CN114716828B - Rubber for low-resistance flame-retardant fuel cell transmission pipeline - Google Patents
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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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
- C08K2003/2224—Magnesium hydroxide
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2201/001—Conductive additives
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2201/011—Nanostructured additives
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- 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
- C08L2203/00—Applications
- C08L2203/18—Applications used for pipes
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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
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention relates to the field of rubber materials, and discloses rubber for a low-resistance flame-retardant fuel cell transmission pipeline, which comprises the following components in parts by weight: 90-110 parts of vinyl silicone rubber, 40-60 parts of fumed silica, 20-40 parts of composite flame retardant, 2-4 parts of conductive agent, 1-3 parts of colorant and 1-2 parts of vulcanizing agent; the composite flame retardant is polypyrrole nanotube composite flame retardant. In the polypyrrole nanotube composite flame retardant, magnesium hydroxide is combined to the surface of the polypyrrole nanotube in the preparation process, the flame retardant effect of the flame retardant is enhanced through the combination effect of the magnesium hydroxide and the polypyrrole nanotube, the dispersibility and the compatibility of the flame retardant are improved, the material is endowed with good flame retardance, and meanwhile, the resistance of the rubber is reduced under the condition of meeting the requirement of mechanical strength, so that the rubber has good static electricity release capacity; the prepared rubber material has excellent flame retardant property and static electricity releasing capacity, and is suitable for being applied to fuel cell transmission pipelines.
Description
Technical Field
The invention relates to the field of rubber materials, in particular to rubber for a low-resistance flame-retardant fuel cell transmission pipeline.
Background
With the development of economy and technology, especially energy crisis and pollution caused by fossil fuels, clean energy has been attracting attention. A hydrogen fuel cell (PEMFC) is a power generation device for directly converting chemical energy of hydrogen and oxygen into electric energy, has the advantages of zero pollution, low noise, high energy conversion rate, good durability and the like, and becomes a product which is widely focused in the field of clean energy.
In hydrogen fuel cells, sealing and transfer lines have a significant impact on their stability, durability, safety, and life costs. Particularly, for a transmission pipeline, the hydrogen leakage monitoring, electrostatic protection, explosion prevention, flame retardance and other aspects are required to be prevented and controlled, so that accidents are prevented, and potential safety hazards are prevented from being caused. The material performance of the transmission pipeline is very high, and the material is required to meet the performance requirements of barrier property, stability, acid resistance, flame retardance and the like.
The silicone rubber is an organic elastomer material prepared by reinforcing and vulcanizing high-relative molecular weight polysiloxane, and two organic groups such as methyl, ethyl, trifluoropropyl, phenyl and the like are usually connected to silicon atoms so as to meet different performance requirements. However, the silicone rubber is inflammable, and the application of the silicone rubber in the fields of aerospace, electronics, electrics and the like is limited. Chinese patent publication No. CN111303636A provides a low heat conduction flame retardant fireproof silicone rubber composite material, comprising, by weight: 60-80 parts of methyl vinyl silicone rubber, 20-40 parts of methyl vinyl phenyl silicone rubber, 15-25 parts of hydrophobic silica aerogel powder, 20-30 parts of metal oxide powder, 5-10 parts of fluxing agent, 3 parts of crosslinking auxiliary agent, 20-30 parts of gas-phase white carbon black, 3 parts of hydroxyl silicone oil, 20-30 parts of organic-inorganic compound flame retardant and 1 part of antioxidant; the metal oxide is selected from one or more of ferric oxide, calcium carbonate and zirconium dioxide; the organic-inorganic compound flame retardant is selected from a mixture of modified pentaerythritol phosphate and silane coupling agent modified aluminum hydroxide; the modified pentaerythritol phosphate is prepared by reacting phosphorus oxychloride modified pentaerythritol phosphate with aminopropyl terminated dimethyl silicone oil. The composite material has good fireproof and heat insulation effects and mechanical properties. However, such materials do not improve the static discharge capability of the silicone rubber, which may lead to leakage of the perforation caused by static accumulation during application in the transmission pipeline due to excessively high overall resistance, and affect the normal operation of the hydrogen fuel cell.
