CN113429712A - Low-resistivity fluororubber for automobile fuel pipeline system and preparation method thereof - Google Patents
Low-resistivity fluororubber for automobile fuel pipeline system and preparation method thereof Download PDFInfo
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- CN113429712A CN113429712A CN202110800238.2A CN202110800238A CN113429712A CN 113429712 A CN113429712 A CN 113429712A CN 202110800238 A CN202110800238 A CN 202110800238A CN 113429712 A CN113429712 A CN 113429712A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08L27/16—Homopolymers or copolymers or vinylidene fluoride
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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
- C08K2003/2206—Oxides; Hydroxides of metals of calcium, strontium or barium
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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
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
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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
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/04—Antistatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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Abstract
The low-resistivity fluororubber for the automobile fuel pipeline system is prepared from ternary fluororubber, carbon black, active magnesium oxide, carbon nano tubes, nano-scale surface silver-plated glass beads, calcium hydroxide, a release agent, a bisphenol AF crosslinking agent and a vulcanization accelerator. Also provides a preparation method of the low-resistivity fluororubber, which is prepared by mixing ternary fluororubberKneading by an internal mixer to generate heat, then adding N-990 carbon black, active magnesium oxide, a carbon nanotube, nano-scale surface silver-plated glass beads, calcium hydroxide and a release agent, and stirring and kneading; turning to an open mill for turning, thinning and discharging, and then taking out and standing; then putting the mixture into an open mill again for mixing, adding bisphenol AF and a vulcanization accelerator, and discharging the mixture after open milling to obtain rubber compound; and (3) placing the rubber compound into a die for compression molding after performing, and then carrying out two-stage vulcanization baking to obtain the required sealing element. The volume resistance of the fluororubbers according to the invention is less than 108Omega cm, seal surface resistivity less than 104Ω。
Description
Technical Field
The invention belongs to the field of chemical industry, and relates to fluororubber, in particular to low-resistivity fluororubber for an automobile fuel pipeline system and a preparation method thereof.
Background
With the emphasis of the automotive industry on safety, the static electricity brought by the fuel line system due to the fuel injection may accumulate along with the flow process and cause the following risks to the fuel system: firstly, the static spark generated after static accumulation ignites fuel steam to cause fire; secondly, the small holes of the parts such as the fuel pipe, the joint and the like are leaked due to electric breakdown; third, static electricity may further affect the operation of the associated electronics of the piping system, such as the wiring harness.
The SEA J1645 standard has been commonly adopted in Europe and the United states to standardize electrostatic discharge solutions for components such as pipe joints, fuel pumps and filters during fuel delivery, requiring the resistivity of the entire pipe to be less than 106Ω：
Since fluororubber is commonly used for sealing rings of various units of fuel pipelines, the general fluororubber belongs to insulating materials, and the volume resistivity of the fluororubber is generally higher than 109Omega cm, the electrostatic discharge requirement of SEA J1645 cannot be met. This requires an antistatic grade of fluororubber material, i.e. having a volume resistivity of between 104Ωcm～108Omega cm.
Disclosure of Invention
The invention aims to provide low-resistivity fluororubber for an automobile fuel pipeline system and a preparation method thereof, and aims to solve the problem that the volume resistivity of the fluororubber in the prior art is generally higher than 109Omega cm, can not satisfy SEA J1645 electrostatic discharge requirement.
The invention relates to low-resistivity fluororubber for an automobile fuel pipeline system, which is prepared from the following raw materials in parts by weight:
further, the ternary fluororubber is a raw rubber obtained by mixing vinylidene fluoride, tetrafluoroethylene and hexafluoropropylene, and FKM (such as Viton-B-600, Tecnoflon @ FOR9383, DAI-EL G-551) with a fluorine content of more than 68% is commercially available.
Further, the release agent is carnauba wax.
Further, the type of the carbon black is N-990.
Further, the vulcanization accelerator is benzyltriphenylphosphonium chloride (BPP).
