CN112852075A - Low-permeability fluororubber product material - Google Patents
Low-permeability fluororubber product material Download PDFInfo
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- CN112852075A CN112852075A CN202110148766.4A CN202110148766A CN112852075A CN 112852075 A CN112852075 A CN 112852075A CN 202110148766 A CN202110148766 A CN 202110148766A CN 112852075 A CN112852075 A CN 112852075A
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- 229920001973 fluoroelastomer Polymers 0.000 title claims abstract description 57
- 239000000463 material Substances 0.000 title claims abstract description 40
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 113
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 111
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical class S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 57
- 239000006229 carbon black Substances 0.000 claims abstract description 50
- 229920001971 elastomer Polymers 0.000 claims abstract description 40
- 229920003051 synthetic elastomer Polymers 0.000 claims abstract description 40
- 239000005061 synthetic rubber Substances 0.000 claims abstract description 40
- 239000005060 rubber Substances 0.000 claims abstract description 39
- 238000002360 preparation method Methods 0.000 claims abstract description 31
- 238000004073 vulcanization Methods 0.000 claims abstract description 25
- 239000011256 inorganic filler Substances 0.000 claims abstract description 17
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 17
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 239000000378 calcium silicate Substances 0.000 claims abstract description 15
- 229910052918 calcium silicate Inorganic materials 0.000 claims abstract description 15
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 claims abstract description 15
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 8
- 239000000920 calcium hydroxide Substances 0.000 claims abstract description 8
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims abstract description 8
- 238000001514 detection method Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 8
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 8
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000465 moulding Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 50
- 239000007822 coupling agent Substances 0.000 claims description 44
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 32
- 235000019441 ethanol Nutrition 0.000 claims description 30
- 238000001035 drying Methods 0.000 claims description 28
- 239000007787 solid Substances 0.000 claims description 28
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 28
- 230000003712 anti-aging effect Effects 0.000 claims description 25
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 21
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 19
- 239000011737 fluorine Substances 0.000 claims description 19
- 229910052731 fluorine Inorganic materials 0.000 claims description 19
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 19
- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical compound CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 14
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 14
- 239000006185 dispersion Substances 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 14
- 239000000725 suspension Substances 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- 238000005303 weighing Methods 0.000 claims description 14
- 230000035699 permeability Effects 0.000 claims description 8
- 229910052582 BN Inorganic materials 0.000 claims description 7
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 239000006057 Non-nutritive feed additive Substances 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 7
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 7
- 239000010439 graphite Substances 0.000 claims description 7
- 229910002804 graphite Inorganic materials 0.000 claims description 7
- 238000007689 inspection Methods 0.000 claims description 7
- 238000003801 milling Methods 0.000 claims description 7
- 239000002048 multi walled nanotube Substances 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 125000005375 organosiloxane group Chemical group 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 238000000967 suction filtration Methods 0.000 claims description 7
- 238000009966 trimming Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000004408 titanium dioxide Substances 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract description 9
- 230000006835 compression Effects 0.000 abstract description 3
- 238000007906 compression Methods 0.000 abstract description 3
- 238000000034 method Methods 0.000 abstract description 3
- 239000000446 fuel Substances 0.000 abstract description 2
- 239000000295 fuel oil Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 125000001153 fluoro group Chemical group F* 0.000 description 3
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000004513 sizing Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 230000035882 stress Effects 0.000 description 2
- 239000005909 Kieselgur Substances 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 241000872198 Serjania polyphylla Species 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000003831 antifriction material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000035 biogenic effect Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229920001059 synthetic polymer Polymers 0.000 description 1
- 229910052905 tridymite Inorganic materials 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
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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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
- C08K3/041—Carbon nanotubes
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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
- 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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- 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
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention discloses a low-permeability fluororubber product material which comprises the following raw materials in parts by weight: fluororubber, calcium silicate, magnesium oxide, calcium hydroxide, WS280, iron oxide red, modified molybdenum disulfide, nano inorganic filler, modified diatomite and modified white carbon black; preparation of synthetic rubber: feeding all the raw materials into an internal mixer according to the parts by weight, detecting the hardness, strength and elongation of the synthetic rubber obtained by the internal mixer, and filtering after detection; carrying out open mixing molding on the qualified synthetic rubber at 60-70 ℃ through an open mill, and then putting the molded rubber into a mold in vulcanization equipment to carry out vulcanization treatment on the rubber; the invention prepares the low-permeability fluororubber product material with excellent fluidity, improved demoulding performance, better methanol and ethanol fuel resistance and good compression stress relaxation through the procedures of preparation of synthetic rubber, molding and vulcanization of rubber, secondary vulcanization post-treatment and the like.
Description
Technical Field
The invention belongs to the technical field of fluororubber, and relates to a fluororubber product material, in particular to a low-permeability fluororubber product material.
