CN109950556B - Preparation method of carbon fiber bipolar plate with three-dimensional porous structure - Google Patents
Preparation method of carbon fiber bipolar plate with three-dimensional porous structure Download PDFInfo
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Abstract
A preparation method of a carbon fiber bipolar plate with a three-dimensional porous structure comprises the steps of taking a polypropylene cyano carbon fiber graphite felt as a conductive filler and a reinforcement material, taking an epoxy resin matrix and taking paraffin as a hole sealing agent, and preparing a polypropylene cyano carbon fiber graphite felt/epoxy resin prepreg and a polypropylene cyano carbon fiber graphite felt/paraffin prepreg by a hot dipping method; preparing a bipolar plate containing paraffin by adopting a hot press molding process; removing paraffin in the bipolar plate by a later dewaxing process to finally obtain the bipolar plate with the double-sided carbon fiber porous structure. The invention has simple preparation process, low preparation cost and little environmental pollution; the adopted epoxy resin matrix and the carbon fiber conductive material in the polypropylene cyano carbon fiber graphite felt have strong bonding force, and the prepared carbon fiber bipolar plate has high mechanical strength, excellent electrochemical corrosion resistance and excellent electrical conductivity; the preparation process is easy to control and is suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of engineering material preparation, and particularly relates to a preparation method of a carbon fiber bipolar plate with a three-dimensional porous structure.
Background
In the technical field of flow battery energy storage, such as redox flow batteries including all-vanadium flow batteries, lead flow batteries and the like, the bipolar plate is one of the key components of the flow battery and provides an electrode reaction site. Due to the long-time charge and discharge state, especially under the condition of charging on the positive side of the bipolar plate, the electrochemical corrosion is serious to the bipolar plate, which can cause the performance deterioration, such as the reduction of the conductivity and the mechanical strength, and the service life of the bipolar plate is shortened. Therefore, the bipolar plate electrode material has high oxidation resistance and corrosion resistance, so that the service life of the electrode material is ensured; secondly, the bipolar plate electrode material has excellent conductivity, ohmic voltage drop in the charging and discharging process is reduced, the voltage efficiency of the battery is improved, and meanwhile, the energy loss of current in the electrode plate transmission process can be reduced, and the energy efficiency of the battery is improved; finally, the bipolar plate electrode material should have good mechanical strength to meet the strength requirements of the battery during assembly.
At present, redox flow batteries such as all-vanadium flow batteries and lead flow batteries mainly adopt conductive filler/polymer matrix composite materials, wherein the conductive filler mainly comprises carbon materials including carbon black, graphite powder, carbon fibers and the like, the polymer comprises thermoplastic resins such as polypropylene, polyethylene, polytetrafluoroethylene and the like, and thermosetting resins such as epoxy resin, phenolic resin and the like. The conductive composite material has the characteristics of light weight, easy processing, low cost and the like, and is widely adopted, and the conductivity is more than 10S/cm; the bending strength is more than 40 MPa; the electrochemical corrosion rate is less than 15 mu A/cm2. However, since the carbon material electrochemically oxidized at the positive electrode side, such as carbon black and graphite powder, is easily oxidized after long-term use, the electrochemical corrosion phenomenon is serious especially for a system with high oxidation electrode potential, and thus the service life of the battery is severely limited.
Disclosure of Invention
The invention aims to provide a carbon fiber bipolar plate with a three-dimensional porous structure, which has the characteristics of improving the conductivity and mechanical property of the existing composite material electrode plate and effectively improving the electrochemical corrosion resistance of the existing composite material electrode plate.
The invention adopts the technical scheme that the preparation method of the carbon fiber bipolar plate with the three-dimensional porous structure is implemented according to the following steps:
step 1, preparing epoxy resin glue solution and paraffin liquid;
step 2, preparing a polypropylene cyano carbon fiber graphite felt/epoxy resin prepreg by using the polypropylene cyano carbon fiber graphite felt;
step 3, preparing two same polypropylene cyano carbon fiber graphite felt/paraffin prepreg by using two same polypropylene cyano carbon fiber graphite felts;
step 4, pressing an electrode plate with two sides containing paraffin by using a polypropylene cyano carbon fiber graphite felt/epoxy resin prepreg and two same polypropylene cyano carbon fiber graphite felt/paraffin prepreg;
and 5, performing dewaxing treatment on the electrode plate with paraffin on two surfaces obtained in the step 4 to obtain the carbon fiber bipolar plate with a porous structure on two surfaces.
The invention is also characterized in that:
the step 1 is implemented according to the following steps:
step 1.1, mixing epoxy resin, a cross-linking agent and a catalyst, and magnetically stirring for 10-30 minutes at the temperature of 50-70 ℃ to obtain an oxygen resin glue solution;
step 1.2, liquefying the paraffin by using 110-130 ℃ silicone oil to obtain paraffin liquid.