Disclosure of Invention
The invention provides rubber for a low-resistance flame-retardant fuel cell transmission pipeline, which aims to solve the problems that the traditional silicone rubber is poor in flame retardance, high in resistance and incapable of releasing static electricity. The composite flame retardant is utilized to realize the flame retardant purpose and enhance the conductivity of the rubber, and the flame retardant and the static electricity releasing capability of the rubber can meet the requirements by matching with other processing aids.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the rubber for the low-resistance flame-retardant fuel cell transmission pipeline comprises the following components in parts by weight: 90-110 parts of vinyl silicone rubber, 40-60 parts of fumed silica, 20-40 parts of composite flame retardant, 2-4 parts of conductive agent, 1-3 parts of colorant and 1-2 parts of vulcanizing agent; the composite flame retardant is polypyrrole nanotube composite flame retardant.
Polypyrrole is a conductive polymer having a conjugated structure in which carbon-carbon single bonds and carbon-carbon double bonds are alternately arranged, and 2 pi electrons in the conjugated double bonds are not fixed to a certain carbon atom, and they can be transferred from one carbon atom to another carbon atom, that is, they have a tendency to extend over the entire molecular chain. I.e. the overlapping of pi-electron clouds within the molecule creates an energy band common to the whole molecule, pi-electrons being similar to free electrons in a metal conductor. Electrons constituting pi bonds can move along a molecular chain in the presence of an electric field, thereby imparting conductivity to polypyrrole. Meanwhile, the polypyrrole nanotube composite flame retardant is generated in the polypyrrole synthesis process, and plays a good flame retardant role through inorganic flame retardant components and polypyrrole in the flame retardant, and the conductivity of the polypyrrole is not changed. When the polypyrrole nanotube composite flame retardant is dispersed in the rubber, the polypyrrole nanotube composite flame retardant has good dispersibility, and can enhance the conductivity uniformity of the rubber. If electrostatic charges are generated, the polypyrrole nanotube composite flame retardant can realize quick conduction, so that the electrostatic charges are transferred, and the static accumulation is reduced.
Preferably, the preparation method of the polypyrrole nanotube composite flame retardant comprises the following steps:
(1) Polypyrrole nanotube synthesis: dissolving pyrrole and doping agent in deionized water, adding oxidant, mixing and reacting for 24-36 h, filtering, washing, drying at 20-30 ℃ for 24-48 h, obtaining polypyrrole nanotube;
(2) And (3) synthesizing a polypyrrole nanotube composite flame retardant: dispersing the polypyrrole nanotube obtained in the step (1) in a magnesium source solution with the concentration of 0.1-1 mol/L, uniformly stirring, adding alkali liquor to the pH value of 9-10, standing for reaction for 4-8 hours, filtering, washing and drying to obtain the polypyrrole nanotube composite flame retardant.
In the process of synthesizing the polypyrrole nanotube composite flame retardant, firstly, the polypyrrole nanotube is synthesized by a doping polymerization method. Polypyrrole nanotube is one-dimensional nanometer material with linear shape and high conductivity. And then, the magnesium hydroxide is polymerized on the surface of the polypyrrole nanotube through hydrogen bond, so that on one hand, the electric conductivity of the polypyrrole nanotube is not changed, and on the other hand, the magnesium hydroxide is a flame retardant with good effect, and the flame retardant capability of the polypyrrole nanotube composite flame retardant can be further improved. In the combustion process, the magnesium hydroxide can be heated and decomposed into magnesium oxide and water, a large amount of heat is absorbed, the temperature rise is slowed down, meanwhile, the discharged water can also inhibit the generation of smoke, the triple functions of flame retardance, smoke suppression and filling are achieved, and the flame retardance effect is excellent. The nitrogen element in the polypyrrole can generate nonflammable gas in the combustion process, so that the contact between the rubber material and oxygen is reduced, the carbon element can generate a compact carbon layer in the combustion process, and the contact between the rubber material and a combustion position is reduced. The magnesium hydroxide is combined to the surface of the polypyrrole nanotube through the combination of the magnesium hydroxide and the polymer material, so that the dispersibility and compatibility of the magnesium hydroxide in the polymer material can be enhanced, the agglomeration of magnesium hydroxide particles can be reduced, and the flame retardant property of the rubber can be improved.
Preferably, in the step (1), the dopant is one of β -naphthalene sulfonic acid and methyl orange, and the oxidant is one of ammonium persulfate, ferric chloride and ferric nitrate. More preferably, the dopant is methyl orange and the oxidant is ferric chloride.
Preferably, in the step (1), the mass ratio of pyrrole to dopant is (3-4): 1.
