
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- NEYNBSGIXOOZGZ-UHFFFAOYSA-L zinc;butoxymethanedithioate Chemical compound [Zn+2].CCCCOC([S-])=S.CCCCOC([S-])=S NEYNBSGIXOOZGZ-UHFFFAOYSA-L 0.000 claims description 2
- DUBNHZYBDBBJHD-UHFFFAOYSA-L ziram Chemical compound [Zn+2].CN(C)C([S-])=S.CN(C)C([S-])=S DUBNHZYBDBBJHD-UHFFFAOYSA-L 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims 2
- VQOXZBDYSJBXMA-NQTDYLQESA-N nystatin A1 Chemical compound O[C@H]1[C@@H](N)[C@H](O)[C@@H](C)O[C@H]1O[C@H]1/C=C/C=C/C=C/C=C/CC/C=C/C=C/[C@H](C)[C@@H](O)[C@@H](C)[C@H](C)OC(=O)C[C@H](O)C[C@H](O)C[C@H](O)CC[C@@H](O)[C@H](O)C[C@](O)(C[C@H](O)[C@H]2C(O)=O)O[C@H]2C1 VQOXZBDYSJBXMA-NQTDYLQESA-N 0.000 claims 1
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- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 description 2
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- OJOWICOBYCXEKR-KRXBUXKQSA-N (5e)-5-ethylidenebicyclo[2.2.1]hept-2-ene Chemical compound C1C2C(=C/C)/CC1C=C2 OJOWICOBYCXEKR-KRXBUXKQSA-N 0.000 description 1
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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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
- C08F255/02—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
- C08F255/06—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms on to ethene-propene-diene terpolymers
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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
- C08K3/02—Elements
- C08K3/04—Carbon
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- 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