The step 2 is implemented according to the following steps:
step 2.1, completely soaking the polypropylene cyano carbon fiber graphite felt in the epoxy resin glue solution obtained in the step 1 for 1-5 minutes;
and 2.2, after the impregnation is finished, taking out the prepreg and placing the prepreg on silicone oil paper, and then adhering a layer of silicone oil paper on the surface of the prepreg to obtain the polypropylene cyano carbon fiber graphite/epoxy resin prepreg.
Step 3 is specifically implemented according to the following steps:
step 3.1, flatly putting two same polypropylene cyano carbon fiber graphite felts into paraffin liquid, and soaking for 1-5 minutes;
and 3.2, after the impregnation is finished, taking out the prepreg and placing the prepreg on silicone oil paper, adhering a layer of silicone oil paper on the surface of the prepreg, and curing and sealing holes by paraffin at room temperature to obtain two same pieces of polypropylene cyano carbon fiber graphite felt/paraffin prepreg.
Step 4 is specifically implemented according to the following steps:
after silicone oil paper on the surfaces of the three prepregs obtained in the steps 2 and 3 is removed, sequentially putting the three prepregs into a hot-pressing die, and placing the three prepregs in the middle to be in contact stacking with the upper and lower polypropylene cyano carbon fiber graphite felt/paraffin prepreg layers without sealing one side with paraffin;
step 4.2, closing the grinding tool, then heating to 80 ℃ at the speed of 1-3 ℃/min, preserving the temperature for 180 minutes, and then gelling at the temperature of 100 ℃ and 150kgf/cm2Hot-press forming;
and 4.3, after forming, heating to 130 ℃ at the speed of 1-3 ℃/min, preserving the heat for 60-90 minutes, finally cooling to room temperature, releasing the pressure and taking out to obtain the electrode plate with paraffin on two sides.
Step 5 is specifically implemented according to the following steps:
step 5.1, placing the electrode plate with paraffin on both sides obtained in the step 4 into 120-150 ℃ silicone oil to remove the paraffin, then placing the electrode plate into 40 mass percent NaOH aqueous solution, and soaking the electrode plate for 2-3 hours at 80-90 ℃;
step 5.2, taking out the mixture after soaking, and transferring the mixture into a boiling oxalic acid solution with the mass percentage of 15% for soaking for 2-3 hours;
and 5.3, finishing soaking, and finally, sequentially carrying out ultrasonic cleaning in acetone and deionized water for 8-10 minutes to obtain the carbon fiber bipolar plate with the porous structure on both sides.
Preparing epoxy resin glue solution in the step 1, wherein the weight percentage of each component is as follows: a crosslinking agent: the catalyst is 100: 80-90: 0.1-0.3.
In the step 1, the epoxy resin is bisphenol A type and has the molecular weight of 300-700; the cross-linking agent is adipic acid; the catalyst is benzyl dimethylamine; the paraffin wax is microcrystalline wax No. 90.
The invention has the beneficial effects that:
1. the method adopts the polypropylene cyano carbon fiber graphite felt with high conductivity as the conductive material and the reinforcement material, the epoxy resin as the matrix, and the paraffin as the porous structure protective agent, so that the material source is rich and the cost is low.
2. The preparation method comprises the steps of preparing a polypropylene cyano carbon fiber graphite felt prepreg by infiltration of an epoxy resin glue solution and paraffin, preparing an electrode plate with paraffin on two sides by adopting a hot pressing process from the polypropylene cyano carbon fiber graphite felt/paraffin prepreg-polypropylene cyano carbon fiber graphite felt/resin glue solution prepreg-polypropylene cyano carbon fiber graphite felt/paraffin prepreg, wherein the intermediate compact layer (a conductive layer of the polypropylene cyano carbon fiber graphite felt/epoxy resin composite material) has high conductivity, mechanical property and electrochemical corrosion resistance.
3. The bipolar plate with the three-dimensional porous structure can be prepared by a simple dewaxing process, and the material can be used as a redox flow battery bipolar plate, and particularly a lead flow battery, can improve electrochemical corrosion resistance, improve battery efficiency and prolong the service life of the battery.
Drawings
Fig. 1 is a process flow diagram of a method for manufacturing a carbon fiber bipolar plate having a three-dimensional porous structure according to the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a preparation method of a carbon fiber bipolar plate with a three-dimensional porous structure, which is implemented according to the following steps:
step 1, preparing epoxy resin glue solution and paraffin liquid;
step 2, preparing a polypropylene cyano carbon fiber graphite felt/epoxy resin prepreg by using the polypropylene cyano carbon fiber graphite felt;
step 3, preparing two same polypropylene cyano carbon fiber graphite felt/paraffin prepreg by using two same polypropylene cyano carbon fiber graphite felts;
step 4, pressing an electrode plate with two sides containing paraffin by using a polypropylene cyano carbon fiber graphite felt/epoxy resin prepreg and two same polypropylene cyano carbon fiber graphite felt/paraffin prepreg;
and 5, performing dewaxing treatment on the electrode plate with paraffin on two surfaces obtained in the step 4 to obtain the carbon fiber bipolar plate with a porous structure on two surfaces.
