CN105111640A - High-elasticity compression permanent set-resistant fluororubber gasket and preparation method therefor - Google Patents
High-elasticity compression permanent set-resistant fluororubber gasket and preparation method therefor Download PDFInfo
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Abstract
The present invention discloses a high-elasticity compression permanent set-resistant fluororubber gasket which comprises the raw materials in parts by weight: 40-60 parts of modified fluoro rubber, 30-40 parts of a copolymer of hexafluoropropene and tetrafluoroethylene, 20-30 parts of methyl phenyl vinyl silicone rubber, 7-15 parts of carbon black, 5-18 parts of nano silicon dioxide, 10-20 parts of clay,14-19 parts of barium sulphate, 8-14 parts of organobentonite, 0.5-0.9 part of 1,4-bis(tert butyl) perox diisopropylbenzene, 1-1.9 parts of dicumyl peroxide, 0.2-0.6 part of magnesium hydroxide, 1-4 parts of hydroxy fluorosilicone oil, 1.5-2.5 parts of polydimethylsiloxane, 1-2 parts of triallyl isocyanurate, 1-3 parts of polyethylene wax, 1-3 parts of stearic acid, 1-2 parts of asphalt and 1-2 parts of glycidyl ether. The present invention further discloses a preparation method for the high-elasticity compression permanent set-resistant fluororubber gasket. According to the present invention, the fluororubber gasket is good in elasticity, good in compression permanent set resistance, simple in preparation method and convenient in actual operation.
Description
Technical field
The present invention relates to fluororubber pad technical field, particularly relate to a kind of high elastic pressure compression permanent deformation fluororubber pad and preparation method thereof.
Background technology
Synthesis macromolecular elastomer containing fluorine atom on the carbon atom that viton refers to main chain or side chain.Viton has the characteristic that high temperature resistant, oil resistant and resistant to many pharmaceutical chemicals corrode, and is the indispensable materials of top science technology such as modern Aviation, guided missile, rocket, space travel.But the requirement of automobile pad to viton is now higher, such as requires higher elasticity and resistance to permanent compression set.
Summary of the invention
The present invention proposes a kind of high elastic pressure compression permanent deformation fluororubber pad and preparation method thereof, good springiness, resistance to permanent compression set is good, and preparation method is simple, is convenient to actually operating.
A kind of high elastic pressure compression permanent deformation fluororubber pad that the present invention proposes, its raw material comprises by weight: modification viton 40-60 part, multipolymer 30-40 part of R 1216 and tetrafluoroethylene, methyl phenyl vinyl silicone rubber 20-30 part, carbon black 7-15 part, nano silicon 5-18 part, clay 10-20 part, barium sulfate 14-19 part, organobentonite 8-14 part, 1, 4-dual-tert-butyl peroxide diisopropyl benzene 0.5-0.9 part, dicumyl peroxide 1-1.9 part, magnesium hydroxide 0.2-0.6 part, hydroxy terminated fluorosilicone oil 1-4 part, polydimethylsiloxane 1.5-2.5 part, cyanacrylate 1-2 part, polyethylene wax 1-3 part, stearic acid 1-3 part, pitch 1-2 part, glycidyl ether 1-2 part.
Preferably, described modification viton adopts following technique to prepare: by weight by 100 parts of water, 1-2 part ammonium perfluorocaprylate and 0.5-2.5 part sodium bicarbonate mix and then add 30-60 part vinylidene and mix, add 0.02-0.09 part ammonium persulphate to be polymerized, polymerization reaction time is 20-50min, add 1-4 part methyl tertbutyl ketone and stir 15-40min, continue to add 5-18 part trifluoro polyethylene to be polymerized, polymerization pressure is 0.2-0.9MPa, polymeric reaction temperature is 110-120 DEG C, polymerization time is 15-35min, cohesion, washing, dry, plasticate and shapingly obtain modification viton.
Preferably, the weight ratio of vinylidene, trifluoro polyethylene and methyl tertbutyl ketone is 50-56:10-14:3-3.6.
Preferably, the multipolymer of modification viton, R 1216 and tetrafluoroethylene and the weight ratio of methyl phenyl vinyl silicone rubber are 50-56:32-34:22-25.
