CN118652499B - A kind of EPDM rubber sealing ring and preparation method thereof - Google Patents
A kind of EPDM rubber sealing ring and preparation method thereof Download PDFInfo
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- CN118652499B CN118652499B CN202410739602.2A CN202410739602A CN118652499B CN 118652499 B CN118652499 B CN 118652499B CN 202410739602 A CN202410739602 A CN 202410739602A CN 118652499 B CN118652499 B CN 118652499B
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- 238000007789 sealing Methods 0.000 title claims abstract description 61
- 229920002943 EPDM rubber Polymers 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 51
- 229920003225 polyurethane elastomer Polymers 0.000 claims abstract description 42
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 32
- INQDDHNZXOAFFD-UHFFFAOYSA-N 2-[2-(2-prop-2-enoyloxyethoxy)ethoxy]ethyl prop-2-enoate Chemical compound C=CC(=O)OCCOCCOCCOC(=O)C=C INQDDHNZXOAFFD-UHFFFAOYSA-N 0.000 claims abstract description 30
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910000077 silane Inorganic materials 0.000 claims abstract description 30
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 239000003054 catalyst Substances 0.000 claims abstract description 15
- 229920000459 Nitrile rubber Polymers 0.000 claims abstract description 14
- 125000005442 diisocyanate group Chemical group 0.000 claims abstract description 14
- 239000002270 dispersing agent Substances 0.000 claims abstract description 14
- FYRWKWGEFZTOQI-UHFFFAOYSA-N 3-prop-2-enoxy-2,2-bis(prop-2-enoxymethyl)propan-1-ol Chemical compound C=CCOCC(CO)(COCC=C)COCC=C FYRWKWGEFZTOQI-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 239000000945 filler Substances 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 10
- 239000004014 plasticizer Substances 0.000 claims abstract description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 16
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 15
- 150000001343 alkyl silanes Chemical class 0.000 claims description 10
- 239000006229 carbon black Substances 0.000 claims description 10
- -1 polytrimethylene Polymers 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 8
- 239000004359 castor oil Substances 0.000 claims description 8
- 235000019438 castor oil Nutrition 0.000 claims description 8
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 8
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 8
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical compound [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 7
- 238000005520 cutting process Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000004080 punching Methods 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 3
- SCPWMSBAGXEGPW-UHFFFAOYSA-N dodecyl(trimethoxy)silane Chemical compound CCCCCCCCCCCC[Si](OC)(OC)OC SCPWMSBAGXEGPW-UHFFFAOYSA-N 0.000 claims description 3
- OYGYKEULCAINCL-UHFFFAOYSA-N triethoxy(hexadecyl)silane Chemical compound CCCCCCCCCCCCCCCC[Si](OCC)(OCC)OCC OYGYKEULCAINCL-UHFFFAOYSA-N 0.000 claims description 3
- 239000004927 clay Substances 0.000 claims description 2
- YGUFXEJWPRRAEK-UHFFFAOYSA-N dodecyl(triethoxy)silane Chemical compound CCCCCCCCCCCC[Si](OCC)(OCC)OCC YGUFXEJWPRRAEK-UHFFFAOYSA-N 0.000 claims description 2
- RSKGMYDENCAJEN-UHFFFAOYSA-N hexadecyl(trimethoxy)silane Chemical compound CCCCCCCCCCCCCCCC[Si](OC)(OC)OC RSKGMYDENCAJEN-UHFFFAOYSA-N 0.000 claims description 2
- 239000003921 oil Substances 0.000 claims description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims 1
- 239000005662 Paraffin oil Substances 0.000 claims 1
- 230000006835 compression Effects 0.000 abstract description 23
- 238000007906 compression Methods 0.000 abstract description 23
- 229920001971 elastomer Polymers 0.000 abstract description 15
- 239000005060 rubber Substances 0.000 abstract description 15
- 230000007774 longterm Effects 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 26
- 238000004073 vulcanization Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- 238000004132 cross linking Methods 0.000 description 5
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 230000002195 synergetic effect Effects 0.000 description 4
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical group CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 238000000748 compression moulding Methods 0.000 description 3
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical group CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 239000012975 dibutyltin dilaurate Substances 0.000 description 2
- 150000001993 dienes Chemical class 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000012974 tin catalyst Substances 0.000 description 2