Specifically, the carbon nanotubes, the nano-sized surface silver-plated glass beads and the bisphenol AF cross-linking agent are all commercially available products, and are not described herein again.
The invention also provides a preparation method of the low-resistivity fluororubber for the automobile fuel pipeline system, which comprises the following steps:
1) weighing each reaction substance according to parts by weight;
2) plasticating by adopting an internal mixer, firstly adding the ternary fluororubber into the internal mixer, rolling and kneading the ternary fluororubber in the internal mixer, adding carbon black, active magnesium oxide, a carbon nano-tube, nano-scale surface silver-plated glass beads, calcium hydroxide and a release agent when the temperature of the fluororubber in the internal mixer rises to 100-120 ℃, and stirring and kneading for 5-10 min;
3) then turning to an open mill for turning, controlling the speed of a roller of the open mill to be 50-60 r/min, controlling the temperature to be 60-80 ℃, thinning and discharging the sheet after mixing for 5-10 min, and then taking out and standing for 8-12 h;
4) then putting the mixture into an open mill again for mixing for 1-2 min, adding bisphenol AF and a vulcanization accelerator, and rolling the mixture into sheets after open milling for 4-8 min to obtain rubber compound;
5) and (3) performing the rubber compound, putting the rubber compound into a forming die, carrying out vulcanization in the forming die at the temperature of 165-180 ℃ for 5-8 min, carrying out die pressing to obtain a required shape, removing flash, carrying out two-stage vulcanization baking at the temperature of 210-230 ℃ for 16-24 h, and finally inspecting to obtain the low-resistivity fluororubber.
Specifically, if the sealing ring is prepared, the sealing ring is molded into a required shape, then the flash is removed, the two-stage vulcanization baking is carried out at the temperature of 210-230 ℃ for 16-24 h, and finally the sealing ring made of the low-resistivity fluororubber material is obtained after inspection.
The components of the formula of the invention have good conductivity, and the substances with conductivity are carbon nano tubes and nano-scale silver-plated glass beads with surfaces, and the addition aims to mainly reduce the resistivity of the fluororubber. Carbon nanotubes, also known as buckytubes, are one-dimensional quantum materials with special structures. Carbon nanotubes are coaxial circular tubes consisting of several to tens of layers of carbon atoms arranged in a hexagonal pattern. The layers are maintained at a fixed distance of about 0.34nm, with a diameter of typically 2-20 nm. The P electrons of carbon atoms on the carbon nano tube form a large-range delocalized pi bond, and the carbon nano tube has some special electrical properties due to the obvious conjugation effect. In the case of carbon nanotubes, the valence band and the conduction band are partially overlapped, and correspond to a half-full band, electrons can move freely, and the carbon nanotubes exhibit metal-like conductivity. The nano-scale surface silver-plated glass beads are dispersed in the rubber compound, and when electrostatic charges are generated, the surface silver plating of the glass beads realizes a quick conductive function, so that the electrostatic charges are transferred, and the conductive function is realized.
The conductive components of the invention are carbon nano-tubes and nano-scale surface silver-plated glass beads, and the higher the component content of the carbon nano-tubes is, the better the conductivity is. However, when the content of the carbon nanotubes is increased, the hardness of the fluororubber formed product is greatly increased with the increase in the carbon nanotube content, and the compression set thereof is also greatly increased, resulting in ultrahigh hardness and poor elasticity of the material. As a rubber sealing product, its elasticity is deteriorated to affect the sealing function, and its hardness is increased to make it difficult to install and use the sealing product. Therefore, the amount of the carbon nanotubes used needs to be controlled within a certain range. The nano-scale surface silver-plated glass beads are added, so that the dispersion degree of the conductive components of the rubber compound is enhanced, and the conductive uniformity of the rubber compound is better. However, since the glass beads with silver-plated surfaces belong to inorganic fillers, the tensile strength of the fluororubber product is greatly increased and the elongation at break is greatly reduced due to excessive increase of the components. Therefore, according to comprehensive analysis, the carbon nano tube and the nano-scale surface silver-plated glass beads are mixed for use, so that the better performance requirements of the hardness, tensile strength, elongation at break and compression permanent deformation of the fluororubber can be ensured while the electrical conductivity of the fluororubber product is ensured.
