CN114316400A - Rubber cloth-sandwiched diaphragm for hydrogen fuel cell and preparation method thereof - Google Patents
Rubber cloth-sandwiched diaphragm for hydrogen fuel cell and preparation method thereof Download PDFInfo
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- CN114316400A CN114316400A CN202111652298.0A CN202111652298A CN114316400A CN 114316400 A CN114316400 A CN 114316400A CN 202111652298 A CN202111652298 A CN 202111652298A CN 114316400 A CN114316400 A CN 114316400A
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Abstract
The invention relates to the technical field of rubber cloth-sandwiched membranes, and particularly discloses a rubber cloth-sandwiched membrane for a hydrogen fuel cell, which comprises base cloth and a rubber material; the rubber material comprises the following raw materials, 40-45 parts of hydrogenated nitrile rubber, 2-3 parts of zinc oxide, 1-2 parts of an anti-aging agent, 5-10 parts of carbon black, 20-25 parts of an inorganic filler, 3-5 parts of graphene, 1-3 parts of KH550, 3-5 parts of a softening agent, 2-3 parts of DCP, 4-6 parts of maleic anhydride modified polybutadiene, 0.5-1 part of 1# vulcanizing agent and 0.5-1 part of DOTG; the preparation method of the rubber material comprises the following steps: the method comprises the following steps: plasticating hydrogenated nitrile rubber in an internal mixer; step two: firstly, adding an anti-aging agent, inorganic filler, graphene and KH550, heating and mixing; step three: adding carbon black, a softening agent, maleic anhydride modified polybutadiene and DOTG, mixing and discharging rubber; step four: putting the prepared material into an open mill, adding a No. 1 vulcanizing agent and peroxide into the open mill, and thinly passing; step five: the invention obtains rubber material, and strengthens the sealing property of the membrane by optimizing the raw materials and the preparation method.
Description
Technical Field
The invention relates to the technical field of rubber cloth-sandwiched membranes, in particular to a rubber cloth-sandwiched membrane for a hydrogen fuel cell and a preparation method thereof.
Background
A hydrogen fuel cell is a power generation device that directly converts chemical energy of hydrogen and oxygen into electrical energy. The basic principle is the reverse reaction of electrolyzed water, hydrogen and oxygen are supplied to the anode and cathode respectively, and after the hydrogen diffuses out through the anode and reacts with the electrolyte, electrons are released to reach the cathode through an external load.
The cloth clamping membrane is used in the hydrogen fuel cell, and has the sealing function and the pressure regulating function. Because the pressure ratio of the sealed hydrogen is higher, rubber has good elasticity to achieve compression sealing, and also has higher barrier property to hydrogen, the bonding strength of rubber and cloth is high, the existing cloth clamping membrane usually adopts hydrogenated nitrile rubber, but the cross-linking density of the pure hydrogenated nitrile rubber is not high, gas is easy to permeate, the sealing performance has defects, and meanwhile, the strength of the cloth clamping membrane is not high due to the poor bonding property between the hydrogenated nitrile rubber and the base cloth.
Disclosure of Invention
The invention aims to provide a rubber cloth sandwiched membrane for a hydrogen fuel cell and a preparation method thereof, so as to improve the adhesive strength and the sealing performance of a membrane product.
In order to achieve the above purpose, the present application provides the following technical solutions:
a rubber cloth-sandwiched diaphragm for a hydrogen fuel cell comprises base cloth and a rubber material wrapped on the base cloth; the rubber material comprises, by mass, 40-45 parts of hydrogenated nitrile rubber, 2-3 parts of zinc oxide, 1-2 parts of an anti-aging agent, 5-10 parts of carbon black, 20-25 parts of an inorganic filler, 3-5 parts of graphene, 1-3 parts of KH550, 3-5 parts of a softener, 2-3 parts of DCP, 4-6 parts of maleic anhydride modified polybutadiene, 0.5-1 part of a No. 1 vulcanizing agent and 0.5-1 part of DOTG.
The preparation method of the rubber cloth sandwiched membrane for the hydrogen fuel cell is further provided, wherein the preparation method of the rubber material comprises the following steps:
the method comprises the following steps: plasticating: plasticating hydrogenated nitrile rubber in an internal mixer;
step two: mixing for the first time: firstly, adding an anti-aging agent, an inorganic filler, graphene and KH550, heating to 110-120 ℃, and mixing;
step three: and (3) mixing for the second time: adding carbon black, a softening agent, maleic anhydride modified polybutadiene and DOTG, mixing and discharging rubber;
step four: thin passing: putting the mixture prepared in the step three into an open mill, adding a No. 1 vulcanizing agent and peroxide into the open mill, adjusting the roller spacing of the open mill, taking down the mixture after the materials completely pass through the rollers, returning the mixture to the upper part of the rollers, and repeatedly passing through the rollers for multiple times;
step five: and (3) sheet preparation: and C, adjusting the roller distance after the thin passing in the step four, and taking the uniformly extruded material off the roller to obtain the rubber material.