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical group OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 description 1
- CPGFMWPQXUXQRX-UHFFFAOYSA-N 3-amino-3-(4-fluorophenyl)propanoic acid Chemical compound OC(=O)CC(N)C1=CC=C(F)C=C1 CPGFMWPQXUXQRX-UHFFFAOYSA-N 0.000 description 1
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
- 229920000181 Ethylene propylene rubber Polymers 0.000 description 1
- 239000005057 Hexamethylene diisocyanate Substances 0.000 description 1
- 239000004594 Masterbatch (MB) Substances 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 125000003342 alkenyl group Chemical group 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- WITDFSFZHZYQHB-UHFFFAOYSA-N dibenzylcarbamothioylsulfanyl n,n-dibenzylcarbamodithioate Chemical compound C=1C=CC=CC=1CN(CC=1C=CC=CC=1)C(=S)SSC(=S)N(CC=1C=CC=CC=1)CC1=CC=CC=C1 WITDFSFZHZYQHB-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- MABAWBWRUSBLKQ-UHFFFAOYSA-N ethenyl-tri(propan-2-yloxy)silane Chemical group CC(C)O[Si](OC(C)C)(OC(C)C)C=C MABAWBWRUSBLKQ-UHFFFAOYSA-N 0.000 description 1
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 229940057995 liquid paraffin Drugs 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000010690 paraffinic oil Substances 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000006235 reinforcing carbon black Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 229930195734 saturated hydrocarbon Natural products 0.000 description 1
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 description 1
- BOXSVZNGTQTENJ-UHFFFAOYSA-L zinc dibutyldithiocarbamate Chemical compound [Zn+2].CCCCN(C([S-])=S)CCCC.CCCCN(C([S-])=S)CCCC BOXSVZNGTQTENJ-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- 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—Ethene-propene or ethene-propene-diene copolymers
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- 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
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Sealing Material Composition (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The application relates to the field of rubber materials, and particularly discloses an ethylene propylene diene monomer rubber sealing ring and a preparation method thereof. The ethylene propylene diene monomer rubber sealing ring is prepared from the following raw materials, by weight, 60-80 parts of ethylene propylene diene monomer rubber, 20-30 parts of silane grafted polyurethane elastomer, 8-15 parts of carboxyl-terminated liquid nitrile rubber, 35-55 parts of filler, 10-20 parts of plasticizer, 5-10 parts of dispersing agent, 3-8 parts of accelerator and 1-3 parts of vulcanizing agent, wherein the silane grafted polyurethane elastomer is prepared by reacting pentaerythritol triallyl ether, triethylene glycol diacrylate, a silane coupling agent, diisocyanate and a catalyst. The preparation process is simple, and the prepared ethylene propylene diene monomer rubber sealing ring has moderate hardness, good compression set and good sealing stability under a long-term compression state.
Description
Technical Field
The application relates to the field of rubber materials, in particular to an ethylene propylene diene monomer rubber sealing ring and a preparation method thereof.
Background
Ethylene Propylene Diene Monomer (EPDM) is a copolymer of ethylene, propylene and a small amount of non-conjugated diene, is one of ethylene propylene rubbers, is expressed by EPDM, has excellent ozone resistance, heat resistance, weather resistance and other ageing resistance, and can be widely used in the fields of automobile parts, waterproof materials for buildings, wire and cable jackets, heat-resistant rubber pipes, rubber belts, automobile sealing parts and the like.
When the ethylene propylene diene monomer is applied to the sealing ring, the ethylene propylene diene monomer is generally composed of ethylene propylene diene monomer, carbon black filler, cross-linking agent, anti-aging agent and the like, the carbon black filler is used in the ethylene propylene diene monomer in a large amount, and the carbon black filler is added, so that the hardness of the prepared sealing ring is increased, and the sealing stability of the sealing ring is easily reduced in a state of long-term sealing compression.
Disclosure of Invention
The application provides an ethylene propylene diene monomer rubber sealing ring and a preparation method thereof, and aims to solve the problem that the sealing stability is easy to be reduced when the sealing ring is used in a state of long-term compression.