Preferably, in the step (1), the ratio (4 to 6) of the amount of the substance of pyrrole to the amount of the oxidizing agent is 1.
Preferably, in the step (2), the mass ratio of the magnesium source solution to the polypyrrole is (200 to 300): 1. The excessive mass of the magnesium source solution may cause excessive amount of magnesium hydroxide to be generated, which may cause the particle size of the particles to increase and reduce the conductivity of the material; when the mass of the magnesium source solution is too small, enough magnesium hydroxide cannot be generated, so that the flame retardant performance of the polypyrrole nanotube composite flame retardant is reduced.
Preferably, in the step (2), the magnesium source solution is one of magnesium chloride, magnesium sulfate and magnesium iodide, and the alkali solution is ammonia water.
Preferably, the conductive agent is one of acetylene black, carbon fiber, carbon nanotube and graphite or a combination thereof. The addition of the conductive agent can further reduce the resistance of the rubber material, but excessive addition of the conventional conductive agent can cause obvious changes in the mechanical properties of the silicone rubber product, such as excessive hardness or reduced elasticity, and the like, so that the silicone rubber product is easy to crack or leak when being applied to a fuel cell transmission pipeline, and therefore, the addition amount of the conductive agent needs to be limited. The polypyrrole nanotube composite flame retardant has good dispersibility, can be mutually supplemented with the conductive agent, and can provide low resistance and simultaneously enable the rubber product to meet the mechanical strength requirement.
Preferably, the colorant is titanium dioxide.
Preferably, the vulcanizing agent is 2, 5-dimethyl-2, 5-di (t-butylperoxy) hexane.
Therefore, the invention has the following beneficial effects: (1) The polypyrrole nanotube composite flame retardant is prepared and applied to the silicon rubber, and the resistance of the rubber is reduced under the condition of meeting the requirement of mechanical strength, so that the rubber has good static electricity releasing capacity; (2) In the polypyrrole nanotube composite flame retardant, magnesium hydroxide is combined to the surface of the polypyrrole nanotube in the preparation process, the flame retardant effect of the flame retardant is enhanced through the composite action of the magnesium hydroxide and the polypyrrole nanotube, the dispersibility and the compatibility of the flame retardant are improved, and the material is endowed with good flame retardance; (3) The prepared rubber material has excellent flame retardant property and static electricity releasing capacity, and is suitable for being applied to fuel cell transmission pipelines.
Detailed Description
The invention is further described below in connection with the following detailed description. It should be understood that these embodiments are useful for illustrating the basic principle, main features and advantages of the present invention, and that the present invention is not limited in scope by the following embodiments; the implementation conditions used in the examples may be further adjusted according to specific requirements, and the implementation conditions not specified are generally those used in routine experiments.
All starting materials are commercially available or prepared by methods conventional in the art, not specifically described in the examples below.
Examples 1 to 4
The preparation method of the rubber for the high-resistance cooling pipeline with high pressure resistance and high temperature resistance comprises the following steps: 1) Mixing: weighing the materials according to the mass ratio, and adding the materials except the vulcanizing agent into a kneader for uniform mixing; 2) Plasticating: adding the mixed sizing material into an internal mixer, and adding a vulcanizing agent to prepare a mixed sizing material for later use; 3) Vulcanizing: vulcanizing the rubber compound on a vulcanizing machine, wherein the vulcanizing temperature is 170 ℃, the pressure is 10MPa, the time is 10min, discharging the rubber after the rubber is finished, cooling, and obtaining the rubber for the low-resistance flame-retardant fuel cell transmission pipeline after the rubber is discharged.
The proportions of the raw materials in examples 1 to 4 are shown in Table 1. The polypyrrole nanotube composite flame retardant is prepared according to the preparation method of the embodiment 5, wherein the conductive agent is one or a combination of acetylene black, carbon fiber, carbon nanotubes and graphite, the colorant is titanium dioxide, and the vulcanizing agent is 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane.
TABLE 1 examples 1-4 Components and proportions
Example 5: preparation of polypyrrole nanotube composite flame retardant
(1) Polypyrrole nanotube synthesis: dissolving pyrrole and a doping agent in deionized water, adding an oxidant, wherein the doping agent is methyl orange, the mass ratio of the pyrrole to the doping agent is 3.5:1, the oxidant is ferric chloride, the mass ratio of the pyrrole to the oxidant is 5:1, mixing and reacting for 30 hours, filtering, washing, and drying at 25 ℃ for 48 hours to obtain the polypyrrole nanotube;
(2) And (3) synthesizing a polypyrrole nanotube composite flame retardant: dispersing the polypyrrole nanotube obtained in the step (1) in a magnesium chloride solution with the mass ratio of the magnesium chloride solution to the polypyrrole of 250:1, stirring uniformly, adding ammonia water to the pH value of 9-10, standing for reaction for 6 hours, filtering, washing and drying to obtain the polypyrrole nanotube composite flame retardant.