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/16—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
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- 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
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- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- 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
- C08K2201/00—Specific properties of additives
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- Processes Of Treating Macromolecular Substances (AREA)
Abstract
本发明提供一种含有丙烯酸酯官能团乙丙橡胶的制备方法。首先在密闭式炼胶机中,将乙丙橡胶、官能化改性剂、引发剂、稳定剂加入进行混炼,混炼完成后得到预混胶,用开炼机薄通剪裁制成胶条进行反应加工待用;然后在反应螺杆挤出机中,将预混胶条、抗氧剂按一定比例经螺杆挤出机反应混合,得到含丙烯酸酯官能团乙丙橡胶;最后用密闭式炼胶机将含有丙烯酸酯官能团乙丙橡胶、硬脂酸、硫化促进剂、硫化剂、炭黑N330、炭黑N660、防老剂RD和增塑剂依次加入进行混炼,得到混炼胶;将混炼胶在硫化机上硫化,测试硫化试片耐油性能、耐热等级及物理机械性能。该方法制备的乙丙橡胶耐油性明显提升,可耐IRM903型油品,耐热等级提高25~50℃,拉伸强度提高65.5%~116.4%,拉断伸长率提高24.3%~40.0%。
Description
技术领域
本发明涉及一种含有丙烯酸酯官能团乙丙橡胶的制备方法,属于高分子材料改性技术领域,具体涉及一种含有丙烯酸酯官能团乙丙橡胶的制备方法及其性能。
背景技术
乙丙橡胶因其具有良好的耐老化性、耐水性和耐热性,一直是橡胶工业的主要材料。但由于乙丙橡胶链结构中不含有极性官能团,不具备耐油特性,使得乙丙橡胶的应用受到很大限制。本发明发现,通过将乙丙橡胶、官能化改性剂、引发剂和稳定剂先在密闭式炼胶机混合均匀,再利用反应螺杆挤出机进行反应接枝,最后得到含有丙烯酸酯官能团的乙丙橡胶。该橡胶除保持原有乙丙橡胶优异的耐老化性能外,耐温等级提高了25~50℃,物理机械性能也有了明显的提升,并且具备了耐IRM903型油的特性,该方法未见之于专利报道。
发明内容
为了解决已有技术存在的问题,本发明提供了一种含有丙烯酸酯官能团乙丙橡胶的制备方法。
一种含有丙烯酸酯官能团乙丙橡胶的制备方法,其步骤条件如下:
在本发明中用密炼机将乙丙橡胶、官能化改性剂、引发剂和稳定剂混合均匀,再将混合后的胶料投入到反应螺杆挤出中反应接枝,得到含有丙烯酸酯官能团的乙丙橡胶。用本发明方法制备的材料在密炼机中与其它助剂、填料混合经硫化成型可获得具备耐油特性的乙丙橡胶硫化胶制品,并且耐热等级和物理机械性能也较改性前的产品有一定程度的提高。
具体的制备步骤为:
(a)在密闭式炼胶机中,将乙丙橡胶(EPDM)、官能化改性剂、引发剂和稳定剂按质量比100.00:20.00~50.00:0.05~1.00:1.00~5.00依次加入进行混炼,混炼时,密闭式炼胶机温度50~100℃,转速20~120转/分,混炼5~10分钟后,打开上顶栓,排胶得到混炼胶。用开炼机薄通成厚度2mm以下薄片,然后剪裁薄片成宽100mm以下的胶条待用;
(b)在反应螺杆挤出机中,将混炼胶条和抗氧剂按质量比100:1~5经螺杆挤出机反应混合后,得到含丙烯酸酯官能团乙丙橡胶。反应螺杆挤出机温度100~200℃,挤出速度20~80r/min,挤出时间1~5分钟;
(c)在密闭式炼胶机中,将含有丙烯酸酯官能团乙丙橡胶、硬脂酸、氧化锌、硫化促进剂、硫化剂、炭黑N330、炭黑N660、防老剂RD和增塑剂按质量比为100.0:0.5~2.0:0~5.00.5~2.0:0.5~3.0:30.0~50.0:30.0~50.0:0.5~2.0:5.0~20.0依次加入进行混炼,混炼时,密闭式炼胶机温度50~100℃,转速20~120转/分,混炼5~10分钟后,打开上顶栓,排胶得到混炼胶;将混炼胶在硫化机上硫化,硫化机温度150~180℃,压力5~15MPa,硫化时间10~30min,待硫化反应完成后,出片,测试其耐油性能、耐热等级及物理机械性能。
本发明密闭式炼胶机不限定型号和体积规格,只要能够将乙丙橡胶和其它助剂混合均匀即可;
本发明反应螺杆挤出机不限定型号和体积规格,只要能够将乙丙橡胶接枝丙烯酸酯官能团即可
本发明所采用的乙丙橡胶(EPDM)不限定牌号包括乙烯、丙烯的二元共聚物或乙烯、丙烯和第三单体的一种或多种。优选乙烯、丙烯和第三单体的三元共聚物,更优选第三单体为乙叉降冰片烯,含量9%的乙丙橡胶4045;
本发明所采用的官能化改性剂包括丙烯酸酯橡胶(ACM)、2-氯丙烯酸乙酯、三丙烯酸丙烷三甲醇酯、三羟甲基丙烷三甲基丙烯酸酯、聚乙二醇二甲基丙烯酸酯、丙烯酸十八酯、季戊四醇四丙烯酸酯和2-甲基-2-丙烯酸-1,12-十二双醇酯的一种或多种。优选丙烯酸酯橡胶(ACM)、2-氯丙烯酸乙酯、三丙烯酸丙烷三甲醇酯、三羟甲基丙烷三甲基丙烯酸酯、聚乙二醇二甲基丙烯酸酯;
本发明所采用的引发剂包括过氧化二异丙苯(DCP)、过氧化苯甲酰(BPO)、过氧化苯甲酰叔丁酯(CP-01)和过氧化甲乙酮(MEKP)的一种或多种。优选过氧化二异丙苯(DCP)和过氧化苯甲酰(BPO);
本发明所采用的稳定剂为氧化钙、氧化镁、氧化铝、硬脂酸钙、硬脂酸镁、硬脂酸铝、硬脂酸钾的一种或多种。优选氧化钙、氧化镁、硬脂酸钙、硬脂酸镁和硬脂酸铝;
本发明所采用的抗氧剂为四(β-(3,5-二叔丁基-4-羟基苯基)丙酸)季戊四醇酯(1010)、β-(4-羟基苯基-3,5-二叔丁基)丙酸正十八碳醇酯(1076)、N,N'-1,6-亚已基-双[3-(3,5-二叔丁基-4-羟基苯基)丙酰胺](1098)、N,N'-双[3-(3,5-二叔丁基-4-羟基苯基)丙酰]肼(1024)、亚磷酸三(2,4-二叔丁基苯基)酯(168)和硫代二丙酸二硬脂醇酯或硫代二丙酸二(十八)酯(DSTP)的一种和多种的一种或多种。优选四(β-(3,5-二叔丁基-4-羟基苯基)丙酸)季戊四醇酯(1010)和β-(4-羟基苯基-3,5-二叔丁基)丙酸正十八碳醇酯(1076);
本发明所采用的硫化促进剂为六次甲基四胺/促进剂H、二苯胍/促进剂D、二硫化四甲基秋兰姆/促进剂TMTD、2-硫醇基苯骈噻唑/促进剂M、二甲基二硫代氨基甲酸锌/促进剂ZDMC、丁基黄原酸锌/促进剂ZBX、N-环己基-2-苯并噻唑次磺酰胺/促进剂CZ、乙烯硫脲/促进剂(NA-22)或过氧化物促进剂:三烯丙基异氰脲酸酯(促进剂TAIC)、N,N’-间苯撑双马来酰亚胺(HVA2)中的一种或多种。优选N-环己基-2-苯并噻唑次磺酰胺/促进剂CZ、三烯丙基异氰脲酸酯(促进剂TAIC)和N,N’-间苯撑双马来酰亚胺(HVA2);