In a first aspect, the application provides an ethylene propylene diene monomer rubber sealing ring, which adopts the following technical scheme:
An ethylene propylene diene monomer rubber sealing ring is prepared from the following raw materials in parts by weight:
60-80 parts of ethylene propylene diene monomer
20-30 Parts of silane grafted polyurethane elastomer
8-15 Parts of carboxyl-terminated liquid nitrile rubber
35-55 Parts of filling material
10-20 Parts of plasticizer
5-10 Parts of dispersing agent
3-8 Parts of promoter
1-3 Parts of vulcanizing agent;
The silane grafted polyurethane elastomer is prepared by reacting pentaerythritol triallyl ether, triethylene glycol diacrylate, a silane coupling agent, diisocyanate and a catalyst.
By adopting the technical scheme, the ethylene propylene diene monomer is a copolymer of ethylene, propylene and a small amount of non-conjugated diene, the main chain is composed of chemically stable saturated hydrocarbon, unsaturated double bonds are contained in the side chain, so that the sealing ring has better ageing resistance and flexibility, the silane grafted polyurethane elastomer has better crosslinking network structure, better flexibility and elasticity, active carboxyl groups are arranged at two ends of a carboxyl-terminated liquid nitrile rubber molecular chain segment, better elasticity and strength are realized, the ethylene propylene diene monomer, the silane grafted polyurethane elastomer and the carboxyl-terminated liquid nitrile rubber are compounded in better amount to serve as a rubber system, the three have better synergistic effect, the prepared sealing ring has better flexibility and compression set resistance under the action of a vulcanizing agent and a promoter, the filling material has the effect of improving the mechanical strength of the sealing ring, but the addition of the filling material increases the hardness of the sealing ring, so that the compression set resistance of the prepared sealing ring is reduced, and the filling of the silane grafted polyurethane elastomer prepared by pentaerythritol triallyl ether, triethylene glycol diacrylate, silane coupling agent, diisocyanate and a catalyst is added, the sealing ring is better in the application, the sealing ring is better in the better compression set resistance and better dispersion state, and better compression set resistance is realized under the action of the sealing ring, and the sealing ring is better compression set is realized, and the sealing ring has better compression set resistance and better compression set resistance is realized.
Preferably, the silane grafted polyurethane elastomer is prepared from the following raw materials in parts by weight:
20-40 parts of diisocyanate
Alkane coupling agent 5-8 parts
Pentaerythritol triallyl ether 5-10 parts
3-8 Parts of triethylene glycol diacrylate
1-3 Parts of a catalyst.
Through the technical scheme, under the action of the catalyst, the diisocyanate and the silane coupling agent are subjected to grafting reaction, pentaerythritol triallyl ether has a branched chain alkenyl structure, triethylene glycol diacrylate has an acrylic unsaturated structure and can be subjected to further crosslinking reaction with the diisocyanate, and the diisocyanate and the triethylene glycol diacrylate have good synergistic effect, so that the silane grafted polyurethane elastomer with a compact interweaved network molecular structure is prepared, has good temperature resistance and elasticity, and can further improve the flexibility and permanent compression set resistance of the prepared sealing ring.
Preferably, the silane coupling agent consists of a vinyl silane coupling agent and a long-chain alkyl silane coupling agent with the weight ratio of (0.2-0.5), wherein the long-chain alkyl silane coupling agent is one or more of dodecyl trimethoxy silane, dodecyl triethoxy silane, hexadecyl trimethoxy silane and hexadecyl triethoxy silane.
By adopting the technical scheme, the long-chain alkyl silane coupling agent has a hydrophobic flexible chain segment, can be stably dispersed and interwoven in a reticular molecular structure, further improves the network structure stability and compactness of the prepared silane grafted polyurethane elastomer, has a better synergistic effect with the vinyl silane coupling agent by a better dosage ratio, can be stably interwoven and grafted with a diisocyanate system, improves the flexibility and elasticity of the prepared silane grafted polyurethane elastomer, and further improves the compression set resistance of the prepared sealing ring.
Preferably, the catalyst consists of an organic tin catalyst and an organic amine catalyst in a weight ratio of (1-2): 1, wherein the organic tin catalyst is dibutyl tin dilaurate and/or stannous octoate, and the organic amine catalyst is triethylamine or dimethylamine. One or a combination of diethylenetriamine.