Due to the insulating properties of fluororubbers themselves, the conductivity of the products made of fluororubbers is very poor, which is not favorable for electrostatic discharge. The invention designs a formula of low-resistance fluororubber of an automobile fuel pipeline system beneficial to electrostatic discharge, and a fluororubber sealing element prepared by using the formula meets the requirements of fuel resistance and high temperature resistance, and simultaneously the surface resistivity of a sealing element product is lower than 104Ω。
Compared with the prior art, the invention has remarkable technical progress. Aiming at the problem of high resistivity of the fluororubber, the invention provides a novel fluororubber formula which can reduce the resistivity of the fluororubber so that the volume resistance is lower than 108Omega cm, and the surface resistivity of the sealing member made of the same is less than 104Omega (50V direct current voltage, 50% relative humidity, O-ring specification phi 9.6x phi 2), therefore the sealing element made of the antistatic conductive fluororubber meets the requirement of SAE J1645 on static electricity release, and meanwhile, the product meets the requirement of SAE J2044 on sealing of quick joints of fuel pipelines.
Detailed Description
Example 1
The invention relates to low-resistivity fluororubber for an automobile fuel pipeline system, which is prepared from the following raw materials in parts by weight:
further, the ternary fluororubber is a raw rubber prepared by mixing vinylidene fluoride, tetrafluoroethylene and hexafluoropropylene, and FKM (such as Viton-B-600, Tecnoflon @ FOR9383, DAI-EL G-551) with fluorine content of more than 68% can also be purchased on the market.
Further, the release agent is carnauba wax.
Further, the type of the carbon black is N-990.
Further, the vulcanization accelerator is benzyltriphenylphosphonium chloride (BPP).
Specifically, the carbon nanotubes, the nano-sized surface silver-plated glass beads and the bisphenol AF cross-linking agent are all commercially available products, and are not described herein again.
The invention also provides a preparation method of the low-resistivity fluororubber for the automobile fuel pipeline system, which comprises the following steps:
1) weighing each reaction substance according to parts by weight;
2) plasticating by adopting an internal mixer, firstly adding the ternary fluororubber into the internal mixer, rolling and kneading the ternary fluororubber in the internal mixer, adding N-990 carbon black, activated magnesium oxide, a carbon nano-tube, nano-scale surface silver-plated glass beads, calcium hydroxide and a release agent when the temperature of the fluororubber in the internal mixer rises to 100-120 ℃, and stirring and kneading for 5-10 min;
3) then turning to an open mill for turning, controlling the speed of a roller of the open mill to be 50-60 r/min, controlling the temperature to be 60-80 ℃, thinning and discharging the sheet after mixing for 5-10 min, and then taking out and standing for 8-12 h;
4) then putting the mixture into an open mill again for mixing for 1-2 min, adding bisphenol AF and a vulcanization accelerator, and rolling the mixture into sheets after open milling for 4-8 min to obtain rubber compound;
5) and (3) performing the rubber compound, putting the rubber compound into a forming die, wherein the vulcanization temperature in the forming die is 165-180 ℃ for 5-8 min, die-pressing to obtain a required shape, removing flash, performing secondary vulcanization baking at the temperature of 210-230 ℃ for 16-24 h, and finally inspecting to obtain the required low-resistivity fluororubber.
Specifically, if the sealing ring is prepared, the sealing ring is molded into a required shape, then the flash is removed, the two-stage vulcanization baking is carried out at the temperature of 210-230 ℃ for 16-24 h, and finally the sealing ring made of the low-resistivity fluororubber material is obtained after inspection.