Background
Fluororubbers are rubbers known to be resistant to alcoholic fuel oils. With the demand of social development, the 'national six' standard strictly controls the emission limit of pollutants, the two-day and night emission limit requirement in evaporative emission is reduced to 0.65 g from 2 g of the original 'national five', and the fuel oil permeability is required to be below 40g mm/m2 day. The domestic ternary fluorine glue with high fluorine content cannot meet the requirement; the home-made polyfluoro rubber sizing material with high fluorine content has poor manufacturability and low product percent of pass; the imported ternary fluorine rubber can meet the requirement of fuel oil permeability, but the material cost is twice as high as that of the domestic product. The invention provides a low-permeability fluororubber product material which has excellent fluidity, improved demolding performance, better methanol and ethanol fuel resistance and good compression stress relaxation, and is prepared by blending a rubber formula.
Disclosure of Invention
The invention aims to solve the problem that domestic ternary fluorine glue with high fluorine content cannot meet the requirement; the home-made polyfluoro rubber sizing material with high fluorine content has poor manufacturability and low product percent of pass; the imported ternary fluorine rubber can meet the requirement of fuel oil permeability, but the material cost is doubled compared with that of domestic products, so that the low-permeability fluorine rubber product material is provided.
The purpose of the invention can be realized by the following technical scheme:
a low-permeability fluororubber product material comprises the following raw materials in parts by weight: 84-90 parts of fluororubber, 4-6 parts of calcium silicate, 1.5-2.5 parts of magnesium oxide, 4-6 parts of calcium hydroxide, WS 280: 0.3-0.7 part of iron oxide red, 0.3-0.7 part of modified molybdenum disulfide, 12-18 parts of nano inorganic filler, 2-4 parts of modified diatomite and 2-4 parts of modified white carbon black;
the preparation process of the low-permeability fluororubber product material comprises the following steps:
the first step is as follows: preparation of synthetic rubber: feeding all the raw materials into an internal mixer according to the parts by weight, detecting the hardness, the strength and the elongation of the synthetic rubber obtained by the internal mixer, and filtering after detection, wherein the synthetic rubber with the hardness of 70 +/-5 degrees, the strength of more than or equal to 10MPa and the elongation of more than or equal to 175 percent is qualified synthetic rubber;
the second step is that: and (3) forming and vulcanizing rubber: the qualified synthetic rubber is processed by open milling and molding at 60-70 ℃ through an open mill, and then the molded rubber is put into a mold in vulcanization equipment under the pressure of 170-2And the temperature is 175-185 ℃, the rubber is vulcanized for 300 seconds at the vulcanization time of 240-;
the third step: post-treatment and inspection: trimming the vulcanized product, putting the trimmed product in an oven for secondary vulcanization at 230-250 ℃ for 8-16 h, and then inspecting the size and the appearance to obtain a qualified finished product.
Preferably, the fluorine content of the fluororubber is more than 70%; WS280 is an organosiloxane-based processing aid; the calcium silicate is surface treated with a siloxane.
Preferably, the preparation process of the modified molybdenum disulfide comprises the following steps: adding molybdenum disulfide and n-dodecyl mercaptan into 1-methyl-2-pyrrolidone, stirring and mixing, and performing ultrasonic dispersion for 1-2 hours to obtain a modified molybdenum disulfide suspension dispersion liquid; and carrying out reduced pressure suction filtration, washing and drying on the modified molybdenum disulfide suspension dispersion liquid to obtain the modified molybdenum disulfide.
Preferably, the mass ratio of the molybdenum disulfide, the n-dodecyl mercaptan and the 1-methyl-2-pyrrolidone is controlled to be 2.2-2.5:1.2-1.5: 20-22.
Preferably, the modified diatomite comprises the following steps:
weighing diatomite, putting the diatomite into a container, and putting the container into a constant-temperature water bath kettle at 90 ℃ for stirring and preheating; weighing the coupling agent in corresponding parts by weight, adding absolute ethyl alcohol for dissolving, and respectively dropwise adding the coupling agent into the diatomite under the condition of stirring at a low speed of 300 r/min; then the rotating speed of the stirrer is adjusted to 1500r/min, the mixture is stirred and reacted for 60min, and finally the modified diatomite is obtained after being taken out.
Preferably, the mass ratio of the diatomite to the coupling agent to the absolute ethyl alcohol is controlled to be 50-60:50-60: 300-350; the silane coupling agent is one or more of a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH 570.
Preferably, the preparation process of the modified white carbon black comprises the following steps:
the first step is as follows: adding white carbon black into 95% ethanol solution by mass percent and performing ultrasonic dispersion to obtain solution A; adding the anti-aging coupling agent into a 95% ethanol aqueous solution, and performing ultrasonic dispersion to obtain a solution B; mixing the solution A and the solution B and continuing to perform ultrasonic dispersion; refluxing the mixture for 2-3h under the protection of nitrogen, and spin-drying the solvent to obtain a solid;
the second step is that: drying the solid in a vacuum oven at 50-60 ℃ for 1-2 h; then washing the solid with absolute ethyl alcohol to remove the anti-aging coupling agent which is not grafted to the surface of the white carbon black; and then placing the cleaned solid in a vacuum oven for drying to obtain the modified white carbon black.