By adopting the technical scheme, the catalyst with a better dosage ratio can stably catalyze the grafting reaction, and the elasticity and the molecular structure compactness of the prepared silane grafted polyurethane elastomer are further improved.
Preferably, the silane grafted polyurethane elastomer is prepared by the steps of:
A1, adding diisocyanate, pentaerythritol triallyl ether and triethylene glycol diacrylate into reaction equipment, heating to 40-60 ℃, and uniformly mixing to prepare a mixture A;
and A2, adding a silane coupling agent and a catalyst into the mixture A, vacuumizing, heating to 80-95 ℃, and reacting for 1-3 hours to obtain the silane grafted polyurethane elastomer.
By adopting the technical scheme, each component can stably carry out grafting reaction, and the silane grafted polyurethane elastomer with stable performance is prepared.
Preferably, the filler is one or a combination of carbon black, white carbon black, calcium carbonate, talcum powder, barium sulfate and clay.
By adopting the technical scheme, the filler is suitable for the rubber system provided by the application, and has a better performance reinforcing effect on the rubber system.
Preferably, the plasticizer is paraffinic oil and/or naphthenic oil.
By adopting the technical scheme, the plasticizer can improve the processing stability and fluidity of a rubber system and the comprehensive performance of the prepared sealing ring.
Preferably, the dispersant consists of hydrogenated castor oil and polytrimethylene ether glycol in a weight ratio of 1 (0.2-0.8).
By adopting the technical scheme, the polytrimethylene ether glycol has a spiral molecular structure, and is compounded with hydrogenated castor oil to be used as a dispersing agent, so that the vulcanization crosslinking degree of a rubber system can be improved, and the flexibility and compression set resistance of the prepared sealing ring are further improved.
Preferably, the accelerator is one or a combination of DPTT, CBS-80, TT-80 and BZ-80, and the vulcanizing agent is S-80 and/or a bis-di-penta vulcanizing agent.
By adopting the technical scheme, the vulcanizing agent and the accelerator are suitable for the rubber system, and have moderate vulcanizing rate and good vulcanizing efficiency.
In a second aspect, the application provides a preparation method of an ethylene propylene diene monomer rubber sealing ring, which adopts the following technical scheme:
The preparation method of the ethylene propylene diene monomer rubber sealing ring comprises the following preparation steps:
s1, mixing ethylene propylene diene monomer rubber, silane grafted polyurethane elastomer, carboxyl-terminated liquid nitrile rubber, a filler, a plasticizer and a dispersing agent to prepare a mixed material I;
S2, after the temperature is reduced to be less than 90 ℃, adding an accelerator and a vulcanizing agent for mixing, tabletting and cutting to obtain a pre-tabletting;
and S3, performing compression molding vulcanization molding and punching on the prefabricated piece to obtain the sealing ring.
Through adopting above-mentioned technical scheme, carry out the pugging with each raw materials earlier, cool down after the pugging and add promoter and vulcanizing agent, the cooling is in order that vulcanizing agent and promoter can mix to the system steadily, and can not influence vulcanizing agent and promoter's vulcanization stability, later carry out the preforming, cut into prefabricated piece, carry out the vulcanization shaping with prefabricated piece, the in-process of vulcanization shaping forms the shape of sealing washer, later carries out die-cutting, gets rid of the leftover bits to this preparation obtains the stable ethylene propylene diene monomer rubber sealing washer of performance.
Preferably, the mixing temperature in the step S1 is 160-180 ℃, and the molding temperature in the step S3 is 170-180 ℃.
By adopting the technical scheme, the better mixing temperature can ensure that the raw materials of all the components are uniformly mixed, have better fluidity and viscosity, are easy to carry out the later processing procedures, and the better molding temperature can ensure that the prefabricated sheet is stably vulcanized and crosslinked, so that the sealing ring with better flexibility and compression set resistance is prepared.