The step 1 is implemented according to the following steps:
step 1.1, sequentially weighing and adding epoxy resin, a cross-linking agent and a catalyst into a beaker, and magnetically stirring for 10-30 minutes at the temperature of 50-70 ℃ to fully mix the epoxy resin, the cross-linking agent and the catalyst to obtain a light yellow epoxy resin glue solution;
step 1.2, weighing paraffin and pouring the paraffin into a glass groove, adding the paraffin into an oil bath kettle to 110-;
in the step 1, epoxy resin glue solution A is prepared, and the weight percentages of the components are as follows: a crosslinking agent: the catalyst is 100: 80-90: 0.1-0.3.
Wherein, the epoxy resin is bisphenol A type epoxy resin which is thermosetting resin, has good bonding strength and chemical resistance, the molecular weight is preferably 300-700, the commercial brands are E-42, E-44 and E-51, and the softening point is less than 30 ℃;
the cross-linking agent is adipic acid which is an organic dicarboxylic acid, and organic functional group carboxylic acid can be esterified with an epoxy group in the epoxy resin to generate macromolecules with a net structure;
the catalyst is benzyl dimethylamine which is organic tertiary amine and can catalyze the cross-linking agent oxalic acid to provide negative ion active center and promote the polymerization reaction of the epoxy resin and the cross-linking agent anion;
the paraffin serves as a hole sealing protector of a porous carbon fiber polypropylene cyano carbon fiber graphite felt, is No. 90 microcrystalline wax, and is characterized in that odorless and tasteless white amorphous solid wax is mainly branched saturated hydrocarbon, contains a small amount of cyclic and straight-chain hydrocarbon, has the density of about 0.9 g/mL, has the melting point of more than 90 ℃, and can retain the porous structure of the polypropylene cyano carbon fiber graphite felt through the processes of high-temperature infiltration, low-temperature curing, high-temperature dewaxing and the like;
after the mixed glue solution of the epoxy resin, the cross-linking agent and the catalyst is cured at high temperature, the elastic modulus of the mixed glue solution is more than 3GPa, and the mixed glue solution can be tightly bonded with carbon fibers in a polypropylene cyano carbon fiber graphite felt to prepare a plate with certain mechanical property, conductive function and electrochemical corrosion resistance.
The step 2 is implemented according to the following steps:
step 2.1, completely dipping the polypropylene cyano carbon fiber graphite felt into the glass containing the epoxy resin glue solution obtained in the step 1 for 1-5 minutes;
and 2.2, after the impregnation is finished, taking out the prepreg and placing the prepreg on silicone oil paper, and then attaching a layer of silicone oil paper on the surface of the prepreg to obtain the polypropylene cyano carbon fiber graphite felt/epoxy resin prepreg.
In the step 2, the bulk density of the polypropylene cyano carbon fiber graphite felt is 0.1-0.15g/cm3Carbon content greater than 99%, polypropylene cyano carbon fiberThe conductivity of the polypropylene cyano carbon fiber in the graphite felt is more than 1 multiplied by 102S/cm. The polypropylene cyano carbon fiber graphite felt is used as a conductive filler, a three-dimensional porous structure can be provided, a large number of active points are provided for electrode reaction, and the battery efficiency is improved; meanwhile, the composite material can be used as a reinforcement to improve the bending strength of the plate; in addition, the polypropylene cyano carbon fiber has high electrochemical corrosion resistance and good chemical stability, and can improve the service life of the bipolar plate.
The resin takes a polypropylene cyano carbon fiber graphite felt as a conductive material, and the length, the width and the thickness of the polypropylene cyano carbon fiber graphite felt are 10cm, 10cm and 0.5 cm.
Step 3 is specifically implemented according to the following steps:
step 3.1, flatly placing two same polypropylene cyano carbon fiber graphite felts into the glass tank filled with paraffin liquid in the step 2, and soaking for 1-5 minutes;
and 3.2, after the impregnation is finished, taking out the prepreg and placing the prepreg on silicone oil paper, adhering a layer of silicone oil paper on the surface of the prepreg, and curing and sealing holes by paraffin at room temperature to obtain two same pieces of polypropylene cyano carbon fiber graphite felt/paraffin prepreg.
In the step 3.2, the thickness of the paraffin hole sealing is 4-5 mm.
In the step 3, the polypropylene cyano carbon fiber graphite felt is a conductive material, and the length, the width and the thickness of the polypropylene cyano carbon fiber graphite felt are 10cm, 10cm and 1 cm.