Preferably, the mass ratio of the white carbon black to the ethanol solution with the mass fraction of 95% is controlled to be 10-15: 50-60; the mass ratio of the anti-aging coupling agent to the 95% ethanol solution is controlled to be 6-8: 40-50.
Preferably, the nano inorganic filler comprises nano barium sulfate, hexagonal boron nitride, rutile titanium dioxide, multi-walled carbon nanotubes and graphite.
Compared with the prior art, the invention has the beneficial effects that:
the invention prepares a hyposmosis fluorine rubber product material with excellent fluidity, improved demoulding performance, better methanol and ethanol fuel oil resistance and good compression stress relaxation through the procedures of preparation of synthetic rubber, molding and vulcanization of rubber, secondary vulcanization post-treatment and the like;
molybdenum disulfide is added into the fluororubber as an anti-friction agent to improve the friction performance of the fluororubber; according to the invention, the molybdenum disulfide is modified by n-dodecyl mercaptan, so that the modifier is adhered to the surface of the molybdenum disulfide sheet, the dispersibility and stability of the molybdenum disulfide in the fluororubber product material are improved, the interaction among molybdenum disulfide sheet layers can be effectively weakened, and the phenomenon of agglomeration and stacking of the molybdenum disulfide can be avoided; the interaction between the molybdenum disulfide and polymer molecular chains is enhanced; thereby the fluororubber has excellent performance of reducing surface friction;
diatomaceous earth is a biogenic porous silicalite; the main component is amorphous silicon dioxide formed by the skeleton of unicellular diatom and has a chemical formula of SiO2nH 2O. Mineralogically belongs to opal-AG; the diatomite has a unique shell structure and has nano-scale micropores formed by macropores in a biological framework and gaps of silicon dioxide spheres, so that the diatomite has the properties of light weight, large specific surface area, strong adsorption performance and the like; because of the advantages of no toxicity, safety, good chemical stability and the like, the diatomite is an important nonmetallic mineral material; silane coupling agent exists on the surface of the diatomite, and chemical adsorption occurs between the surface of the diatomite particles and the silane coupling agent, so that a new Si-O-Si bond is formed; the tensile strength and the elongation at break of the low-permeability fluororubber product material are improved by adding the modified diatomite;
the anti-aging coupling agent is one or more of silane coupling agent Si69 and silane coupling agent Si 75. According to the invention, the surface modification is carried out on the white carbon black through the anti-aging coupling agent to obtain the white carbon black with the surface grafted with the anti-aging agent, and the strength and the tearing strength of the modified white carbon black are both greatly improved; the compatibility of the white carbon black and the rubber is improved, the anti-aging agent is prevented from volatilizing, and the modified white carbon black is applied to the low-permeability fluororubber product material to ensure that the low-permeability fluororubber product material has high thermal oxidation resistance, ozone resistance and damp-heat aging resistance; the method solves the problems that in the prior art, the surface of the white carbon black has a large amount of silicon hydroxyl groups, so that the white carbon black has acidity, hygroscopicity and hydrophilicity; therefore, when the white carbon is filled into the rubber, there is a problem that vulcanization is delayed and aggregates are formed in the rubber;
the nano inorganic filler can obviously prolong the positive vulcanization time of the fluororubber; when the hardness levels of vulcanized rubbers are the same, the nano inorganic filler has an obvious reinforcing effect on fluororubber; the fluororubber is a synthetic polymer elastomer containing fluorine atoms in the main chain or side chain carbon atoms. Because the C-F bond energy is large (485kJ/mol), and the covalent radius of fluorine atoms is 0.064nm, which is equivalent to half of the length of the C-C bond, the fluorine atoms can be tightly arranged around carbon atoms, and a strong shielding effect is generated on the C-C main chain of the polymer, so that the fluorine rubber is in overall chemical inertness, and the interface bonding strength between the fluorine rubber and the filler which is commonly used at present is low.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A low-permeability fluororubber product material comprises the following raw materials in parts by weight: 84 parts of fluororubber, 4 parts of calcium silicate, 1.5 parts of magnesium oxide, 4 parts of calcium hydroxide, WS 280: 0.3 part of iron oxide red, 0.3 part of modified molybdenum disulfide, 12 parts of nano inorganic filler, 2 parts of modified diatomite and 2 parts of modified white carbon black;
the preparation process of the low-permeability fluororubber product material comprises the following steps:
the first step is as follows: preparation of synthetic rubber: feeding all the raw materials into an internal mixer according to the parts by weight, detecting the hardness, the strength and the elongation of the synthetic rubber obtained by the internal mixer, and filtering after detection, wherein the synthetic rubber with the hardness of 65 degrees, the strength of more than or equal to 10MPa and the elongation of more than or equal to 175 percent is qualified synthetic rubber;
the second step is that: and (3) forming and vulcanizing rubber: the qualified synthetic rubber is processed by open milling at 60 ℃ through an open mill, and then the molded rubber is put into a mold in vulcanization equipment under the pressure of 170Kgf/cm2Vulcanizing the rubber at the temperature of 175 ℃, wherein the vulcanizing time is 240 seconds;
the third step: post-treatment and inspection: trimming the vulcanized product, putting the trimmed product in an oven for secondary vulcanization at 230 ℃ for 8h, and then inspecting the size and the appearance to obtain a qualified finished product.