The principle and the advantages of the scheme are as follows: in practical application, in the technical scheme, in order to improve the adhesive strength and the sealing performance of the membrane, a research and development team considers from two aspects of membrane materials and membrane processing methods, firstly, acrylic acid modified hydrogenated nitrile raw rubber is adopted from raw materials of the membrane, various vulcanization modes of peroxide, metal oxide and No. 1 vulcanizing agent can be adopted, the crosslinking density is increased, the gas diffusion is reduced, and further, maleic anhydride modified polybutadiene is adopted as an auxiliary crosslinking agent to increase the adhesive effect; in the preparation method of the diaphragm, the flaky inorganic filler is adopted, the silane coupling agent KH550 is added, and banburying is carried out at the temperature of 110-120 ℃, so that a silanization reaction is carried out, the combination with rubber is increased, the gas barrier capability is increased, and the overall sealing effect of the diaphragm is improved.
Preferably, the hydrogenation degree of the hydrogenated nitrile rubber is 95%, and the hydrogenated nitrile rubber is prepared by acrylic acid polymerization modification with the acrylonitrile content of 33%.
In the technical scheme, the content of acrylonitrile can influence the heat resistance of the nitrile rubber, the unsaturated degree of molecules is reduced,
preferably, the anti-aging agent is anti-aging agent 445; the carbon black is a fast extrusion carbon black.
In the technical scheme, the anti-aging agent 445 and the fast extrusion carbon black are respectively the anti-aging agent and the carbon black commonly used in the field, the raw material source is wide, and the application technology is mature.
Preferably, the inorganic filler is one or more of kaolin, diatomite and sodium metasilicate.
In the technical scheme, the kaolin, the diatomite and the sodium metasilicate are common inorganic fillers, the sources of the raw materials are wide, and the application technology is mature.
Preferably, the softener is trioctyl trimellitate.
In the technical scheme, trioctyl trimellitate is a heat-resistant and durable plasticizer, has the advantages of a polyester plasticizer and a monomer plasticizer, and has better intermiscibility, processability and low temperature compared with the polyester plasticizer.
Preferably, the plastication time in the step one is 80-110 s; the mixing time in the second step is 80-110 s; the mixing time in the third step is 80-110 s, and the thickness of the rubber material in the fifth step is 3 mm.
In the technical scheme, plasticity of internal materials can be effectively increased by controlling plastication time, transitional plastication can lead the interior to be filled with water vapor and low-molecular volatile gas, so that oxygen concentration is reduced, oxidative cracking reaction is slowed down, mixing unevenness is easily caused by too short mixing time, molecular chain fracture sizing materials are easily sticky and mechanical property is reduced, and the quality of rubber is effectively ensured by controlling time.
Preferably, the inorganic filler in the second step is in a flake shape, and the number of thin passes in the fourth step is at least three.
In the technical scheme, the inorganic filler adopts a flaky structure, so that the diffusion path of gas can be increased, the barrier property of the gas is improved, the mixing effect of materials can be increased through multiple thin passes, and the materials are more uniform.
Preferably, the preparation method of the cloth-sandwiched membrane comprises the following steps;
step 1: preparing an adhesive, soaking the base cloth in the adhesive, taking out after soaking, and airing at normal temperature;
step 2: and vulcanizing and molding the rubber material and the base cloth in the mold.
Wherein the adhesive in the step 1 comprises the following raw materials in parts by mass; 1-3 parts of vinyltriethoxysilane, 3-5 parts of TD870 resin, 50-60 parts of absolute ethyl alcohol and 15-25 parts of epoxy resin.
In the technical scheme: the vinyl triethoxysilane can be activated on the surface of the base cloth, the two resins and the cloth form an adhesive layer to improve the adhesive effect, and on the other hand, a chemical bond can be formed to further increase the adhesive strength.
Preferably, the method for preparing the adhesive in the step 1 is to mix and stir the raw materials, wherein the stirring speed is 5 plus or minus 1rad/s, the temperature is 50 plus or minus 5 ℃, the stirring time is 30 plus or minus 2min, and the time for soaking the base cloth in the adhesive is 30 plus or minus 5 s.