本发明所采用的硫化剂为硫磺、六亚甲基二胺氨基甲酸盐(Diak No.1)、2,5-二甲基-2,5-双(叔丁基过氧基)己烷(双2-5)或过氧化二叔丁基(DTBP)中一种或多种。优选硫磺、六亚甲基二胺氨基甲酸盐(Diak No.1)和2,5-二甲基-2,5-双(叔丁基过氧基)己烷(双2-5);
本发明所采用的增塑剂为石蜡油2280、环烷油K30或芳烃油SUNDEX790中一种或多种。优选石蜡油2280和环烷油K30;
本发明所采用的硬脂酸、氧化锌、炭黑N330、炭黑N660、防老剂RD和增塑剂均为市售品,具体厂家和参数见表1。
表1.助剂信息表
本发明所采用的通用橡胶包括乙丙橡胶和丙烯酸酯橡胶,具体指标参数见表2。
表2.橡胶原料信息表
有益效果:
本发明具有以下有益效果:
(a)本发明可赋予乙丙橡胶耐IRM903型油的特性,拓宽了乙丙橡胶的应用领域,价格低于市场上性能需求相近的丙烯酸酯橡胶(ACM)和乙烯-丙烯酸酯共聚物(AEM),详细情况见表3。
(b)本发明材料的耐温等级和物理机械性能相比于乙丙橡胶均有一定提高,其中耐温提高25~50℃,拉伸强度提高65.5%~116.4%,拉断伸长率提高24.3%~40.0%,可耐IRM903型油品,见表4。
具体实施方式
本发明实施例中用到的设备,设备的厂家及型号如下,本领域技术人员可以根据需求选择适合的设备,设备的选择不同不影响本发明的发明构思。
密闭式炼胶机:南京创博机械设备有限公司,ML-4.5L;
反应螺杆挤出机:南京创博机械设备有限公司,TSH-25;
材料试验机:吉林祎胜科技有限公司,GDWDW-10KN。
实施例1:
制备含有丙烯酸酯官能团乙丙橡胶,其步骤和条件如下:
(a)在密闭式炼胶机中,将乙丙橡胶(4045)、官能化改性剂ACM、引发剂过氧化二异丙苯(DCP)和稳定剂氧化钙按质量比100.00:20.00:0.05:1.00依次加入进行混炼,混炼时,密闭式炼胶机温度100℃,转速20转/分,混炼10分钟后,打开上顶栓,排胶得到混炼胶。用开炼机薄通成厚度1.9mm薄片,然后剪裁薄片成宽95mm的胶条待用;
(b)在反应螺杆挤出机中,将混炼胶条和抗氧剂1010按质量比100:1经反应螺杆挤出机反应混合后,得到含丙烯酸酯官能团乙丙橡胶。反应螺杆挤出机温度150℃,挤出速度20r/min,挤出时间5分钟;
(c)在密闭式炼胶机中,将含有丙烯酸酯官能团乙丙橡胶、硬脂酸、氧化锌、硫化促进剂CZ、硫磺、炭黑N330、炭黑N660、防老剂RD和石蜡油2280按质量比为100.0:1.0:3.0:1.0:1.5:30.0:30.0:0.5:5.0依次加入进行混炼,混炼时,密闭式炼胶机温度50℃,转速20转/分,混炼10分钟后,打开上顶栓,排胶得到混炼胶;将混炼胶在硫化机上硫化,硫化机温度150℃,压力5MPa,硫化时间30min,待硫化反应完成后,出片,测试其耐油性能、耐热等级及物理机械性能,详见表3和表4。
实施例2:
制备含有丙烯酸酯官能团乙丙橡胶,其步骤和条件如下:
(a)在密闭式炼胶机中,将乙丙橡胶(3072P)、官能化改性剂三羟甲基丙烷三甲基丙烯酸酯、引发剂过氧化苯甲酰(BPO)和稳定剂硬脂酸钙按质量比100.00:50.00:1.00:5.00依次加入进行混炼,混炼时,密闭式炼胶机温度50℃,转速120转/分,混炼5分钟后,打开上顶栓,排胶得到混炼胶。用开炼机薄通成厚度1.5mm薄片,然后剪裁薄片成宽80mm的胶条待用;
(b)在反应螺杆挤出机中,将混炼胶条,抗氧剂1076按质量比100:5经反应螺杆挤出机反应混合后,得到含丙烯酸酯官能团乙丙橡胶。反应螺杆挤出机温度200℃,挤出速度80r/min,挤出时间1分钟;