In summary, the application has the following beneficial effects:
1. According to the ethylene propylene diene monomer rubber sealing ring, ethylene propylene diene monomer rubber, a silane grafted polyurethane elastomer and carboxyl-terminated liquid nitrile rubber are used as a rubber system, and a filler, a dispersing agent, an accelerator and a vulcanizing agent are compounded, wherein the silane grafted polyurethane elastomer is prepared by reacting pentaerythritol triallyl ether, triethylene glycol diacrylate, a silane coupling agent, diisocyanate and a catalyst, the prepared silane grafted polyurethane elastomer has an interweaved reticular molecular structure, the dispersion uniformity of the filler in the rubber system can be improved, meanwhile, the temperature resistance, the flexibility and the compression set resistance of the prepared sealing ring can be improved, and the prepared ethylene propylene diene monomer rubber sealing ring can be used in a state of long-term compression and is stable in sealing.
2. The hydrogenated castor oil and the polytrimethylene ether glycol with the preferable dosage ratio can further improve the vulcanization crosslinking degree of the rubber system, and further improve the flexibility and compression set resistance of the prepared sealing ring.
3. According to the preparation method, the ethylene propylene diene monomer rubber sealing ring with stable performance is prepared by firstly mixing the raw materials, cooling after mixing, adding the accelerator and the vulcanizing agent, tabletting and cutting into a preformed sheet, vulcanizing and forming the preformed sheet, forming the shape of the sealing ring in the vulcanizing and forming process, and then punching and removing leftover materials.
Detailed Description
The present application will be described in further detail with reference to examples.
The following are sources and specifications of some of the raw materials of the present application, and the raw materials used in the preparation examples and examples of the present application are commercially available, including but not limited to the following types and manufacturers of raw materials, and raw materials with equivalent properties may be used:
1. ethylene propylene diene monomer 10950C;
2. carboxyl-terminated liquid nitrile rubber: gram, CAS:25265-19-4, nitrile rubber (CTBN);
3. carbon black, namely carbopol reinforcing carbon black N550;
4. White carbon black, namely cabot TS-530;
5. calcium carbonate, namely light calcium carbonate, 800-1250 meshes;
6. talcum powder of 800-1250 mesh;
7. hydrogenated castor oil, basf CO40;
8. polytrimethylene ether glycol, korea SK ECOPROL H2700;
9. DPTT, dipentamethylenethiuram tetrasulfide, CAS number 120-54-7;
10. CBS-80: ai Kem pre-dispersed masterbatch;
11. TT-80, rubber accelerator, chemical, tetrabenzyl thiuram disulfide;
12. BZ-80, rubber accelerator, lu Chuan chemical industry, 80% zinc di-n-butyl dithiocarbamate, 20% polymer and dispersant mixture;
13. s-80 French MLPC S-80 vulcanizing agent.
Preparation example of silane grafted polyurethane elastomer
Preparation example 1
Preparation example 1 discloses a silane grafted polyurethane elastomer, which is prepared by the following steps:
a1, adding 6kg of hexamethylene diisocyanate serving as diisocyanate, 2.4kg of pentaerythritol triallyl ether and 0.4kg of triethylene glycol diacrylate into a reaction kettle, heating to 40 ℃, mixing for 30min, and uniformly mixing to obtain a mixture A;
A2, adding 1kg of vinyl trimethoxy silane serving as a silane coupling agent and a catalyst consisting of 0.05kg of dibutyltin dilaurate and 0.05kg of dimethylamine into the mixture A, heating to 80 ℃ under the vacuumizing condition of-0.08 MPa, and reacting for 1h to obtain the silane grafted polyurethane elastomer.
PREPARATION EXAMPLES 2-3
Preparation examples 2 to 3 differ from preparation example 1 in the amounts of raw materials and the preparation conditions, see in particular Table 1 below.
TABLE 1 raw materials amounts and preparation conditions of preparation examples 1 to 3
Preparation example 4
Preparation example 4 differs from preparation example 2 in that the silane coupling agent in preparation example 4 is composed of a vinyl silane coupling agent and a long-chain alkyl silane coupling agent in a weight ratio of 1:0.2, the vinyl silane coupling agent is vinyl triisopropoxy silane, the long-chain alkyl silane coupling agent is dodecyl trimethoxy silane, and the other is the same as preparation example 2.