Preferably, carbon black, nano silicon, clay, barium sulfate and bentonite weight ratio are 8-10:10-14:16-18:15-16 part 10-12.
Preferably, the weight ratio of Isosorbide-5-Nitrae-dual-tert-butyl peroxide diisopropyl benzene, dicumyl peroxide and cyanacrylate is 0.6-0.8:1.2-1.4:1.4-1.6.
Preferably, its raw material comprises by weight: modification viton 50-56 part, multipolymer 32-34 part of R 1216 and tetrafluoroethylene, methyl phenyl vinyl silicone rubber 22-25 part, carbon black 8-10 part, nano silicon 10-14 part, clay 16-18 part, barium sulfate 15-16 part, organobentonite 10-12 part, 1, 4-dual-tert-butyl peroxide diisopropyl benzene 0.6-0.8 part, dicumyl peroxide 1.2-1.4 part, magnesium hydroxide 0.4-0.5 part, hydroxy terminated fluorosilicone oil 2-3.4 part, polydimethylsiloxane 2-2.2 part, cyanacrylate 1.4-1.6 part, polyethylene wax 2-2.4 part, stearic acid 1.5-2.3 part, pitch 1.4-1.6 part, glycidyl ether 1.4-1.5 part.
The invention allows for a kind of preparation technology of high elastic pressure compression permanent deformation fluororubber pad, comprise the steps:
S1, carbon black, nano silicon, clay, barium sulfate, organobentonite, hydroxy terminated fluorosilicone oil, polydimethylsiloxane are sent in mill and mixed, mixing temperature is 60-68 DEG C, and mixing time is 30-60min, thin-pass 2-4 time, slice, obtains the first prefabricated material;
S2, the multipolymer of modification viton, R 1216 and tetrafluoroethylene, methyl phenyl vinyl silicone rubber are sent into mill mixing, melting temperature is 70-80 DEG C, mixing time is 15-30min, raised temperature is to 85-92 DEG C, add magnesium hydroxide mixing, mixing time is 15-30min, and bag roller obtains the second prefabricated material;
S3, under whipped state, the first prefabricated material is added in the second prefabricated material, adding speed is 0.5-1.8 part/min, add completely and continue to stir 15-20min, continue to add 1,4-dual-tert-butyl peroxide diisopropyl benzene, dicumyl peroxide, cyanacrylate, polyethylene wax, stearic acid, pitch, glycidyl ether are mixing, melting temperature is 90-94 DEG C, and mixing time is 15-30min, obtains the 3rd prefabricated material;
S4, the 3rd prefabricated material is sent into sulfuration in vulcanizer, curing temperature is 120-150 DEG C, and curing time is 5-15min, and send in baking oven and heat, Heating temperature is 160-180 DEG C, and heat-up time is 20-40min, obtains viton diaphragm seal.
In the present invention, with the multipolymer of modification viton, R 1216 and tetrafluoroethylene, methyl phenyl vinyl silicone rubber and for major ingredient, good springiness, resistance to permanent compression set is good; In the preparation process of modification viton, using vinylidene and trifluoro polyethylene as polymerization single polymerization monomer, using ammonium persulphate as initiator, and add appropriate methyl tertbutyl ketone, and the conservative control joining day with add rear stirring extent and effectively can regulate the molecular size range of product, by limiting the molecular structure after vinylidene and trifluoro polyethylene polymerization, and on molecular chain, introduce methyl tertbutyl ketone, resistance to permanent compression set is good, and good processability, not easily produce trace during sulfuration; Adopt 1,4-dual-tert-butyl peroxide diisopropyl benzene, dicumyl peroxide and cyanacrylate are as vulcanization system, cyanacrylate effectively can assist crosslinking reaction, improve cross-linking efficiency, make sizing material have good incipient scorch simultaneously, adopt the goods elasticity of this vulcanization system, under high temperature, compression set resistant is good; Adopt carbon black, nano silicon, clay, barium sulfate and organobentonite as reinforcing and filling system, there is high fillibility, and goods wear resistance is good, product can be made to have heat-resisting, oil resistant, low compression deformation rate, high resilience and low delayed feature; The magnesium hydroxide added, polyethylene wax, stearic acid, pitch, glycidyl ether, with base-material, there is good consistency, possess high lubricant effect, it effectively can improve the mobility of sizing material, viscosity and release property, and elasticity and resistance to permanent compression set strengthen further.