(c)在密闭式炼胶机中,将含有丙烯酸酯官能团乙丙橡胶、硬脂酸、氧化锌、硫化促进剂TAIC、硫化剂双2-5、炭黑N330、炭黑N660、防老剂RD和环烷油K30按质量比为100.0:0.5:5.0:1.5:3.0:50.0:50.0:2.0:20.0依次加入进行混炼,混炼时,密闭式炼胶机温度100℃,转速120转/分,混炼5分钟后,打开上顶栓,排胶得到混炼胶;将混炼胶在硫化机上硫化,硫化机温度180℃,压力15MPa,硫化时间10min,待硫化反应完成后,出片,测试其耐油性能、耐热等级及物理机械性能,详见表3和表4。
实施例3:
制备含有丙烯酸酯官能团乙丙橡胶,其步骤和条件如下:
(a)在密闭式炼胶机中,将乙丙橡胶(4045)、官能化改性剂三丙烯酸丙烷三甲醇酯、引发剂DCP和稳定剂硬脂酸镁按质量比100.00:40.00:0.10:2.00依次加入进行混炼,混炼时,密闭式炼胶机温度70℃,转速60转/分,混炼8分钟后,打开上顶栓,排胶得到混炼胶。用开炼机薄通成厚度1.6mm薄片,然后剪裁薄片成宽70mm的胶条待用;
(b)在反应螺杆挤出机中,将混炼胶条和抗氧剂1076按质量比100:2经反应螺杆挤出机反应混合后,得到含丙烯酸酯官能团乙丙橡胶。反应螺杆挤出机温度180℃,挤出速度60r/min,挤出时间3分钟;
(c)在密闭式炼胶机中,将含有丙烯酸酯官能团乙丙橡胶、硬脂酸、氧化锌、硫化促进剂HVA2、硫化剂双2-5、炭黑N330、炭黑N660、防老剂RD和石蜡油2280按质量比为100.0:0.5:4.0:1.5:2.0:35.0:40.0:1.0:15.0依次加入进行混炼,混炼时,密闭式炼胶机温度70℃,转速60转/分,混炼8分钟后,打开上顶栓,排胶得到混炼胶;将混炼胶在硫化机上硫化,硫化机温度160℃,压力10MPa,硫化时间15min,待硫化反应完成后,出片,测试其耐油性能、耐热等级及物理机械性能,详见表3和表4。
实施例4:
(a)步骤官能化改性剂采用2-氯丙烯酸乙酯,(b)步骤抗氧剂用1098,(c)步骤硫化促进剂用TAIC,硫化剂用Diak No.1,其它步骤与实施例3相同,详见表3和表4。
实施例5:
(a)步骤官能化改性剂采用三羟甲基丙烷三甲基丙烯酸酯,(b)步骤抗氧剂用1024,(c)步骤硫化促进剂用CZ,硫化剂用硫磺,其它步骤与实施例3相同,详见表3和表4。
实施例6:
(a)步骤官能化改性剂采用聚乙二醇二甲基丙烯酸酯,(b)步骤抗氧剂用DSTP,其它步骤与实施例3相同,详见表3和表4。
对比例1:
在密闭式炼胶机中,将含有乙丙橡胶(4045)、硬脂酸、氧化锌、硫化促进剂HVA2、硫化剂双2-5、炭黑N330、炭黑N660、防老剂RD和石蜡油2280按质量比为100.0:0.5:4.0:1.5:2.0:35.0:40.0:1.0:15.0依次加入进行混炼,混炼时,密闭式炼胶机温度70℃,转速60转/分,混炼8分钟后,打开上顶栓,排胶得到混炼胶;将混炼胶在硫化机上硫化,硫化机温度160℃,压力10MPa,硫化时间15min,待硫化反应完成后,出片,测试其耐油性能、耐热等级及物理机械性能,详见表3和表4。
对比例2:
在密闭式炼胶机中,将乙丙橡胶(4045)、官能化改性剂三丙烯酸丙烷三甲醇酯、硬脂酸、氧化锌、硫化促进剂HVA2、硫化剂双2-5、炭黑N330、炭黑N660、防老剂RD和石蜡油2280按质量比为71.43:28.57:0.5:4.0:1.5:2.0:35.0:40.0:1.0:15.0依次加入进行混炼,混炼时,密闭式炼胶机温度70℃,转速60转/分,混炼8分钟后,打开上顶栓,排胶得到混炼胶;将混炼胶在硫化机上硫化,硫化机温度160℃,压力10MPa,硫化时间15min,待硫化反应完成后,出片,测试其耐油性能、耐热等级及物理机械性能,详见表3和表4。