Preparation example 5
Preparation example 5 differs from preparation example 2 in that the silane coupling agent is composed of a vinyl silane coupling agent and a long-chain alkyl silane coupling agent in a weight ratio of 1:0.5, the vinyl silane coupling agent is vinyl trimethoxy silane, the long-chain alkyl silane coupling agent is hexadecyl triethoxy silane, and the other is the same as preparation example 2.
Preparation of comparative example 1
Preparation example 1 was different from preparation example 1 in that pentaerythritol triallyl ether was replaced with triethylene glycol diacrylate in equal amount, and the other was the same as in preparation example 1.
Preparation of comparative example 2
Comparative preparation 2 differs from preparation 1 in that triethylene glycol diacrylate was replaced with hydroxyethyl acrylate in equal amounts, and the other is the same as preparation 1.
Preparation of comparative example 3
Preparation example 3 is different from preparation example 1 in that pentaerythritol triallyl ether and triethylene glycol diacrylate are replaced with polyether triol (Acomat, TO 330) in equal amounts, and the other is the same as preparation example 1.
Examples
Example 1
Embodiment 1 discloses an ethylene propylene diene monomer rubber sealing ring, which is prepared by the following steps:
S1, mixing 6kg of ethylene propylene diene monomer rubber, 2kg of silane grafted polyurethane elastomer prepared in preparation example 1, 0.8kg of carboxyl-terminated liquid nitrile rubber, 3.5kg of carbon black serving as a filler, 1kg of No. 26 liquid paraffin serving as a plasticizer and 0.5kg of 1, 4-butanediol serving as a dispersing agent at 160 ℃ for 1h to prepare a mixed material I;
s2, after cooling to 89 ℃, adding 0.3kgDPTT serving as an accelerator and 0.1kg of a double-di-penta vulcanizing agent to carry out mixing, mixing for 30min, tabletting and cutting to obtain a pre-tabletting with the thickness of 3 mm;
s3, using a plate molding vulcanizing machine, performing compression molding vulcanization molding on the pre-manufactured sheet at a compression molding temperature of 170 ℃ for 25 seconds, and then performing punching to obtain the sealing ring with the outer diameter of 12.8mm, the inner diameter of 10.6mm and the thickness of 0.8 mm.
Examples 2 to 3
Examples 2-3 differ from example 1 in the amount of raw materials, the preparation conditions and the source of the silane-grafted polyurethane elastomer, see in particular Table 2 below.
TABLE 2 raw materials amounts, preparation conditions and sources of silane-grafted polyurethane elastomer for examples 1-3
Example 4
Example 4 differs from example 2 in that the silane-grafted polyurethane elastomer originates from preparation example 4, the remainder being identical to example 2.
Example 5
Example 5 differs from example 2 in that the silane-grafted polyurethane elastomer originates from preparation 5, the remainder being identical to example 2.
Example 6
Example 6 differs from example 2 in that the dispersant consists of hydrogenated castor oil and polytrimethylene ether glycol in a weight ratio of 1:0.2, the remainder being the same as in example 2.
Example 7
Example 7 differs from example 2 in that the dispersant consists of hydrogenated castor oil and polytrimethylene ether glycol in a weight ratio of 1:0.8, the remainder being the same as example 2.
Comparative example
Comparative examples 1 to 3
Comparative examples 1-3 differ from example 1 in the source of the silane-grafted polyurethane elastomer, see in particular Table 3 below.
Table 3 Source list of silane-grafted polyurethane elastomers of comparative examples 1-3
| Comparative example | Source list of silane grafted polyurethane elastomer |
| Comparative example 1 | Preparation of comparative example 1 |
| Comparative example 2 | Preparation of comparative example 2 |
| Comparative example 3 | Preparation of comparative example 3 |
Comparative example 4
Comparative example 4 differs from example 1 in that the dispersant was replaced with the silane-grafted polyurethane elastomer in equal amounts, the other being the same as in example 1.
Comparative example 5
Comparative example 5 differs from example 1 in that the silane-grafted polyurethane elastomer was replaced by an equivalent amount of a carboxyl-terminated liquid nitrile rubber, the other being the same as in example 1.