Accompanying drawing explanation
Fig. 1 is preparation technology's schema of a kind of high elastic pressure compression permanent deformation fluororubber pad that the present invention proposes.
Embodiment
As shown in Figure 1, Fig. 1 is preparation technology's schema of a kind of high elastic pressure compression permanent deformation fluororubber pad that the present invention proposes.
Below, by specific embodiment, technical scheme of the present invention is described in detail.
Embodiment 1
A kind of high elastic pressure compression permanent deformation fluororubber pad, its raw material comprises by weight: modification viton 60 parts, the multipolymer of R 1216 and tetrafluoroethylene 30 parts, methyl phenyl vinyl silicone rubber 28 parts, carbon black 7 parts, nano silicon 18 parts, clay 10 parts, 18.6 parts, barium sulfate, organobentonite 8 parts, 1, 4-dual-tert-butyl peroxide diisopropyl benzene 0.9 part, dicumyl peroxide 1 part, magnesium hydroxide 0.45 part, hydroxy terminated fluorosilicone oil 1 part, polydimethylsiloxane 2.5 parts, cyanacrylate 1 part, polyethylene wax 2.8 parts, stearic acid 1 part, pitch 2 parts, glycidyl ether 1 part.
Embodiment 2
A kind of high elastic pressure compression permanent deformation fluororubber pad, its raw material comprises by weight: modification viton 40 parts, the multipolymer of R 1216 and tetrafluoroethylene 40 parts, methyl phenyl vinyl silicone rubber 21 parts, carbon black 15 parts, nano silicon 5 parts, clay 20 parts, 14.2 parts, barium sulfate, organobentonite 14 parts, 1, 4-dual-tert-butyl peroxide diisopropyl benzene 0.5 part, dicumyl peroxide 1.9 parts, magnesium hydroxide 0.32 part, hydroxy terminated fluorosilicone oil 4 parts, polydimethylsiloxane 1.5 parts, cyanacrylate 2 parts, polyethylene wax 1.2 parts, stearic acid 3 parts, pitch 1 part, glycidyl ether 2 parts.
Embodiment 3
A kind of high elastic pressure compression permanent deformation fluororubber pad, its raw material comprises by weight: modification viton 56 parts, the multipolymer of R 1216 and tetrafluoroethylene 32 parts, methyl phenyl vinyl silicone rubber 25 parts, carbon black 8 parts, nano silicon 14 parts, clay 16 parts, 16 parts, barium sulfate, organobentonite 10 parts, 1, 4-dual-tert-butyl peroxide diisopropyl benzene 0.8 part, dicumyl peroxide 1.2 parts, magnesium hydroxide 0.5 part, hydroxy terminated fluorosilicone oil 2 parts, polydimethylsiloxane 2.178 parts, cyanacrylate 1.4 parts, polyethylene wax 2.4 parts, stearic acid 1.5 parts, pitch 1.58 parts, glycidyl ether 1.4 parts.
Described modification viton adopts following technique to prepare: 100 parts of water, 2 parts of ammonium perfluorocaprylates and 0.5 part of sodium bicarbonate are mixed by weight and then add 59 parts of vinylidenes and mix, add 0.02 part of ammonium persulphate to be polymerized, polymerization reaction time is 50min, add 1 part of methyl tertbutyl ketone and stir 36min, continue to add 5 parts of trifluoro polyethylene to be polymerized, polymerization pressure is 0.9MPa, polymeric reaction temperature is 110 DEG C, polymerization time is 32min, cohesion, washing, dry, plasticating shapingly obtains modification viton.