Step 4 is as shown in fig. 1, and is specifically implemented according to the following steps:
step 4.1, after silicone oil paper on the surfaces of the three prepregs obtained in the steps 2 and 3 is removed, sequentially putting the three prepregs into a hot-pressing die, and placing the three prepregs in the middle to be in contact stacking with the upper and lower polypropylene cyano carbon fiber graphite felt/paraffin prepreg on the side without sealing holes with paraffin;
step 4.2, closing the grinding tool, then heating to 80 ℃ at the speed of 1-3 ℃/min, preserving the temperature for 180 minutes, and then gelling at the temperature of 100 ℃ and 150kgf/cm2Hot-press forming;
and 4.3, after forming, heating to 130 ℃ at the speed of 1-3 ℃/min, preserving the heat for 60-90 minutes, finally cooling to room temperature along with a furnace, releasing the pressure and taking out to obtain the electrode plate with paraffin on two sides.
Step 5 is specifically implemented according to the following steps:
step 5.1, placing the electrode plate with paraffin on both sides in the step 4 into 120-150 ℃ silicon oil to remove the paraffin, then placing the electrode plate into 40 mass percent NaOH aqueous solution, and soaking the electrode plate for 2-3 hours at 80-90 ℃;
step 5.2, taking out the mixture after soaking, and transferring the mixture into a boiling oxalic acid solution with the mass percentage of 15% for soaking for 2-3 hours;
and 5.3, finishing soaking, and finally, sequentially carrying out ultrasonic cleaning in acetone and deionized water for 8-10 minutes to obtain the bipolar plate with the porous structure on both sides.
The performance test of the prepared bipolar plate needs to be explained, and according to the report of the literature, the conductivity of the polypropylene cyano carbon fiber is more than 1 x 102S/cm, the electrochemical corrosion resistance meets the requirements of the flow battery, and the performance test is mainly carried out on a middle compact layer of the bipolar plate, namely a polypropylene cyano carbon fiber graphite felt/epoxy resin conducting layer. After removing the porous polypropylene cyano carbon fiber graphite felts on the two sides of the bipolar plate, measuring the conductivity of the middle compact layer by adopting a four-probe method, wherein the conductivity is more than 1 multiplied by 102S/cm; according to the national standard GB1449-2005-T, the bending strength of the middle compact layer measured by a three-point bending method is more than 59 MPa; h at 3M2SO4Adopting an electrochemical linear polarization method as electrolyte to obtain the intermediate compact layer with the corrosion rate less than 1 muA/cm2。
Example 1
Step 1, preparing an epoxy resin solution and paraffin liquid;
step 1.1, taking epoxy resin as a matrix, and enabling the weight percentage to meet the following requirements: a crosslinking agent: sequentially weighing the epoxy resin, the cross-linking agent and the catalyst, adding the epoxy resin, the cross-linking agent and the catalyst into a beaker, and magnetically stirring the mixture for 10 minutes at the temperature of 50 ℃ to fully mix the epoxy resin, the cross-linking agent and the catalyst to obtain a light yellow epoxy resin glue solution;
step 1.2, weighing edible paraffin, pouring the edible paraffin into a glass groove, adding the edible paraffin into the glass groove by using an oil bath pan to 110 ℃, and completely liquefying the edible paraffin to obtain low-viscosity paraffin liquid with the thickness of 4 mm;
step 2, preparing a polypropylene cyano carbon fiber graphite felt/epoxy resin prepreg by using the polypropylene cyano carbon fiber graphite felt;
step 2.1, completely dipping the polypropylene cyano carbon fiber graphite felt into the glass containing the epoxy resin glue solution obtained in the step 1 for 1 minute, wherein the specification of the polypropylene cyano carbon fiber graphite felt is as follows: the dimensions of length × width × thickness are 10cm × 10cm × 0.5 cm;
and 2.2, after the impregnation is finished, taking out the prepreg and placing the prepreg on silicone oil paper, and then attaching a layer of silicone oil paper on the surface of the prepreg to obtain the polypropylene cyano carbon fiber graphite felt/epoxy resin prepreg.
Step 3, preparing two same polypropylene cyano carbon fiber graphite felt/paraffin prepreg by using two same polypropylene cyano carbon fiber graphite felts;
step 3.1, flatly placing two pieces of polypropylene cyano carbon fiber graphite felt which are made of the same material in the step 2 into a glass tank filled with paraffin liquid in the step 2, and soaking for 1 minute, wherein the polypropylene cyano carbon fiber graphite felt is in the specification: the dimensions of length × width × thickness are 10cm × 10cm × 1 cm;
and 3.2, after the impregnation is finished, taking out the obtained product and placing the obtained product on silicone oil paper, adhering a layer of silicone oil paper on the surface of the obtained product, and sealing holes by paraffin curing at room temperature to obtain two same pieces of polypropylene cyano carbon fiber graphite felt/paraffin prepreg, wherein the thickness of the paraffin sealed holes is 4 mm.