Testing and comparison of different conductive components:
as can be seen from example 1, the volume resistance of the mixture of carbon nanotubes and nanosilver-coated glass beads is less than 108Omega cm meets the requirements, has the function of static electricity conduction, and keeps the hardness, tensile strength, fracture compression ratio and compression permanent deformation of the fluororubber at better performance levels. While example 2, which does not contain any conductive component, is excellent in physical properties and compression set, the volume resistance thereof is 2.3X1013And the insulation grade is classified as an insulation grade, and the conductive function is not provided. In example 3, the volume resistance was greatly reduced and the conductivity was very excellent by adding the carbon nanotube, but the hardness and tensile strength were increased, the elongation at break was reduced, and the compression set was very poor, that is, the compression set value was very poor as a sealing material, reflecting the poor elasticity of the material, which is unfavorable as a sealing function.
Claims (7)
1. The low-resistivity fluororubber for the automobile fuel pipeline system is characterized by being prepared from the following raw materials in parts by weight:
2. the low-resistivity fluororubber for automotive fuel pipe systems according to claim 1, characterized in that: the ternary fluororubber is prepared by mixing vinylidene fluoride, tetrafluoroethylene and hexafluoropropylene.
3. The low-resistivity fluororubber for automotive fuel pipe systems according to claim 1, characterized in that: the volume resistivity of the low-resistivity fluororubber is 104Ωcm～108Ωcm。
4. The low-resistivity fluororubber for automotive fuel pipe systems according to claim 1, characterized in that: the type of the carbon black is N-990.
5. The low-resistivity fluororubber for automotive fuel pipe systems according to claim 1, characterized in that: the release agent is carnauba wax.
6. The low-resistivity fluororubber for automotive fuel pipe systems according to claim 1, characterized in that: the vulcanization accelerator is benzyltriphenylphosphonium chloride.
7. The preparation method of the low-resistivity fluororubber for the automobile fuel pipeline system, which is characterized by comprising the following steps of:
1) weighing each reaction substance according to parts by weight;
2) plasticating by adopting an internal mixer, firstly adding the ternary fluororubber into the internal mixer, rolling and kneading the ternary fluororubber in the internal mixer, adding carbon black, active magnesium oxide, a carbon nano-tube, nano-scale surface silver-plated glass beads, calcium hydroxide and a release agent when the temperature of the fluororubber in the internal mixer rises to 100-120 ℃, and stirring and kneading for 5-10 min;
3) then turning to an open mill for turning, controlling the speed of a roller of the open mill to be 50-60 r/min, controlling the temperature to be 60-80 ℃, thinning and discharging the sheet after mixing for 5-10 min, and then taking out and standing for 8-12 h;
4) then putting the mixture into an open mill again for mixing for 1-2 min, adding bisphenol AF and a vulcanization accelerator, and rolling the mixture into sheets after open milling for 4-8 min to obtain rubber compound;
5) and (3) performing the rubber compound, putting the rubber compound into a forming die, carrying out vulcanization in the forming die at the temperature of 165-180 ℃ for 5-8 min, carrying out die pressing to obtain a required shape, removing flash, carrying out two-stage vulcanization baking at the temperature of 210-230 ℃ for 16-24 h, and finally inspecting to obtain the low-resistivity fluororubber.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114410038A (en) * | 2021-11-16 | 2022-04-29 | 江苏鹏翎胶管有限公司 | Conductive fluororubber, fuel pipeline and application thereof, preparation method of fuel pipeline and fuel system |
| CN114752162A (en) * | 2021-11-26 | 2022-07-15 | 浙江户润密封系统有限公司 | Conductive fluororubber for oil seal and production method thereof |
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2021
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114410038A (en) * | 2021-11-16 | 2022-04-29 | 江苏鹏翎胶管有限公司 | Conductive fluororubber, fuel pipeline and application thereof, preparation method of fuel pipeline and fuel system |
| CN114752162A (en) * | 2021-11-26 | 2022-07-15 | 浙江户润密封系统有限公司 | Conductive fluororubber for oil seal and production method thereof |
| CN114752162B (en) * | 2021-11-26 | 2023-07-21 | 浙江户润密封系统有限公司 | Production method of conductive fluororubber for oil seal |
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