Example 6: preparation of polypyrrole nanotube composite flame retardant
(1) Polypyrrole nanotube synthesis: dissolving pyrrole and a doping agent in deionized water, adding an oxidant, wherein the doping agent is methyl orange, the mass ratio of the pyrrole to the doping agent is 3:1, the oxidant is ferric nitrate, the mass ratio of the pyrrole to the oxidant is 6:1, mixing and reacting for 24 hours, filtering, washing, and drying at 20 ℃ for 48 hours to obtain polypyrrole nanotubes;
(2) And (3) synthesizing a polypyrrole nanotube composite flame retardant: dispersing the polypyrrole nanotube obtained in the step (1) in a magnesium sulfate solution with the mass ratio of 0.1mol/L, namely 200:1, stirring uniformly, adding ammonia water to the pH value of 9-10, standing for reaction for 8 hours, filtering, washing and drying to obtain the polypyrrole nanotube composite flame retardant.
Example 7: preparation of polypyrrole nanotube composite flame retardant
(1) Polypyrrole nanotube synthesis: dissolving pyrrole and a doping agent in deionized water, adding an oxidant, wherein the doping agent is beta-naphthalene sulfonic acid, the mass ratio of the pyrrole to the doping agent is 4:1, the oxidant is ammonium persulfate, the mass ratio of the pyrrole to the oxidant is 4:1, mixing, reacting for 36 hours, filtering, washing, and drying at 30 ℃ for 24 hours to obtain polypyrrole nanotubes;
(2) And (3) synthesizing a polypyrrole nanotube composite flame retardant: dispersing the polypyrrole nanotube obtained in the step (1) in a magnesium iodide solution with the mass ratio of 0.6mol/L, namely 300:1, stirring uniformly, adding ammonia water to the pH value of 9-10, standing for 4 hours, filtering, washing and drying to obtain the polypyrrole nanotube composite flame retardant.
Comparative example 1
The comparative example is common silicon rubber, and comprises the following components in parts by weight: 100 parts of vinyl silicone rubber, 45 parts of fumed silica, 3 parts of low-molecular hydroxyl silicone oil and 1.5 parts of biwu.
Comparative example 2
The comparative example differs from example 1 in that the formulation was replaced with magnesium hydroxide in an amount equal to the mass fraction of the composite flame retardant.
Comparative example 3
The comparative example differs from example 1 in that no conductive agent was added to the formulation.
Comparative example 4
This comparative example differs from example 1 in that the composite flame retardant was replaced with carbon nanotubes in the formulation.
TABLE 2 Property parameters of the compounds prepared in examples 1 to 4 and comparative examples 1 to 3
Table 2 shows the performance parameters of the compounds prepared in examples 1 to 4 and comparative examples 1 to 4, wherein the hot air aging performance was tested under the condition of 175℃for 70 hours; the oil resistance test conditions were that the test was carried out in ASTM3# oil at 100deg.C for 70 hours; the test condition of the cold liquid resistance is that the cold liquid is refluxed for 70 hours under the condition of the special cold liquid of hydrogen fuel cell, the Glysantin FC G20-00/50; the test standard of the flame retardant property is referred to EN 45545-2R23 HL2, wherein the requirement on the oxygen index is more than or equal to 28, the requirement on the Ds (max) smoke density is less than or equal to 600, and the requirement on the toxicity test is less than or equal to 1.8; the test conditions for compression set were 70h at 100 ℃; the low temperature performance is that the product is placed at the temperature of minus 40 ℃ for 3min.