In the technical scheme, the stirring speed and time are controlled to ensure the uniformity of the adhesive, so that the surface of the base cloth can be activated to the maximum extent by the vinyltriethoxysilane in the soaking process of the base cloth, and the strength is improved.
Detailed Description
The following is a detailed description of the embodiments, but the embodiments of the present invention are not limited thereto. Unless otherwise specified, the technical means used in the following embodiments are conventional means well known to those skilled in the art; the experimental methods used are all conventional methods; the materials, reagents and the like used are all commercially available.
The scheme is summarized as follows:
example 1
A rubber cloth-sandwiched diaphragm for a hydrogen fuel cell comprises base cloth and a rubber material wrapped on the base cloth; the rubber material comprises, by mass, 40-45 parts of hydrogenated nitrile rubber, 2-3 parts of zinc oxide, 1-2 parts of an anti-aging agent, 5-10 parts of carbon black, 20-25 parts of an inorganic filler, 3-5 parts of graphene, 1-3 parts of KH550, 3-5 parts of a softener, 2-3 parts of DCP, 4-6 parts of maleic anhydride modified polybutadiene, 0.5-1 part of a No. 1 vulcanizing agent and 0.5-1 part of DOTG.
The Chinese name of the No. 1 vulcanizing agent in the raw materials is hexamethylene diamine carbamate, and the molecular formula of the hexamethylene diamine carbamate is C7H16N2O2。
The hydrogenation degree of the hydrogenated nitrile rubber is 95%, the hydrogenated nitrile rubber is prepared by acrylic acid polymerization modification with the acrylonitrile content of 33%, the anti-aging agent is an anti-aging agent 445, the carbon black is fast extrusion carbon black, and the inorganic filler is one or a combination of more of kaolin, diatomite and sodium metasilicate.
A preparation method for manufacturing the rubber cloth-sandwiched membrane for the hydrogen fuel cell comprises the following steps: the method comprises the following steps:
step 1: preparing an adhesive, soaking the base cloth in the adhesive for 30 +/-5 seconds, taking out, and airing at normal temperature;
step 2: and vulcanizing and molding the rubber material and the base cloth in the mold.
Wherein the adhesive in the step 1 comprises the following raw materials in parts by mass: 1-3 parts of vinyltriethoxysilane, 3-5 parts of TD870 resin, 50-60 parts of absolute ethyl alcohol and 15-25 parts of epoxy resin.
The adhesive is prepared by mixing and stirring the raw materials at the stirring speed of 5 +/-1 rad/s and the temperature of 50 +/-5 ℃ for 30 +/-2 min.
In the present embodiment, it is preferable that the soaking time of the base cloth is set to 30 s; in the mixing and stirring process of the adhesive, the stirring speed is 5rad/s, the temperature is 50 ℃, and the stirring time is 30 min.
In the step 2, the preparation method of the rubber material comprises the following steps;
the method comprises the following steps: plasticating: plasticating the hydrogenated nitrile rubber in an internal mixer for 80-110 s;
step two: mixing for the first time: firstly, adding an anti-aging agent, a flaky inorganic filler, graphene and KH550, heating to 110-120 ℃, and mixing for 80-110 s;
step three: and (3) mixing for the second time: adding carbon black, a softening agent, maleic anhydride modified polybutadiene and DOTG, mixing for 80-110 s, and discharging rubber;
step four: thin passing: putting the mixture prepared in the step three into an open mill, adding a No. 1 vulcanizing agent and peroxide into the open mill, adjusting the roller spacing of the open mill, taking down the mixture after the materials completely pass through the rollers, returning the mixture to the upper part of the rollers, and repeatedly passing through the rollers for multiple times;
step five: and (3) sheet preparation: and (5) adjusting the roller distance after the thin passing in the step four, and taking the uniformly extruded material off the roller to obtain the rubber material with the thickness of 3 mm.
In this embodiment, preferably, in the step one, the plastication time is controlled to be 90s, in the step two, the mixing time is controlled to be 90s, the temperature rise is controlled to be 120 ℃, in the step three, the mixing time is controlled to be 90s, and in the step four, the number of the thin passes is three.
Examples 2 to 3 and comparative example 1
The difference from the example 1 lies in the different proportions of the components, wherein the rubber material has the following composition proportion in table 1, and the adhesive has the following composition proportion in table 2.
Table 1 shows the composition ratios (by weight) of the rubber materials in examples 1 to 3 and comparative example 1
Table 2 shows the composition ratios of the binders in examples 1 and 4 to 5, and the binder components and the amounts added in examples 2 and 3 are the same as those in example 1.