对比例3:
(a)在密闭式炼胶机中,将乙丙橡胶(4045)、官能化改性剂三丙烯酸丙烷三甲醇酯、引发剂DCP和稳定剂硬脂酸镁按质量比100.00:40.00:0.10:2.00依次加入进行混炼,混炼时,密闭式炼胶机温度70℃,转速60转/分,混炼8分钟后,打开上顶栓,排胶得到混炼胶。用开炼机薄通成厚度1.6mm薄片,然后剪裁薄片成宽70mm的胶条待用;
(b)在密闭式炼胶机中,将含有混合的乙丙胶条、硬脂酸、氧化锌、硫化促进剂HVA2、硫化剂双2-5、炭黑N330、炭黑N660、防老剂RD和石蜡油2280按质量比为100.0:0.5:4.0:1.5:2.0:35.0:40.0:1.0:15.0依次加入进行混炼,混炼时,密闭式炼胶机温度70℃,转速60转/分,混炼8分钟后,打开上顶栓,排胶得到混炼胶;将混炼胶在硫化机上硫化,硫化机温度160℃,压力10MPa,硫化时间15min,待硫化反应完成后,出片,测试其耐油性能、耐热等级及物理机械性能,详见表3和表4。
表3.含有丙烯酸酯官能团乙丙橡胶的耐油性能
*耐油试验按照“GB/T 1690-2010硫化橡胶或热塑性橡胶耐液体试验方法”测定,试验条件70℃×96h,油品型号:符合ASTM标准IRM903型油;
*硬度变化按以下公式计算:硬度变化=样品耐油试验后的硬度-样品耐油试验前的硬度;
*拉伸强度变化率按照以下公式计算:拉伸强度变化率=(样品耐油试验后的拉伸强度-样品耐油试验前的拉伸强度)÷样品耐油试验前的拉伸强度×100%;
*拉断伸长率变化率按照以下公式计算:拉断伸长率变化率=(样品耐油试验后的拉断伸长率-样品耐油试验前的拉断伸长率)÷样品耐油试验前的拉断伸长率×100%;
*体积变化率按照以下公式计算:体积变化率=(样品耐油试验后的体积-样品耐油试验前的体积)÷样品耐油试验前的体积×100%。
表4.含有丙烯酸酯官能团乙丙橡胶的耐热等级和物理机械性能
*耐温等级按照“GB/T 20028-2005应用阿累尼乌斯图推算高分子材料贮存寿命和最高使用温度”测定。
*拉伸强度和扯断伸长率按照“GB/T 528-2009硫化橡胶或热塑性橡胶拉伸应力应变性能的测定”测试。
从表3、表4数据可知,采用本发明方法制备的含丙烯酸酯乙丙橡胶在IRM903型油中硬度变化、拉伸强度变化率、拉断伸长变化率和体积变化率的数据指标明显优于未采取此工艺的乙丙橡胶产品,说明本发明的材料具有耐IRM903型油的特性。同时,本发明方法制备的含丙烯酸酯乙丙橡胶较传统技术产品拉伸强度提高65.5%~116.4%,拉断伸长率提高24.3%~40.0%,耐热温度可提高25~50℃,表明本发明材料还具备提高物理机械性能、增加耐热等级的作用。
Claims (10)
1.一种含有丙烯酸酯官能团乙丙橡胶的制备方法,其特征在于,所述制备方法按照以下步骤进行:
(a)在密闭式炼胶机中,将乙丙橡胶、官能化改性剂、引发剂和稳定剂按质量比100.00:15.00~55.00:0.01~1.50:0.50~5.50(加入进行混炼,混炼时,密闭式炼胶机温度50~100℃,转速20~120转/分,混炼5~10分钟后,排胶得到混炼胶;用开炼机薄通成厚度1.5~2.5mm 薄片,然后剪裁薄片成宽50~100mm的胶条待用;所述的官能化改性剂包括2-氯丙烯酸乙酯、三丙烯酸丙烷三甲醇酯、三羟甲基丙烷三甲基丙烯酸酯、聚乙二醇二甲基丙烯酸酯、丙烯酸十八酯、季戊四醇四丙烯酸酯和2-甲基-2-丙烯酸-1,12-十二双醇酯的一种或多种;
(b)在反应螺杆挤出机中,将混炼胶条和抗氧剂按质量比100:1~5经螺杆挤出机反应混合后,得到含丙烯酸酯官能团乙丙橡胶;反应螺杆挤出机温度100~200℃,挤出速度20~80r/min,挤出时间1~5分钟;