The fluorine content of the fluororubber is more than 70%; WS280 is an organosiloxane-based processing aid; the calcium silicate is surface treated with a siloxane.
The preparation process of the modified molybdenum disulfide comprises the following steps: adding molybdenum disulfide and n-dodecyl mercaptan into 1-methyl-2-pyrrolidone, stirring and mixing, and performing ultrasonic dispersion for 1h to obtain a modified molybdenum disulfide suspension dispersion liquid; and carrying out reduced pressure suction filtration, washing and drying on the modified molybdenum disulfide suspension dispersion liquid to obtain the modified molybdenum disulfide.
The mass ratio of the molybdenum disulfide to the n-dodecyl mercaptan to the 1-methyl-2-pyrrolidone is controlled to be 2.2:1.2: 20.
The modified diatomite comprises the following steps:
weighing diatomite, putting the diatomite into a container, and putting the container into a constant-temperature water bath kettle at 90 ℃ for stirring and preheating; weighing the coupling agent in corresponding parts by weight, adding absolute ethyl alcohol for dissolving, and respectively dropwise adding the coupling agent into the diatomite under the condition of stirring at a low speed of 300 r/min; then the rotating speed of the stirrer is adjusted to 1500r/min, the mixture is stirred and reacted for 60min, and finally the modified diatomite is obtained after being taken out.
Controlling the mass ratio of the diatomite, the coupling agent and the absolute ethyl alcohol to be 50-60:50-60: 300-350; the silane coupling agent is one or more of a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH 570.
The preparation process of the modified white carbon black comprises the following steps:
the first step is as follows: adding white carbon black into 95% ethanol solution by mass percent and performing ultrasonic dispersion to obtain solution A; adding the anti-aging coupling agent into a 95% ethanol aqueous solution, and performing ultrasonic dispersion to obtain a solution B; mixing the solution A and the solution B and continuing to perform ultrasonic dispersion; refluxing the mixture for 2h under the protection of nitrogen, and spin-drying the solvent to obtain a solid;
the second step is that: drying the solid in a vacuum oven at 50 ℃ for 1-2 h; then washing the solid with absolute ethyl alcohol to remove the anti-aging coupling agent which is not grafted to the surface of the white carbon black; and then placing the cleaned solid in a vacuum oven for drying to obtain the modified white carbon black.
Controlling the mass ratio of the white carbon black to the ethanol solution with the mass fraction of 95% to be 10: 50; the mass ratio of the anti-aging coupling agent to the ethanol solution with the mass fraction of 95% is controlled to be 6: 40.
The nano inorganic filler comprises nano barium sulfate, hexagonal boron nitride, rutile type titanium dioxide, multi-walled carbon nano tubes and graphite.
Example 2
A low-permeability fluororubber product material comprises the following raw materials in parts by weight: 85 parts of fluororubber, 5 parts of calcium silicate, 1.8 parts of magnesium oxide, 5 parts of calcium hydroxide, WS 280: 0.4 part of iron oxide red, 0.4 part of modified molybdenum disulfide, 13 parts of nano inorganic filler, 3 parts of modified diatomite and 3 parts of modified white carbon black;
the preparation process of the low-permeability fluororubber product material comprises the following steps:
the first step is as follows: preparation of synthetic rubber: feeding all the raw materials into an internal mixer according to the parts by weight, detecting the hardness, the strength and the elongation of the synthetic rubber obtained by the internal mixer, and filtering after detection, wherein the synthetic rubber with the hardness of 68 degrees, the strength of more than or equal to 10MPa and the elongation of more than or equal to 175 percent is qualified synthetic rubber;
the second step is that: and (3) forming and vulcanizing rubber: the qualified synthetic rubber is processed by open milling at 62 ℃ through an open mill, and then the molded rubber is put into a mold in vulcanization equipment under the pressure of 172Kgf/cm2Vulcanizing the rubber at 177 ℃ for 250 seconds;
the third step: post-treatment and inspection: trimming the vulcanized product, putting the trimmed product in an oven for secondary vulcanization at 240 ℃ for 10h, and then inspecting the size and the appearance to obtain a qualified finished product.
The fluorine content of the fluororubber is more than 70%; WS280 is an organosiloxane-based processing aid; the calcium silicate is surface treated with a siloxane.