With reference to Fig. 1, the preparation technology of described high elastic pressure compression permanent deformation fluororubber pad, comprises the steps:
S1, carbon black, nano silicon, clay, barium sulfate, organobentonite, hydroxy terminated fluorosilicone oil, polydimethylsiloxane are sent in mill and mixed, mixing temperature is 60 DEG C, and mixing time is 60min, thin-pass 2 times, and slice obtains the first prefabricated material;
S2, the multipolymer of modification viton, R 1216 and tetrafluoroethylene, methyl phenyl vinyl silicone rubber are sent into mill mixing, melting temperature is 78 DEG C, mixing time is 15min, raised temperature to 92 DEG C, add magnesium hydroxide mixing, mixing time is 15min, and bag roller obtains the second prefabricated material;
S3, under whipped state, the first prefabricated material is added in the second prefabricated material, adding speed is 1.75 parts/min, add completely and continue to stir 15min, continue to add 1,4-dual-tert-butyl peroxide diisopropyl benzene, dicumyl peroxide, cyanacrylate, polyethylene wax, stearic acid, pitch, glycidyl ether are mixing, melting temperature is 94 DEG C, and mixing time is 15min, obtains the 3rd prefabricated material;
S4, the 3rd prefabricated material is sent into sulfuration in vulcanizer, curing temperature is 148 DEG C, and curing time is 5min, and send in baking oven and heat, Heating temperature is 180 DEG C, and heat-up time is 20min, obtains viton diaphragm seal.
Embodiment 4
A kind of high elastic pressure compression permanent deformation fluororubber pad, its raw material comprises by weight: modification viton 50 parts, the multipolymer of R 1216 and tetrafluoroethylene 34 parts, methyl phenyl vinyl silicone rubber 22 parts, carbon black 10 parts, nano silicon 10 parts, clay 18 parts, 15 parts, barium sulfate, organobentonite 12 parts, 1, 4-dual-tert-butyl peroxide diisopropyl benzene 0.6 part, dicumyl peroxide 1.4 parts, magnesium hydroxide 0.4 part, hydroxy terminated fluorosilicone oil 3.4 parts, polydimethylsiloxane 2 parts, cyanacrylate 1.6 parts, polyethylene wax 2 parts, stearic acid 2.3 parts, pitch 1.4 parts, glycidyl ether 1.5 parts.
Described modification viton adopts following technique to prepare: 100 parts of water, 1 part of ammonium perfluorocaprylate and 2.5 parts of sodium bicarbonates are mixed by weight and then add 30 parts of vinylidenes and mix, add 0.09 part of ammonium persulphate to be polymerized, polymerization reaction time is 20min, add 4 parts of methyl tertbutyl ketone and stir 15min, continue to add 18 parts of trifluoro polyethylene to be polymerized, polymerization pressure is 0.2MPa, polymeric reaction temperature is 120 DEG C, polymerization time is 15min, cohesion, washing, dry, plasticating shapingly obtains modification viton.
The preparation technology of described high elastic pressure compression permanent deformation fluororubber pad, comprises the steps:
S1, carbon black, nano silicon, clay, barium sulfate, organobentonite, hydroxy terminated fluorosilicone oil, polydimethylsiloxane are sent in mill and mixed, mixing temperature is 68 DEG C, and mixing time is 30min, thin-pass 4 times, and slice obtains the first prefabricated material;
S2, the multipolymer of modification viton, R 1216 and tetrafluoroethylene, methyl phenyl vinyl silicone rubber are sent into mill mixing, melting temperature is 70 DEG C, mixing time is 30min, raised temperature to 85 DEG C, add magnesium hydroxide mixing, mixing time is 30min, and bag roller obtains the second prefabricated material;
S3, under whipped state, the first prefabricated material is added in the second prefabricated material, adding speed is 0.5 part/min, add completely and continue to stir 20min, continue to add 1,4-dual-tert-butyl peroxide diisopropyl benzene, dicumyl peroxide, cyanacrylate, polyethylene wax, stearic acid, pitch, glycidyl ether are mixing, melting temperature is 90 DEG C, and mixing time is 30min, obtains the 3rd prefabricated material;
S4, the 3rd prefabricated material is sent into sulfuration in vulcanizer, curing temperature is 120 DEG C, and curing time is 15min, and send in baking oven and heat, Heating temperature is 160 DEG C, and heat-up time is 40min, obtains viton diaphragm seal.
Embodiment 5
A kind of high elastic pressure compression permanent deformation fluororubber pad, its raw material comprises by weight: modification viton 52 parts, the multipolymer of R 1216 and tetrafluoroethylene 33 parts, methyl phenyl vinyl silicone rubber 24 parts, carbon black 9 parts, nano silicon 12 parts, clay 17.4 parts, 15.2 parts, barium sulfate, organobentonite 11.5 parts, 1, 4-dual-tert-butyl peroxide diisopropyl benzene 0.75 part, dicumyl peroxide 1.32 parts, magnesium hydroxide 0.46 part, hydroxy terminated fluorosilicone oil 3.2 parts, polydimethylsiloxane 2.15 parts, cyanacrylate 1.52 parts, polyethylene wax 2.2 parts, stearic acid 2.1 parts, pitch 1.5 parts, glycidyl ether 1.46 parts.