Performance test
The ethylene propylene diene monomer rubber seal rings prepared in examples 1 to 7 and comparative examples 1 to 5 were subjected to performance test as follows:
(1) Hardness test
According to the testing method in GB/T531.1-2008, testing the hardness (unit: shore A) of the prepared ethylene propylene diene monomer rubber sealing ring, and testing and recording the testing result;
(2) Resistance to permanent compression set:
a) Testing at normal temperature (23+ -2deg.C) for 360h according to the test method in GB/T1683-2018, testing and recording compression set (unit:%);
b) The compression set (unit:%) was tested and recorded according to the test method in GB/T1683-2018 for 360 hours at a temperature of 200 ℃ and a humidity of 85%;
The following are the performance test data of the ethylene propylene diene monomer rubber seal rings prepared in examples 1-7 and comparative examples 1-5, see in particular Table 4 below.
Table 4 table of performance test data for ethylene propylene diene monomer rubber seal rings prepared in examples 1-7 and comparative examples 1-5.
By combining examples 1-3 with comparative examples 1-3 and comparative example 5 with 4, it can be seen that the ethylene propylene diene monomer rubber sealing ring prepared by using the silane grafted polyurethane elastomer prepared by the application has moderate hardness and good compression deformation resistance, and when the ethylene propylene diene monomer rubber, the silane grafted polyurethane elastomer and the carboxyl-terminated liquid nitrile rubber are compounded for use, good synergistic effect can be generated, the compression resistance of the prepared ethylene propylene diene monomer rubber sealing ring is good, the performance of the prepared ethylene propylene diene monomer rubber sealing ring is obviously reduced by compounding the ethylene propylene diene monomer rubber, the silane grafted polyurethane elastomer and the carboxyl-terminated liquid nitrile rubber in comparative example 5, and the performance of the prepared ethylene propylene diene monomer rubber sealing ring prepared by not using pentaerythritol triallyl ether, triethylene glycol diacrylate, a silane coupling agent, diisocyanate and the silane grafted polyurethane elastomer prepared by reacting a catalyst is also reduced.
As can be seen from the combination of examples 1-3 and examples 4-5 and Table 4, the silane-grafted polyurethane elastomer prepared by using the vinyl silane coupling agent and the long-chain alkyl silane coupling agent in the preferred proportions of the present application has better performance.
By combining examples 1-5 with examples 6-7 and comparative example 4 and combining table 4, it can be seen that the vulcanization crosslinking density of the prepared ethylene propylene diene monomer rubber sealing ring can be further improved and the performance of the prepared ethylene propylene diene monomer rubber sealing ring can be improved by compounding hydrogenated castor oil and polytrimethylene ether glycol in a better proportion.
The present embodiment is only for explanation of the present application and is not to be construed as limiting the present application, and modifications to the present embodiment, which may not creatively contribute to the present application as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present application.
Claims (6)
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| CN104169353A (en) * | 2012-03-19 | 2014-11-26 | Sika技术股份公司 | Composition based on silane-terminated polymers |
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| EP0919582A4 (en) * | 1997-06-17 | 2004-12-29 | Konishi Co Ltd | Process for the preparation of urethane resins and urethane resin compositions |
| JP2016104834A (en) * | 2014-12-01 | 2016-06-09 | 株式会社カネカ | Modified thermoplastic urethane elastomer modified by core shell polymer |
| CN110527134B (en) * | 2019-08-23 | 2022-06-24 | 江苏大毛牛新材料有限公司 | Rubber sheet coated with silica aerogel coating and preparation process thereof |
| CN113563588A (en) * | 2021-07-28 | 2021-10-29 | 北京化工大学 | Hydroxyl-terminated siloxane, silicon polyurethane containing same and preparation method thereof |
| CN113881148A (en) * | 2021-09-24 | 2022-01-04 | 安徽京鸿密封件技术有限公司 | Low-compression permanent-deformation sulfur-vulcanized sealing ring ethylene propylene diene monomer rubber material |
| CN117004142B (en) * | 2023-08-18 | 2024-03-19 | 东莞市博恩密封技术有限公司 | High-low temperature compression deformation resistant EPDM rubber and preparation method thereof |
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| CN104423164A (en) * | 2013-08-30 | 2015-03-18 | 富士胶片株式会社 | Resin Composition For Laser Engraving, Process For Producing Flexographic Printing Plate Precursor For Laser Engraving, Flexographic Printing Plate Precursor, And Flexographic Printing Plate |
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