The preparation process of the modified molybdenum disulfide comprises the following steps: adding molybdenum disulfide and n-dodecyl mercaptan into 1-methyl-2-pyrrolidone, stirring and mixing, and performing ultrasonic dispersion for 1-2 hours to obtain a modified molybdenum disulfide suspension dispersion liquid; and carrying out reduced pressure suction filtration, washing and drying on the modified molybdenum disulfide suspension dispersion liquid to obtain the modified molybdenum disulfide.
The mass ratio of the molybdenum disulfide to the n-dodecyl mercaptan to the 1-methyl-2-pyrrolidone is controlled to be 2.3:1.3: 21.
The modified diatomite comprises the following steps:
weighing diatomite, putting the diatomite into a container, and putting the container into a constant-temperature water bath kettle at 90 ℃ for stirring and preheating; weighing the coupling agent in corresponding parts by weight, adding absolute ethyl alcohol for dissolving, and respectively dropwise adding the coupling agent into the diatomite under the condition of stirring at a low speed of 300 r/min; then the rotating speed of the stirrer is adjusted to 1500r/min, the mixture is stirred and reacted for 60min, and finally the modified diatomite is obtained after being taken out.
Preferably, the mass ratio of the diatomite to the coupling agent to the absolute ethyl alcohol is controlled to be 52:52: 310; the silane coupling agent is one or more of a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH 570.
The preparation process of the modified white carbon black comprises the following steps:
the first step is as follows: adding white carbon black into 95% ethanol solution by mass percent and performing ultrasonic dispersion to obtain solution A; adding the anti-aging coupling agent into a 95% ethanol aqueous solution, and performing ultrasonic dispersion to obtain a solution B; mixing the solution A and the solution B and continuing to perform ultrasonic dispersion; refluxing the mixture for 2h under the protection of nitrogen, and spin-drying the solvent to obtain a solid;
the second step is that: drying the solid in a vacuum oven at 52 ℃ for 1-2 h; then washing the solid with absolute ethyl alcohol to remove the anti-aging coupling agent which is not grafted to the surface of the white carbon black; and then placing the cleaned solid in a vacuum oven for drying to obtain the modified white carbon black.
Controlling the mass ratio of the white carbon black to the ethanol solution with the mass fraction of 95% to be 12: 52; the mass ratio of the anti-aging coupling agent to the ethanol solution with the mass fraction of 95% is controlled to be 7: 42.
The nano inorganic filler comprises nano barium sulfate, hexagonal boron nitride, rutile type titanium dioxide, multi-walled carbon nano tubes and graphite.
Example 3
A low-permeability fluororubber product material comprises the following raw materials in parts by weight: 87 parts of fluororubber, 5 parts of calcium silicate, 2.0 parts of magnesium oxide, 5 parts of calcium hydroxide, WS 280: 0.5 part of iron oxide red, 0.5 part of modified molybdenum disulfide, 16 parts of nano inorganic filler, 3 parts of modified diatomite and 3 parts of modified white carbon black;
the preparation process of the low-permeability fluororubber product material comprises the following steps:
the first step is as follows: preparation of synthetic rubber: feeding all the raw materials into an internal mixer according to the parts by weight, detecting the hardness, the strength and the elongation of the synthetic rubber obtained by the internal mixer, and filtering after detection, wherein the synthetic rubber with the hardness of 70 degrees, the strength of more than or equal to 10MPa and the elongation of more than or equal to 175 percent is qualified synthetic rubber;
the second step is that: and (3) forming and vulcanizing rubber: the qualified synthetic rubber is processed by open milling at 65 ℃ through an open mill, and then the molded rubber is put into a mold in vulcanization equipment under the pressure of 178Kgf/cm2Vulcanizing the rubber at the temperature of 180 ℃ for 270 seconds;
the third step: post-treatment and inspection: trimming the vulcanized product, putting the trimmed product in an oven for secondary vulcanization at 240 ℃ for 12h, and then inspecting the size and the appearance to obtain a qualified finished product.
The fluorine content of the fluororubber is more than 70%; WS280 is an organosiloxane-based processing aid; the calcium silicate is surface treated with a siloxane.
The preparation process of the modified molybdenum disulfide comprises the following steps: adding molybdenum disulfide and n-dodecyl mercaptan into 1-methyl-2-pyrrolidone, stirring and mixing, and performing ultrasonic dispersion for 2 hours to obtain a modified molybdenum disulfide suspension dispersion liquid; and carrying out reduced pressure suction filtration, washing and drying on the modified molybdenum disulfide suspension dispersion liquid to obtain the modified molybdenum disulfide.
The mass ratio of the molybdenum disulfide to the n-dodecyl mercaptan to the 1-methyl-2-pyrrolidone is controlled to be 2.4:1.4: 21.
The modified diatomite comprises the following steps:
weighing diatomite, putting the diatomite into a container, and putting the container into a constant-temperature water bath kettle at 90 ℃ for stirring and preheating; weighing the coupling agent in corresponding parts by weight, adding absolute ethyl alcohol for dissolving, and respectively dropwise adding the coupling agent into the diatomite under the condition of stirring at a low speed of 300 r/min; then the rotating speed of the stirrer is adjusted to 1500r/min, the mixture is stirred and reacted for 60min, and finally the modified diatomite is obtained after being taken out.