Described modification viton adopts following technique to prepare: 100 parts of water, 1.6 parts of ammonium perfluorocaprylates and 2.1 parts of sodium bicarbonates are mixed by weight and then add 55 parts of vinylidenes and mix, add 0.06 part of ammonium persulphate to be polymerized, polymerization reaction time is 42min, add 2.6 parts of methyl tertbutyl ketone and stir 32min, continue to add 12 parts of trifluoro polyethylene to be polymerized, polymerization pressure is 0.64MPa, polymeric reaction temperature is 116 DEG C, polymerization time is 21min, cohesion, washing, dry, plasticating shapingly obtains modification viton.
The preparation technology of described high elastic pressure compression permanent deformation fluororubber pad, comprises the steps:
S1, carbon black, nano silicon, clay, barium sulfate, organobentonite, hydroxy terminated fluorosilicone oil, polydimethylsiloxane are sent in mill and mixed, mixing temperature is 64 DEG C, and mixing time is 55min, thin-pass 3 times, and slice obtains the first prefabricated material;
S2, the multipolymer of modification viton, R 1216 and tetrafluoroethylene, methyl phenyl vinyl silicone rubber are sent into mill mixing, melting temperature is 76 DEG C, mixing time is 24min, raised temperature to 91 DEG C, add magnesium hydroxide mixing, mixing time is 24min, and bag roller obtains the second prefabricated material;
S3, under whipped state, the first prefabricated material is added in the second prefabricated material, adding speed is 1.4 parts/min, add completely and continue to stir 18min, continue to add 1,4-dual-tert-butyl peroxide diisopropyl benzene, dicumyl peroxide, cyanacrylate, polyethylene wax, stearic acid, pitch, glycidyl ether are mixing, melting temperature is 92 DEG C, and mixing time is 24min, obtains the 3rd prefabricated material;
S4, the 3rd prefabricated material is sent into sulfuration in vulcanizer, curing temperature is 145 DEG C, and curing time is 12min, and send in baking oven and heat, Heating temperature is 172 DEG C, and heat-up time is 36min, obtains viton diaphragm seal.
The above; be only the present invention's preferably embodiment; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.
Claims (8)
1. a high elastic pressure compression permanent deformation fluororubber pad, it is characterized in that, its raw material comprises by weight: modification viton 40-60 part, multipolymer 30-40 part of R 1216 and tetrafluoroethylene, methyl phenyl vinyl silicone rubber 20-30 part, carbon black 7-15 part, nano silicon 5-18 part, clay 10-20 part, barium sulfate 14-19 part, organobentonite 8-14 part, 1, 4-dual-tert-butyl peroxide diisopropyl benzene 0.5-0.9 part, dicumyl peroxide 1-1.9 part, magnesium hydroxide 0.2-0.6 part, hydroxy terminated fluorosilicone oil 1-4 part, polydimethylsiloxane 1.5-2.5 part, cyanacrylate 1-2 part, polyethylene wax 1-3 part, stearic acid 1-3 part, pitch 1-2 part, glycidyl ether 1-2 part.
2. high elastic pressure compression permanent deformation fluororubber pad according to claim 1, it is characterized in that, described modification viton adopts following technique to prepare: by weight by 100 parts of water, 1-2 part ammonium perfluorocaprylate and 0.5-2.5 part sodium bicarbonate mix and then add 30-60 part vinylidene and mix, add 0.02-0.09 part ammonium persulphate to be polymerized, polymerization reaction time is 20-50min, add 1-4 part methyl tertbutyl ketone and stir 15-40min, continue to add 5-18 part trifluoro polyethylene to be polymerized, polymerization pressure is 0.2-0.9MPa, polymeric reaction temperature is 110-120 DEG C, polymerization time is 15-35min, cohesion, washing, dry, plasticate and shapingly obtain modification viton.