Step 4, pressing an electrode plate with two sides containing paraffin by using a polypropylene cyano carbon fiber graphite felt/epoxy resin prepreg and two same polypropylene cyano carbon fiber graphite felt/paraffin prepreg;
step 4.1, after silicone oil paper on the surfaces of the three prepregs obtained in the steps 2 and 3 is removed, sequentially putting the three prepregs into a hot-pressing die, and placing the three prepregs in the middle to be in contact stacking with the upper and lower polypropylene cyano carbon fiber graphite felt/paraffin prepreg on the side without sealing holes with paraffin;
step 4.2, closing the grinding tool, and then heating to 1 DEG CHeating to 80 deg.C at a rate of/min, keeping the temperature for 120 min, and gelling at 100kgf/cm2Hot-press forming;
and 4.3, after forming, heating to 130 ℃ at the speed of 1 ℃/min, preserving the heat for 60 minutes, finally cooling to room temperature along with a furnace, releasing the pressure and taking out to obtain the electrode plate with paraffin on two sides.
Step 5, the electrode plate with double surfaces containing paraffin wax obtained in the step 4 is subjected to paraffin removal treatment to prepare a carbon fiber bipolar plate with double surfaces in a porous structure;
step 5.1, placing the electrode plate with double sides containing paraffin wax obtained in the step 4 into silicone oil at 120 ℃ to remove the paraffin wax, then placing the electrode plate into NaOH aqueous solution with the mass percentage of 40%, and soaking the electrode plate for 2 hours at 80 ℃;
step 5.2, taking out the mixture after soaking, and moving the mixture into a boiling oxalic acid solution with the mass percentage of 15% for soaking for 2 hours;
and 5.3, finishing soaking, and finally, sequentially carrying out ultrasonic cleaning in acetone and deionized water for 8 minutes to obtain the bipolar plate with the porous structure on both sides.
The performance of the prepared polypropylene cyano carbon fiber graphite felt/epoxy resin compact layer in the middle of the bipolar plate is tested, and the conductivity of the conductive plate is 2.3 multiplied by 102S/cm; the bending strength is 64 MPa; the corrosion rate is 0.2 muA/cm2。
Example 2
Step 1, preparing an epoxy resin solution and paraffin liquid;
step 1.1, taking epoxy resin as a matrix, and enabling the weight percentage to meet the following requirements: a crosslinking agent: sequentially weighing the epoxy resin, the cross-linking agent and the catalyst, adding the epoxy resin, the cross-linking agent and the catalyst into a beaker, and magnetically stirring the mixture for 14 minutes at the temperature of 54 ℃ to fully mix the epoxy resin, the cross-linking agent and the catalyst to obtain a light yellow epoxy resin glue solution;
step 1.2, weighing the edible paraffin, pouring the edible paraffin into a glass groove, adding the edible paraffin into the glass groove by using an oil bath pan to 120 ℃, and completely liquefying the edible paraffin to obtain low-viscosity paraffin liquid with the thickness of 4 mm.
Step 2, preparing a polypropylene cyano carbon fiber graphite felt/epoxy resin prepreg by using the polypropylene cyano carbon fiber graphite felt;
step 2.1, completely dipping the polypropylene cyano carbon fiber graphite felt into the glass containing the epoxy resin glue solution obtained in the step 1 for 3 minutes, wherein the specification of the polypropylene cyano carbon fiber graphite felt is as follows: the dimensions of length × width × thickness are 10cm × 10cm × 0.5 cm;
and 2.2, after the impregnation is finished, taking out the prepreg and placing the prepreg on silicone oil paper, and then attaching a layer of silicone oil paper on the surface of the prepreg to obtain the polypropylene cyano carbon fiber graphite felt/epoxy resin prepreg.
Step 3, preparing two same polypropylene cyano carbon fiber graphite felt/paraffin prepreg by using two same polypropylene cyano carbon fiber graphite felts;
step 3.1, flatly placing two pieces of polypropylene cyano carbon fiber graphite felt which are made of the same material in the step 2 into a glass tank filled with paraffin liquid in the step 2, and soaking for 4 minutes, wherein the polypropylene cyano carbon fiber graphite felt is in the specification: the dimensions of length × width × thickness are 10cm × 10cm × 1 cm;
and 3.2, after the impregnation is finished, taking out and placing the impregnated paper on silicone oil paper, adhering a layer of silicone oil paper on the surface, and sealing holes by paraffin curing at room temperature to obtain two same pieces of polypropylene cyano carbon fiber graphite felt/paraffin prepreg, wherein the thickness of the paraffin sealed holes is 5 mm.
Step 4, pressing an electrode plate with two sides containing paraffin by using a polypropylene cyano carbon fiber graphite felt/epoxy resin prepreg and two same polypropylene cyano carbon fiber graphite felt/paraffin prepreg;
step 4.1, after silicone oil paper on the surfaces of the three prepregs obtained in the steps 2 and 3 is removed, sequentially putting the three prepregs into a hot-pressing die, and placing the three prepregs in the middle to be in contact stacking with the upper and lower polypropylene cyano carbon fiber graphite felt/paraffin prepreg on the side without sealing holes with paraffin;
step 4.2, closing the grinding tool, heating to 80 ℃ at the speed of 3 ℃/min, keeping the temperature for 170 minutes, and gelling at 120kgf/cm2Hot-press forming;
and 4.3, after forming, heating to 130 ℃ at the speed of 2 ℃/min, preserving the heat for 70 minutes, finally cooling to room temperature along with a furnace, releasing the pressure and taking out to obtain the electrode plate with paraffin on two sides.