Controlling the mass ratio of the diatomite to the coupling agent to the absolute ethyl alcohol to be 57:57: 330; the silane coupling agent is one or more of a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH 570.
The preparation process of the modified white carbon black comprises the following steps:
the first step is as follows: adding white carbon black into 95% ethanol solution by mass percent and performing ultrasonic dispersion to obtain solution A; adding the anti-aging coupling agent into a 95% ethanol aqueous solution, and performing ultrasonic dispersion to obtain a solution B; mixing the solution A and the solution B and continuing to perform ultrasonic dispersion; refluxing the mixture for 3h under the protection of nitrogen, and spin-drying the solvent to obtain a solid;
the second step is that: drying the solid in a vacuum oven at 55 ℃ for 2 h; then washing the solid with absolute ethyl alcohol to remove the anti-aging coupling agent which is not grafted to the surface of the white carbon black; and then placing the cleaned solid in a vacuum oven for drying to obtain the modified white carbon black.
Controlling the mass ratio of the white carbon black to the ethanol solution with the mass fraction of 95% to be 13: 57; and controlling the mass ratio of the anti-aging coupling agent to the 95% ethanol solution to be 7: 45.
The nano inorganic filler comprises nano barium sulfate, hexagonal boron nitride, rutile type titanium dioxide, multi-walled carbon nano tubes and graphite.
Example 4
A low-permeability fluororubber product material comprises the following raw materials in parts by weight: 88 parts of fluororubber, 5 parts of calcium silicate, 2.3 parts of magnesium oxide, 5 parts of calcium hydroxide, WS 280: 0.6 part of iron oxide red, 0.6 part of modified molybdenum disulfide, 16 parts of nano inorganic filler, 3 parts of modified diatomite and 3 parts of modified white carbon black;
the preparation process of the low-permeability fluororubber product material comprises the following steps:
the first step is as follows: preparation of synthetic rubber: feeding all the raw materials into an internal mixer according to the parts by weight, detecting the hardness, the strength and the elongation of the synthetic rubber obtained by the internal mixer, and filtering after detection, wherein the synthetic rubber with the hardness of 73 degrees, the strength of more than or equal to 10MPa and the elongation of more than or equal to 175 percent is qualified synthetic rubber;
the second step is that: and (3) forming and vulcanizing rubber: the qualified synthetic rubber is processed by open milling at 68 ℃ through an open mill, and then the molded rubber is put into a mold in vulcanization equipment under the pressure of 178Kgf/cm2Vulcanizing the rubber at 183 deg.c for 280 sec;
the third step: post-treatment and inspection: trimming the vulcanized product, putting the trimmed product in an oven for secondary vulcanization at 240 ℃ for 15h, and then inspecting the size and the appearance to obtain a qualified finished product.
The fluorine content of the fluororubber is more than 70%; WS280 is an organosiloxane-based processing aid; the calcium silicate is surface treated with a siloxane.
The preparation process of the modified molybdenum disulfide comprises the following steps: adding molybdenum disulfide and n-dodecyl mercaptan into 1-methyl-2-pyrrolidone, stirring and mixing, and performing ultrasonic dispersion for 2 hours to obtain a modified molybdenum disulfide suspension dispersion liquid; and carrying out reduced pressure suction filtration, washing and drying on the modified molybdenum disulfide suspension dispersion liquid to obtain the modified molybdenum disulfide.
The mass ratio of the molybdenum disulfide to the n-dodecyl mercaptan to the 1-methyl-2-pyrrolidone is controlled to be 2.4:1.4: 21.
The modified diatomite comprises the following steps:
weighing diatomite, putting the diatomite into a container, and putting the container into a constant-temperature water bath kettle at 90 ℃ for stirring and preheating; weighing the coupling agent in corresponding parts by weight, adding absolute ethyl alcohol for dissolving, and respectively dropwise adding the coupling agent into the diatomite under the condition of stirring at a low speed of 300 r/min; then the rotating speed of the stirrer is adjusted to 1500r/min, the mixture is stirred and reacted for 60min, and finally the modified diatomite is obtained after being taken out.
Controlling the mass ratio of the diatomite, the coupling agent and the absolute ethyl alcohol to be 50-60:50-60: 300-350; the silane coupling agent is one or more of a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH 570.
The preparation process of the modified white carbon black comprises the following steps:
the first step is as follows: adding white carbon black into 95% ethanol solution by mass percent and performing ultrasonic dispersion to obtain solution A; adding the anti-aging coupling agent into a 95% ethanol aqueous solution, and performing ultrasonic dispersion to obtain a solution B; mixing the solution A and the solution B and continuing to perform ultrasonic dispersion; refluxing the mixture for 3h under the protection of nitrogen, and spin-drying the solvent to obtain a solid;
the second step is that: drying the solid in a vacuum oven at 58 ℃ for 2 h; then washing the solid with absolute ethyl alcohol to remove the anti-aging coupling agent which is not grafted to the surface of the white carbon black; and then placing the cleaned solid in a vacuum oven for drying to obtain the modified white carbon black.