3. high elastic pressure compression permanent deformation fluororubber pad according to claim 2, is characterized in that, the weight ratio of vinylidene, trifluoro polyethylene and methyl tertbutyl ketone is 50-56:10-14:3-3.6.
4. the high elastic pressure compression permanent deformation fluororubber pad according to any one of claim 1-3, it is characterized in that, the multipolymer of modification viton, R 1216 and tetrafluoroethylene and the weight ratio of methyl phenyl vinyl silicone rubber are 50-56:32-34:22-25.
5. the high elastic pressure compression permanent deformation fluororubber pad according to any one of claim 1-4, is characterized in that, carbon black, nano silicon, clay, barium sulfate and bentonite weight ratio are 8-10:10-14:16-18:15-16 part 10-12.
6. the high elastic pressure compression permanent deformation fluororubber pad according to any one of claim 1-5, it is characterized in that, the weight ratio of Isosorbide-5-Nitrae-dual-tert-butyl peroxide diisopropyl benzene, dicumyl peroxide and cyanacrylate is 0.6-0.8:1.2-1.4:1.4-1.6.
7. the high elastic pressure compression permanent deformation fluororubber pad according to any one of claim 1-6, it is characterized in that, its raw material comprises by weight: modification viton 50-56 part, multipolymer 32-34 part of R 1216 and tetrafluoroethylene, methyl phenyl vinyl silicone rubber 22-25 part, carbon black 8-10 part, nano silicon 10-14 part, clay 16-18 part, barium sulfate 15-16 part, organobentonite 10-12 part, 1, 4-dual-tert-butyl peroxide diisopropyl benzene 0.6-0.8 part, dicumyl peroxide 1.2-1.4 part, magnesium hydroxide 0.4-0.5 part, hydroxy terminated fluorosilicone oil 2-3.4 part, polydimethylsiloxane 2-2.2 part, cyanacrylate 1.4-1.6 part, polyethylene wax 2-2.4 part, stearic acid 1.5-2.3 part, pitch 1.4-1.6 part, glycidyl ether 1.4-1.5 part.
8. a preparation technology for the high elastic pressure compression permanent deformation fluororubber pad according to any one of claim 1-7, is characterized in that, comprise the steps:
S1, carbon black, nano silicon, clay, barium sulfate, organobentonite, hydroxy terminated fluorosilicone oil, polydimethylsiloxane are sent in mill and mixed, mixing temperature is 60-68 DEG C, and mixing time is 30-60min, thin-pass 2-4 time, slice, obtains the first prefabricated material;
S2, the multipolymer of modification viton, R 1216 and tetrafluoroethylene, methyl phenyl vinyl silicone rubber are sent into mill mixing, melting temperature is 70-80 DEG C, mixing time is 15-30min, raised temperature is to 85-92 DEG C, add magnesium hydroxide mixing, mixing time is 15-30min, and bag roller obtains the second prefabricated material;
S3, under whipped state, the first prefabricated material is added in the second prefabricated material, adding speed is 0.5-1.8 part/min, add completely and continue to stir 15-20min, continue to add 1,4-dual-tert-butyl peroxide diisopropyl benzene, dicumyl peroxide, cyanacrylate, polyethylene wax, stearic acid, pitch, glycidyl ether are mixing, melting temperature is 90-94 DEG C, and mixing time is 15-30min, obtains the 3rd prefabricated material;
S4, the 3rd prefabricated material is sent into sulfuration in vulcanizer, curing temperature is 120-150 DEG C, and curing time is 5-15min, and send in baking oven and heat, Heating temperature is 160-180 DEG C, and heat-up time is 20-40min, obtains viton diaphragm seal.
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| CN109385095A (en) * | 2018-09-30 | 2019-02-26 | 东莞市臻邦新材料科技有限公司 | A kind of high thermal conductivity springs back by force silica gel pad and preparation method thereof |
| CN114805965A (en) * | 2022-04-28 | 2022-07-29 | 绍兴华运输送设备有限公司 | Permanent compression resistant sealing ring for carrier roller and preparation method thereof |
| CN114805965B (en) * | 2022-04-28 | 2023-09-05 | 绍兴华运输送设备有限公司 | Permanent compression-resistant sealing ring for carrier roller and preparation method thereof |
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