Comparative example 3:
the difference from example 1 is that: the flaky inorganic filler used in example 1 was replaced with a powdery inorganic filler, while KH550 was not added inside.
Comparative example 4:
the difference from example 1 is that: the inorganic filler in the flake form used in example 1 was replaced with an inorganic filler in the powder form.
Comparative example 5:
the difference from example 1 is that: no KH550 was added internally.
Comparative example 6:
the difference from example 1 is that: the maleic anhydride-modified polybutadiene used in example 1 was replaced with a usual polybutadiene.
Comparative example 7:
the difference from example 1 is that: the acrylic modified hydrogenated nitrile rubber used in example 1 was replaced with unmodified hydrogenated nitrile rubber.
The cloth-sandwiched membranes obtained in examples 1-5 and comparative examples 1-7 were subjected to performance tests, test methods and standards: the hydrogen permeability coefficient was measured by VAC-V2 of the company Jinan Languang, the gas permeability coefficient was measured in GB/T1038, and the adhesion strength between rubber and cloth was measured in GB/T11211-1998 in units of (KN/M), and the results were expressed as an average in each group in triplicate, and the results are shown in Table 3.
In summary, the following steps:
1. as can be seen from table 3, it is,the hydrogen permeability coefficient and the adhesive strength of the rubber and the cloth in examples 1 to 5 are both larger than those in comparative examples 1 to 7, wherein the adhesive strength of the rubber and the cloth in example 1 is as high as 3.01, and the hydrogen permeability coefficient reaches 0.6510-17m2/(Pa.s), it can be obtained that the cloth-sandwiched rubber diaphragm prepared by the technical scheme of the invention has obvious advantages.
2. The bonding strength between the rubber layer and the base cloth in the cloth-sandwiched rubber diaphragm obtained by the invention is obviously higher than that of comparative examples 1-7, the acrylic acid modified hydrogenated nitrile raw rubber is adopted in the invention, and the various vulcanization modes of peroxide, metal oxide and No. 1 vulcanizing agent can be adopted, so that the crosslinking density is increased, the gas diffusion is reduced, the rubber in a final product is not perfectly attached to the base cloth due to low viscosity between the base cloth and the rubber, and the maleic anhydride modified polybutadiene is adopted as an auxiliary crosslinking agent in the formula, so that the bonding effect is increased; in the preparation method of the diaphragm, the flaky inorganic filler is adopted, the silane coupling agent KH550 is added, and banburying is carried out at the temperature of 110-120 ℃, so that a silanization reaction is carried out, the combination with rubber is increased, the gas barrier capability is increased, and the overall sealing effect of the diaphragm is improved.
Comparative examples 1 and 2 are respectively insufficient or excessive maleic anhydride modified polybutadiene, and it can be seen from examination of the final experimental data that the insufficient or excessive maleic anhydride modified polybutadiene adversely affects the hydrogen permeability coefficient of the product and the adhesive strength between the rubber and the cloth, and comparative examples 3, 4 and 5 show that the inorganic filler and the KH550 are adjusted, so that the hydrogen permeability coefficient of the product and the adhesive strength between the rubber and the cloth can be affected to a certain extent, the maleic anhydride modified polybutadiene used in comparative example 6 is replaced by the conventional polybutadiene, the hydrogen permeability coefficient of the product and the adhesive strength between the rubber and the cloth are also low, the acrylic modified hydrogenated nitrile rubber used in comparative example 7 is replaced by the unmodified hydrogenated nitrile rubber, the hydrogen permeability coefficient of the product and the adhesive strength between the rubber and the cloth are lowest, the acrylic acid modified hydrogenated nitrile raw rubber can be enhanced to a certain degree under a 1# vulcanizing agent and peroxide composite vulcanizing system, the crosslinking density is increased, and the gas diffusion is reduced, so that the strength and the sealing effect of the cloth-sandwiched rubber are further improved, the final barrier capability of the cloth-sandwiched diaphragm is effectively improved by the cooperation between KH550 and the flaky inorganic filler, the overall strength of the diaphragm can be effectively improved by adopting the maleic anhydride modified polybutadiene as the auxiliary crosslinking agent, and the diaphragm produced by the invention has obvious advantages.
The diaphragm prepared by the invention has high bonding degree and good bonding property between the rubber material and the base cloth, and the prepared diaphragm has strong sealing capability, can effectively reduce the diffusion of gas and avoids the loss of hydrogen.
The foregoing is merely an example of the present invention and common general knowledge in the art of designing and/or characterizing particular aspects and/or features is not described in any greater detail herein. It should be noted that, for those skilled in the art, without departing from the technical solution of the present invention, several variations and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.