Controlling the mass ratio of the white carbon black to the ethanol solution with the mass fraction of 95% to be 14: 63; and controlling the mass ratio of the anti-aging coupling agent to the 95% ethanol solution to be 7: 48.
The nano inorganic filler comprises nano barium sulfate, hexagonal boron nitride, rutile type titanium dioxide, multi-walled carbon nano tubes and graphite.
Example 5
A low-permeability fluororubber product material comprises the following raw materials in parts by weight: 90 parts of fluororubber, 6 parts of calcium silicate, 2.5 parts of magnesium oxide, 6 parts of calcium hydroxide, WS 280: 0.7 part of iron oxide red, 0.7 part of modified molybdenum disulfide, 18 parts of nano inorganic filler, 4 parts of modified diatomite and 4 parts of modified white carbon black;
the preparation process of the low-permeability fluororubber product material comprises the following steps:
the first step is as follows: preparation of synthetic rubber: feeding all the raw materials into an internal mixer according to the parts by weight, detecting the hardness, strength and elongation of the synthetic rubber obtained by the internal mixer, and filtering after detection, wherein the synthetic rubber with the hardness of 75 degrees, the strength of more than or equal to 10MPa and the elongation of more than or equal to 175 percent is qualified synthetic rubber;
the second step is that: and (3) forming and vulcanizing rubber: the qualified synthetic rubber is processed by open milling at 70 ℃ through an open mill, and then the molded rubber is put into a mold in vulcanization equipment under the pressure of 190Kgf/cm2And the temperature is 185 ℃, the rubber is vulcanized for 300 seconds at the vulcanization time of 240-;
the third step: post-treatment and inspection: trimming the vulcanized product, putting the trimmed product in an oven for secondary vulcanization at-250 ℃ for 16h, and then inspecting the size and the appearance to obtain a qualified finished product.
The fluorine content of the fluororubber is more than 70%; WS280 is an organosiloxane-based processing aid; the calcium silicate is surface treated with a siloxane.
The preparation process of the modified molybdenum disulfide comprises the following steps: adding molybdenum disulfide and n-dodecyl mercaptan into 1-methyl-2-pyrrolidone, stirring and mixing, and performing ultrasonic dispersion for 2 hours to obtain a modified molybdenum disulfide suspension dispersion liquid; and carrying out reduced pressure suction filtration, washing and drying on the modified molybdenum disulfide suspension dispersion liquid to obtain the modified molybdenum disulfide.
The mass ratio of the molybdenum disulfide to the n-dodecyl mercaptan to the 1-methyl-2-pyrrolidone is controlled to be 2.5:1.5: 22.
The modified diatomite comprises the following steps:
weighing diatomite, putting the diatomite into a container, and putting the container into a constant-temperature water bath kettle at 90 ℃ for stirring and preheating; weighing the coupling agent in corresponding parts by weight, adding absolute ethyl alcohol for dissolving, and respectively dropwise adding the coupling agent into the diatomite under the condition of stirring at a low speed of 300 r/min; then the rotating speed of the stirrer is adjusted to 1500r/min, the mixture is stirred and reacted for 60min, and finally the modified diatomite is obtained after being taken out.
Controlling the mass ratio of the diatomite to the coupling agent to the absolute ethyl alcohol to be 60:60: 350; the silane coupling agent is one or more of a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH 570.
The preparation process of the modified white carbon black comprises the following steps:
the first step is as follows: adding white carbon black into 95% ethanol solution by mass percent and performing ultrasonic dispersion to obtain solution A; adding the anti-aging coupling agent into a 95% ethanol aqueous solution, and performing ultrasonic dispersion to obtain a solution B; mixing the solution A and the solution B and continuing to perform ultrasonic dispersion; refluxing the mixture for 3h under the protection of nitrogen, and spin-drying the solvent to obtain a solid;
drying the solid in a vacuum oven at 60 ℃ for 2 h; then washing the solid with absolute ethyl alcohol to remove the anti-aging coupling agent which is not grafted to the surface of the white carbon black; and then placing the cleaned solid in a vacuum oven for drying to obtain the modified white carbon black.
Controlling the mass ratio of the white carbon black to the ethanol solution with the mass fraction of 95% to be 15: 60; the mass ratio of the anti-aging coupling agent to the ethanol solution with the mass fraction of 95% is controlled to be 8: 50.
The nano inorganic filler comprises nano barium sulfate, hexagonal boron nitride, rutile type titanium dioxide, multi-walled carbon nano tubes and graphite.
Comparative example 1
Comparative example 1 is a commercially available fluororubber product.