As can be seen from Table 2, the rubber materials prepared in examples 1-4 have good flame retardant property due to the addition of the composite flame retardant, and can meet the flame retardant property requirement in EN 45545-2R23 HL2. Meanwhile, the resistance of the rubber material can be obviously reduced, so that the rubber material has good static electricity discharge performance. The resistance of the common silicone rubber prepared in comparative example 1 is obviously larger than that of examples 1-4, and the common silicone rubber does not have flame retardant property and cannot meet the performance requirement of EN 45545-2R23 HL2. In comparative example 2, only magnesium hydroxide is added as a flame retardant, and although the flame retardant performance can meet the requirements, the resistance is still too large, the oil resistance is poor, and the use requirements of a hydrogen energy battery transmission pipeline cannot be met. Comparative example 3 was free of conductive agent added to the formulation, and although the electrical resistance could be reduced due to the conductive properties of the composite flame retardant, it was still higher than examples 1-4. In comparative example 4, the composite flame retardant is completely replaced by the conductive agent in the preparation process, and the obtained rubber material has lower resistance, but does not have flame retardant property, and the mechanical property is greatly changed, so that the hardness is increased, the elasticity is reduced, and the use requirement cannot be met.
Claims (7)
1. The rubber for the low-resistance flame-retardant fuel cell transmission pipeline is characterized by comprising the following components in parts by weight: 90-110 parts of vinyl silicone rubber, 40-60 parts of fumed silica, 20-40 parts of composite flame retardant, 2-4 parts of conductive agent, 1-3 parts of colorant and 1-2 parts of vulcanizing agent; the composite flame retardant is polypyrrole nanotube composite flame retardant, and the conductive agent is one or a combination of acetylene black, carbon fiber, carbon nanotube and graphite;
the preparation method of the polypyrrole nanotube composite flame retardant comprises the following steps:
(1) Polypyrrole nanotube synthesis: dissolving pyrrole and a doping agent in deionized water, adding an oxidizing agent, mixing and reacting for 24-36 hours, filtering, washing, and drying at 20-30 ℃ for 24-48 hours to obtain polypyrrole nanotubes; the doping agent is one of beta-naphthalene sulfonic acid and methyl orange, and the oxidant is one of ammonium persulfate, ferric chloride and ferric nitrate;
(2) And (3) synthesizing a polypyrrole nanotube composite flame retardant: dispersing the polypyrrole nanotube obtained in the step (1) in a magnesium source solution with the concentration of 0.1-1 mol/L, uniformly stirring, adding alkali liquor to the pH value of 9-10, standing for reaction for 4-8 hours, filtering, washing and drying to obtain the polypyrrole nanotube composite flame retardant.
2. The rubber for a low-resistance flame-retardant fuel cell transmission line according to claim 1, wherein in the step (1), the mass ratio of pyrrole to dopant is (3-4): 1.
3. The rubber for a low-resistance flame-retardant fuel cell transfer line according to claim 1, wherein the ratio of the amount of the azole to the amount of the oxidizing agent in the step (1) is (4 to 6): 1.
4. The rubber for a low-resistance flame-retardant fuel cell transmission line according to claim 1, wherein in the step (2), the mass ratio of the magnesium source solution to the polypyrrole is (200-300): 1.
5. The rubber for a low-resistance flame-retardant fuel cell transmission line according to claim 1, wherein in the step (2), the magnesium source solution is one of magnesium chloride, magnesium sulfate and magnesium iodide, and the alkali solution is ammonia water.
6. The rubber for a low-resistance flame-retardant fuel cell transfer line according to claim 1, wherein the coloring agent is titanium dioxide.
7. The rubber for a low-resistance flame-retardant fuel cell transfer line according to claim 1, wherein the vulcanizing agent is 2, 5-dimethyl-2, 5-di (t-butylperoxy) hexane.
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| CN102964838A (en) * | 2012-11-09 | 2013-03-13 | 高润宝 | Nanometer magnesium hydroxide flame retarding silicon rubber composite material and preparation method thereof |
| CN102964595B (en) * | 2012-11-12 | 2014-05-28 | 南昌航空大学 | Preparation method of barium-magnesium ferrite/SDBS (sodium dodecyl benzene sulfonate)-modified carbon nanotube/polypyrrole composite wave-absorbing material |
| CN103840074A (en) * | 2014-02-12 | 2014-06-04 | 中国科学院化学研究所 | Method for preparing composite thermoelectric material of PPY cladding carbon nano tube |
| CN111303636B (en) * | 2020-04-03 | 2021-05-28 | 中国科学院长春应用化学研究所 | Low-heat-conductivity flame-retardant fireproof silicone rubber composite material and preparation method thereof |
| CN113637328B (en) * | 2021-07-21 | 2022-03-25 | 浙江新安化工集团股份有限公司 | Flame-retardant insulating silicone rubber and preparation method thereof |
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