Step 5, the electrode plate with double surfaces containing paraffin wax obtained in the step 4 is subjected to paraffin removal treatment to prepare a carbon fiber bipolar plate with double surfaces in a porous structure;
step 5.1, placing the electrode plate with double sides containing paraffin wax obtained in the step 4 into silicone oil at 150 ℃ to remove the paraffin wax, then placing the electrode plate into NaOH aqueous solution with the mass percentage of 40%, and soaking the electrode plate for 2 hours at 80 ℃;
step 5.2, taking out the mixture after soaking, and moving the mixture into a boiling oxalic acid solution with the mass percentage of 15% for soaking for 2 hours;
and 5.3, finishing soaking, and finally, sequentially carrying out ultrasonic cleaning in acetone and deionized water for 9 minutes to prepare the bipolar plate with the porous structure on both sides.
The performance of the prepared polypropylene cyano carbon fiber graphite felt/epoxy resin compact layer in the middle of the bipolar plate is tested, and the conductivity of the conductive plate is 1.9 multiplied by 102S/cm; the bending strength is 63 MPa; the corrosion rate is 0.44 mu A/cm2。
Example 3
Step 1, preparing an epoxy resin solution and paraffin liquid;
step 1.1, taking epoxy resin as a matrix, and enabling the weight percentage to meet the following requirements: a crosslinking agent: sequentially weighing the epoxy resin, the cross-linking agent and the catalyst into a beaker, and magnetically stirring for 20 minutes at the temperature of 60 ℃ to fully mix the epoxy resin, the cross-linking agent and the catalyst to obtain a light yellow epoxy resin glue solution, wherein the ratio of the catalyst to the cross-linking agent to the catalyst is 100: 85: 0.2;
step 1.2, weighing the edible paraffin, pouring the edible paraffin into a glass groove, adding the edible paraffin into the glass groove by using an oil bath pan to 118 ℃, and completely liquefying the edible paraffin to obtain low-viscosity paraffin liquid with the thickness of 4 mm.
Step 2, preparing a polypropylene cyano carbon fiber graphite felt/epoxy resin prepreg by using the polypropylene cyano carbon fiber graphite felt;
step 2.1, completely dipping the polypropylene cyano carbon fiber graphite felt into the glass containing the epoxy resin glue solution obtained in the step 1 for 4 minutes, wherein the specification of the polypropylene cyano carbon fiber graphite felt is as follows: the dimensions of length × width × thickness are 10cm × 10cm × 0.5 cm;
and 2.2, after the impregnation is finished, taking out the prepreg and placing the prepreg on silicone oil paper, and then attaching a layer of silicone oil paper on the surface of the prepreg to obtain the polypropylene cyano carbon fiber graphite felt/epoxy resin prepreg.
Step 3, preparing two same polypropylene cyano carbon fiber graphite felt/paraffin prepreg by using two same polypropylene cyano carbon fiber graphite felts;
step 3.1, flatly placing two pieces of polypropylene cyano carbon fiber graphite felt which are made of the same material in the step 2 into a glass tank filled with paraffin liquid in the step 2, and soaking for 3 minutes, wherein the polypropylene cyano carbon fiber graphite felt is in the specification: the dimensions of length × width × thickness are 10cm × 10cm × 1 cm;
and 3.2, after the impregnation is finished, taking out the obtained product and placing the obtained product on silicone oil paper, adhering a layer of silicone oil paper on the surface of the obtained product, and sealing holes by paraffin curing at room temperature to obtain two same pieces of polypropylene cyano carbon fiber graphite felt/paraffin prepreg, wherein the thickness of the paraffin sealed holes is 4.5 mm.
Step 4, pressing an electrode plate with two sides containing paraffin by using a polypropylene cyano carbon fiber graphite felt/epoxy resin prepreg and two same polypropylene cyano carbon fiber graphite felt/paraffin prepreg;
step 4.1, after silicone oil paper on the surfaces of the three prepregs obtained in the steps 2 and 3 is removed, sequentially putting the three prepregs into a hot-pressing die, and placing the three prepregs in the middle to be in contact stacking with the upper and lower polypropylene cyano carbon fiber graphite felt/paraffin prepreg on the side without sealing holes with paraffin;
step 4.2, closing the grinding tool, then heating to 80 ℃ at the speed of 2 ℃/min, keeping the temperature for 160 minutes, and gelling at 140kgf/cm2Hot-press forming;
and 4.3, after forming, heating to 130 ℃ at the speed of 2.5 ℃/min, preserving the heat for 80 minutes, finally cooling to room temperature along with a furnace, releasing the pressure and taking out to obtain the electrode plate with paraffin on two sides.