The antibacterial performance of the samples obtained in each group of examples and comparative examples is tested, and the mechanical properties of the samples are tested;
the preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise forms disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (9)
1. A low permeability fluororubber product material, which is characterized in that: the feed comprises the following raw materials in parts by weight: 84-90 parts of fluororubber, 4-6 parts of calcium silicate, 1.5-2.5 parts of magnesium oxide, 4-6 parts of calcium hydroxide, WS 280: 0.3-0.7 part of iron oxide red, 0.3-0.7 part of modified molybdenum disulfide, 12-18 parts of nano inorganic filler, 2-4 parts of modified diatomite and 2-4 parts of modified white carbon black;
the preparation process of the low-permeability fluororubber product material comprises the following steps:
the first step is as follows: preparation of synthetic rubber: feeding all the raw materials into an internal mixer according to the parts by weight, detecting the hardness, the strength and the elongation of the synthetic rubber obtained by the internal mixer, and filtering after detection, wherein the synthetic rubber with the hardness of 70 +/-5 degrees, the strength of more than or equal to 10MPa and the elongation of more than or equal to 175 percent is qualified synthetic rubber;
the second step is that: and (3) forming and vulcanizing rubber: the qualified synthetic rubber is processed by open milling and molding at 60-70 ℃ through an open mill, and then the molded rubber is put into a mold in vulcanization equipment under the pressure of 170-2And the temperature is 175-185 ℃, the rubber is vulcanized for 300 seconds at the vulcanization time of 240-;
the third step: post-treatment and inspection: trimming the vulcanized product, putting the trimmed product in an oven for secondary vulcanization at 230-250 ℃ for 8-16 h, and then inspecting the size and the appearance to obtain a qualified finished product.
2. A low permeability fluororubber article material according to claim 1, characterized in that said fluororubber has a fluorine content of more than 70%; WS280 is an organosiloxane-based processing aid; the calcium silicate is surface treated with a siloxane.
3. The low-permeability fluororubber product material according to claim 1, wherein the preparation process of the modified molybdenum disulfide comprises the following steps: adding molybdenum disulfide and n-dodecyl mercaptan into 1-methyl-2-pyrrolidone, stirring and mixing, and performing ultrasonic dispersion for 1-2 hours to obtain a modified molybdenum disulfide suspension dispersion liquid; and carrying out reduced pressure suction filtration, washing and drying on the modified molybdenum disulfide suspension dispersion liquid to obtain the modified molybdenum disulfide.
4. A low permeability fluororubber formed product material according to claim 3, wherein the mass ratio of molybdenum disulfide, n-dodecanethiol and 1-methyl-2-pyrrolidone is controlled to 2.2-2.5:1.2-1.5: 20-22.
5. A low permeability fluororubber formed product material according to claim 1, characterized in that the modified diatomaceous earth comprises the following steps:
weighing diatomite, putting the diatomite into a container, and putting the container into a constant-temperature water bath kettle at 90 ℃ for stirring and preheating; weighing the coupling agent in corresponding parts by weight, adding absolute ethyl alcohol for dissolving, and respectively dropwise adding the coupling agent into the diatomite under the condition of stirring at a low speed of 300 r/min; then the rotating speed of the stirrer is adjusted to 1500r/min, the mixture is stirred and reacted for 60min, and finally the modified diatomite is obtained after being taken out.
6. The low-permeability fluororubber product material according to claim 5, wherein the mass ratio of diatomite, coupling agent and absolute ethanol is controlled to be 50-60:50-60: 300-350; the silane coupling agent is one or more of a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH 570.
7. The low-permeability fluororubber product material according to claim 1, wherein the preparation process of modified white carbon black comprises the following steps:
the first step is as follows: adding white carbon black into 95% ethanol solution by mass percent and performing ultrasonic dispersion to obtain solution A; adding the anti-aging coupling agent into a 95% ethanol aqueous solution, and performing ultrasonic dispersion to obtain a solution B; mixing the solution A and the solution B and continuing to perform ultrasonic dispersion; refluxing the mixture for 2-3h under the protection of nitrogen, and spin-drying the solvent to obtain a solid;
the second step is that: drying the solid in a vacuum oven at 50-60 ℃ for 1-2 h; then washing the solid with absolute ethyl alcohol to remove the anti-aging coupling agent which is not grafted to the surface of the white carbon black; and then placing the cleaned solid in a vacuum oven for drying to obtain the modified white carbon black.
8. The low-permeability fluororubber product material according to claim 7, characterized in that the mass ratio of white carbon black to 95% ethanol solution is controlled to 10-15: 50-60; the mass ratio of the anti-aging coupling agent to the 95% ethanol solution is controlled to be 6-8: 40-50.
9. A low permeability fluororubber formed product material according to claim 7, characterized in that the nano inorganic filler comprises nano barium sulfate, hexagonal boron nitride, rutile type titanium dioxide, multi-walled carbon nanotubes and graphite.
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| CN115975313A (en) * | 2022-12-23 | 2023-04-18 | 广东硕成科技股份有限公司 | High-rheological-property fluororubber material, preparation method and product thereof |
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