(c)在密闭式炼胶机中,将含有丙烯酸酯官能团乙丙橡胶、硬脂酸、氧化锌、硫化促进剂、硫化剂、炭黑N330、炭黑N660、防老剂RD和增塑剂按质量比为100.0:0.1~2.5:0~5.5:0.1~2.5:0.1~3.5:25.0~55.0:25.0~55.0:0.1~2.5:1.0~25.0加入进行混炼,混炼时,密闭式炼胶机温度40~120℃,转速20~120转/分,混炼5~10分钟后,排胶得到混炼胶;将混炼胶在硫化机上硫化,硫化机温度130~190℃,压力1~20MPa,硫化时间5~40min,待硫化反应完成后,出片。
2.根据权利要求1所述的方法,其特征在于,
(a)在密闭式炼胶机中,将乙丙橡胶、官能化改性剂、引发剂和稳定剂按质量比100.00:20.00~50.00:0.05~1.00:1.00~5.00加入进行混炼;
(c)在密闭式炼胶机中,将含有丙烯酸酯官能团乙丙橡胶、硬脂酸、氧化锌、硫化促进剂、硫化剂、炭黑N330、炭黑N660、防老剂RD和增塑剂按质量比为100.0:0.5~2.0:0~5.0:0.5~2.0:0.5~3.0:30.0~50.0:30.0~50.0:0.5~2.0:5.0~20.0加入进行混炼,密闭式炼胶机温度50~100℃;将混炼胶在硫化机上硫化,硫化机温度150~180℃,压力5~15MPa,硫化时间10~30min,待硫化反应完成后,出片。
3.根据权利要求1所述的方法,其特征在于,
步骤(a)中所述的乙丙橡胶包括乙烯、丙烯的二元共聚物或乙烯、丙烯和第三单体的三元共聚物的一种或多种。
4.根据权利要求1所述的方法,其特征在于,步骤(a)中所述的引发剂包括过氧化二异丙苯DCP、过氧化苯甲酰BPO、过氧化苯甲酰叔丁酯CP-01和过氧化甲乙酮MEKP的一种或多种。
5.根据权利要求1所述的方法,其特征在于,步骤(a)中所述的稳定剂为氧化钙、氧化镁、氧化铝、硬脂酸钙、硬脂酸镁、硬脂酸铝、硬脂酸钾的一种或多种。
6.根据权利要求1所述的方法,其特征在于,步骤(b)中所述的抗氧剂为四(β-(3,5-二叔丁基-4-羟基苯基)丙酸)季戊四醇酯(1010)、β-(4-羟基苯基-3,5-二叔丁基)丙酸正十八碳醇酯(1076)、N,N'-1,6-亚已基-双[3-(3,5-二叔丁基-4-羟基苯基)丙酰胺](1098)、N,N'-双[3-(3,5-二叔丁基-4-羟基苯基)丙酰]肼(1024)、亚磷酸三(2,4-二叔丁基苯基)酯(168)和硫代二丙酸二硬脂醇酯或硫代二丙酸二(十八)酯(DSTP)的一种或多种。
7.根据权利要求1所述的方法,其特征在于,步骤(c)中所述的硫化促进剂为六次甲基四胺/促进剂H、二苯胍/促进剂D、二硫化四甲基秋兰姆/促进剂TMTD、2-硫醇基苯骈噻唑/促进剂M、二甲基二硫代氨基甲酸锌/促进剂ZDMC、丁基黄原酸锌/促进剂ZBX、N-环己基-2-苯并噻唑次磺酰胺/促进剂CZ、三烯丙基异氰脲酸酯(促进剂TAIC)、N,N’-间苯撑双马来酰亚胺(HVA2)中的一种或多种。
8.根据权利要求1所述的方法,其特征在于,步骤(c)中所述的硫化剂为硫磺、六亚甲基二胺氨基甲酸盐(Diak No.1)、2,5-二甲基-2,5-双(叔丁基过氧基)己烷(双2-5)或过氧化二叔丁基(DTBP)中一种或多种。
9.根据权利要求1所述的方法,其特征在于,步骤(c)中所述的增塑剂为石蜡油2280、环烷油K30或芳烃油SUNDEX790中一种或多种。
10.一种权利要求1-9任一所述制备方法制备得到的含有丙烯酸酯官能团乙丙橡胶。
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