Step 5, the electrode plate with double surfaces containing paraffin wax obtained in the step 4 is subjected to paraffin removal treatment to prepare a carbon fiber bipolar plate with double surfaces in a porous structure;
step 5.1, placing the electrode plate with double sides containing paraffin wax obtained in the step 4 into silicone oil at 140 ℃ to remove the paraffin wax, then placing the electrode plate into NaOH aqueous solution with the mass percentage of 40%, and soaking the electrode plate for 2.5 hours at 80 ℃;
step 5.2, taking out the mixture after soaking, and transferring the mixture into a boiling oxalic acid solution with the mass percentage of 15% for soaking for 2.5 hours;
and 5.3, finishing soaking, and finally, sequentially carrying out ultrasonic cleaning in acetone and deionized water for 8.5 minutes to obtain the bipolar plate with the porous structure on both sides.
The performance of the prepared polypropylene cyano carbon fiber graphite felt/epoxy resin compact layer in the middle of the bipolar plate is tested, and the conductivity of the conductive plate is 2.1 multiplied by 102S/cm; the bending strength is 66 MPa; the corrosion rate is 0.17 muA/cm2。
Example 4
Step 1, preparing an epoxy resin solution and paraffin liquid;
step 1.1, taking epoxy resin as a matrix, and enabling the weight percentage to meet the following requirements: a crosslinking agent: sequentially weighing the epoxy resin, the cross-linking agent and the catalyst, adding the epoxy resin, the cross-linking agent and the catalyst into a beaker, and magnetically stirring the mixture for 17 minutes at the temperature of 66 ℃ to fully mix the epoxy resin, the cross-linking agent and the catalyst to obtain a light yellow epoxy resin glue solution;
step 1.2, weighing edible paraffin, pouring the edible paraffin into a glass groove, adding the edible paraffin into an oil bath kettle to 127 ℃ to completely liquefy the edible paraffin to obtain low-viscosity paraffin liquid with the thickness of 4 mm;
step 2, preparing a polypropylene cyano carbon fiber graphite felt/epoxy resin prepreg by using the polypropylene cyano carbon fiber graphite felt;
step 2.1, completely dipping the polypropylene cyano carbon fiber graphite felt into the glass containing the epoxy resin glue solution obtained in the step 1 for 2 minutes, wherein the specification of the polypropylene cyano carbon fiber graphite felt is as follows: the dimensions of length × width × thickness are 10cm × 10cm × 0.5 cm;
and 2.2, after the impregnation is finished, taking out the prepreg and placing the prepreg on silicone oil paper, and then attaching a layer of silicone oil paper on the surface of the prepreg to obtain the polypropylene cyano carbon fiber graphite felt/epoxy resin prepreg.
Step 3, preparing two same polypropylene cyano carbon fiber graphite felt/paraffin prepreg by using two same polypropylene cyano carbon fiber graphite felts;
step 3.1, flatly placing two pieces of polypropylene cyano carbon fiber graphite felt which are made of the same material in the step 2 into a glass tank filled with paraffin liquid in the step 2, and soaking for 2 minutes, wherein the polypropylene cyano carbon fiber graphite felt is in the specification: the dimensions of length × width × thickness are 10cm × 10cm × 1 cm;
and 3.2, after the impregnation is finished, taking out the obtained product and placing the obtained product on silicone oil paper, adhering a layer of silicone oil paper on the surface of the obtained product, and sealing holes by paraffin curing at room temperature to obtain two same pieces of polypropylene cyano carbon fiber graphite felt/paraffin prepreg, wherein the thickness of the paraffin sealed holes is 4.5 mm.
Step 4, pressing an electrode plate with two sides containing paraffin by using a polypropylene cyano carbon fiber graphite felt/epoxy resin prepreg and two same polypropylene cyano carbon fiber graphite felt/paraffin prepreg;
step 4.1, after silicone oil paper on the surfaces of the three prepregs obtained in the steps 2 and 3 is removed, sequentially putting the three prepregs into a hot-pressing die, and placing the three prepregs in the middle to be in contact stacking with the upper and lower polypropylene cyano carbon fiber graphite felt/paraffin prepreg on the side without sealing holes with paraffin;
step 4.2, closing the grinding tool, heating to 80 ℃ at the speed of 2.5 ℃/min, keeping the temperature for 150 minutes, and gelling at 130kgf/cm2Hot-press forming;
and 4.3, after forming, heating to 130 ℃ at the speed of 3 ℃/min, preserving the heat for 75 minutes, finally cooling to room temperature along with a furnace, releasing the pressure and taking out to obtain the electrode plate with paraffin on two sides.