Claims (10)
1. A rubber cloth-sandwiched diaphragm for a hydrogen fuel cell comprises base cloth and a rubber material wrapped on the base cloth; the method is characterized in that: the rubber material comprises, by mass, 40-45 parts of hydrogenated nitrile rubber, 2-3 parts of zinc oxide, 1-2 parts of an anti-aging agent, 5-10 parts of carbon black, 20-25 parts of an inorganic filler, 3-5 parts of graphene, 1-3 parts of KH550, 3-5 parts of a softener, 2-3 parts of DCP, 4-6 parts of maleic anhydride modified polybutadiene, 0.5-1 part of a No. 1 vulcanizing agent and 0.5-1 part of DOTG.
2. The rubber-cloth-sandwiched membrane for a hydrogen fuel cell according to claim 1, characterized in that: the hydrogenation degree of the hydrogenated nitrile rubber is 95%, and the hydrogenated nitrile rubber is prepared by acrylic acid polymerization modification with the acrylonitrile content of 33%.
3. The rubber-cloth-sandwiched membrane for a hydrogen fuel cell according to claim 1, characterized in that: the anti-aging agent is anti-aging agent 445; the carbon black is a fast extrusion carbon black.
4. The rubber-cloth-sandwiched membrane for a hydrogen fuel cell according to claim 1, characterized in that: the inorganic filler is one or a combination of more of kaolin, diatomite and sodium metasilicate.
5. The rubber-cloth-sandwiched membrane for a hydrogen fuel cell according to claim 1, characterized in that: the softener is trioctyl trimellitate.
6. A production method for producing the rubber-cloth-sandwiched membrane for a hydrogen fuel cell according to any one of claims 1 to 5, characterized in that: the preparation method of the rubber material comprises the following steps:
the method comprises the following steps: plasticating: plasticating hydrogenated nitrile rubber in an internal mixer;
step two: mixing for the first time: firstly, adding an anti-aging agent, an inorganic filler, graphene and KH550, heating to 110-120 ℃, and mixing;
step three: and (3) mixing for the second time: adding carbon black, a softening agent, maleic anhydride modified polybutadiene and DOTG, mixing and discharging rubber;
step four: thin passing: putting the mixture prepared in the step three into an open mill, adding a No. 1 vulcanizing agent and peroxide into the open mill, adjusting the roller spacing of the open mill, taking down the mixture after the materials completely pass through the rollers, returning the mixture to the upper part of the rollers, and repeatedly passing through the rollers for multiple times;
step five: and (3) sheet preparation: and C, adjusting the roller distance after the thin passing in the step four, and taking the uniformly extruded material off the roller to obtain the rubber material.
7. The method for producing a rubber-cloth-sandwiched membrane for a hydrogen fuel cell according to claim 6, characterized in that: in the first step, the plastication time is 80-110 s; the mixing time in the second step is 80-110 s; the mixing time in the third step is 80-110 s, and the thickness of the rubber material obtained in the fifth step is 3 mm.
8. The method for producing a rubber-cloth-sandwiched membrane for a hydrogen fuel cell according to claim 6, characterized in that: the inorganic filler in the second step is flaky, and the number of thin passing in the fourth step is at least three.
9. The method for producing a rubber-cloth-sandwiched membrane for a hydrogen fuel cell according to claim 6, characterized in that: the preparation method of the cloth-sandwiched membrane comprises the following steps;
step 1: preparing an adhesive, soaking the base cloth in the adhesive, taking out after soaking, and airing at normal temperature;
step 2: vulcanizing and molding the rubber material and the base cloth in a mold;
wherein the adhesive in the step 1 comprises the following raw materials in parts by mass: 1-3 parts of vinyltriethoxysilane, 3-5 parts of TD870 resin, 50-60 parts of absolute ethyl alcohol and 15-25 parts of epoxy resin.
10. The method for producing a rubber-cloth-sandwiched membrane for a hydrogen fuel cell according to claim 6, characterized in that: the method for preparing the adhesive in the step 1 is to mix and stir the raw materials, wherein the stirring speed is 5 +/-1 rad/s, the temperature is 50 +/-5 ℃, the stirring time is 30 +/-2 min, and the time for soaking the base cloth in the adhesive is 30 +/-5 s.
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| CN202111652298.0A CN114316400A (en) | 2021-12-30 | 2021-12-30 | Rubber cloth-sandwiched diaphragm for hydrogen fuel cell and preparation method thereof |
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2021
- 2021-12-30 CN CN202111652298.0A patent/CN114316400A/en active Pending
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Application publication date: 20220412 |