Step 5, the electrode plate with double surfaces containing paraffin wax obtained in the step 4 is subjected to paraffin removal treatment to prepare a carbon fiber bipolar plate with double surfaces in a porous structure;
step 5.1, placing the electrode plate with double sides containing paraffin wax obtained in the step 4 into silicone oil at 150 ℃ to remove the paraffin wax, then placing the electrode plate into NaOH aqueous solution with the mass percentage of 40%, and soaking the electrode plate for 2.5 hours at 80 ℃;
step 5.2, taking out the mixture after soaking, and transferring the mixture into a boiling oxalic acid solution with the mass percentage of 15% for soaking for 2.5 hours;
and 5.3, finishing soaking, and finally, sequentially carrying out ultrasonic cleaning in acetone and deionized water for 8.5 minutes to obtain the bipolar plate with the porous structure on both sides.
The performance of the prepared polypropylene cyano carbon fiber graphite felt/epoxy resin compact layer in the middle of the bipolar plate is tested, and the conductivity of the conductive plate is 1.6 multiplied by 102S/cm; the bending strength is 64 MPa; the corrosion rate is 0.11 muA/cm2。
Example 5
Step 1, preparing an epoxy resin solution and paraffin liquid;
step 1.1, taking epoxy resin as a matrix, and enabling the weight percentage to meet the following requirements: a crosslinking agent: sequentially weighing the epoxy resin, the cross-linking agent and the catalyst, adding the epoxy resin, the cross-linking agent and the catalyst into a beaker, and magnetically stirring the mixture for 30 minutes at the temperature of 70 ℃ to fully mix the epoxy resin, the cross-linking agent and the catalyst to obtain a light yellow epoxy resin glue solution;
step 1.2, weighing edible paraffin, pouring the edible paraffin into a glass groove, adding the edible paraffin into the glass groove by using an oil bath pan to 130 ℃, and completely liquefying the edible paraffin to obtain low-viscosity paraffin liquid with the thickness of 4 mm;
step 2, preparing a polypropylene cyano carbon fiber graphite felt/epoxy resin prepreg by using the polypropylene cyano carbon fiber graphite felt;
step 2.1, completely dipping the polypropylene cyano carbon fiber graphite felt into the glass containing the epoxy resin glue solution obtained in the step 1 for 5 minutes, wherein the specification of the polypropylene cyano carbon fiber graphite felt is as follows: the dimensions of length × width × thickness are 10cm × 10cm × 0.5 cm;
and 2.2, after the impregnation is finished, taking out the prepreg and placing the prepreg on silicone oil paper, and then attaching a layer of silicone oil paper on the surface of the prepreg to obtain the polypropylene cyano carbon fiber graphite felt/epoxy resin prepreg.
Step 3, preparing two same polypropylene cyano carbon fiber graphite felt/paraffin prepreg by using two same polypropylene cyano carbon fiber graphite felts;
step 3.1, flatly placing two pieces of polypropylene cyano carbon fiber graphite felt which are made of the same material in the step 2 into a glass tank filled with paraffin liquid in the step 2, and soaking for 5 minutes, wherein the polypropylene cyano carbon fiber graphite felt is in the specification: the dimensions of length × width × thickness are 10cm × 10cm × 1 cm;
and 3.2, after the impregnation is finished, taking out the obtained product and placing the obtained product on silicone oil paper, adhering a layer of silicone oil paper on the surface of the obtained product, and sealing holes by paraffin curing at room temperature to obtain two same pieces of polypropylene cyano carbon fiber graphite felt/paraffin prepreg, wherein the thickness of the paraffin sealed holes is 4.5 mm.
Step 4, pressing an electrode plate with two sides containing paraffin by using a polypropylene cyano carbon fiber graphite felt/epoxy resin prepreg and two same polypropylene cyano carbon fiber graphite felt/paraffin prepreg;
step 4.1, after silicone oil paper on the surfaces of the three prepregs obtained in the steps 2 and 3 is removed, sequentially putting the three prepregs into a hot-pressing die, and placing the three prepregs in the middle to be in contact stacking with the upper and lower polypropylene cyano carbon fiber graphite felt/paraffin prepreg on the side without sealing holes with paraffin;
step 4.2, closing the grinding tool, heating to 80 ℃ at the speed of 2.5 ℃/min, keeping the temperature for 180 minutes, and gelling at 150kgf/cm2Hot-press forming;
and 4.3, after forming, heating to 130 ℃ at the speed of 3 ℃/min, preserving the heat for 90 minutes, finally cooling to room temperature along with a furnace, releasing the pressure and taking out to obtain the electrode plate with paraffin on two sides.
Step 5, the electrode plate with double surfaces containing paraffin wax obtained in the step 4 is subjected to paraffin removal treatment to prepare a carbon fiber bipolar plate with double surfaces in a porous structure;
step 5.1, placing the electrode plate with double sides containing paraffin wax obtained in the step 4 into silicone oil at 150 ℃ to remove the paraffin wax, then placing the electrode plate into NaOH aqueous solution with the mass percentage of 40%, and soaking the electrode plate for 3 hours at 80 ℃;
step 5.2, taking out the mixture after soaking, and moving the mixture into a boiling oxalic acid solution with the mass percentage of 15% for soaking for 3 hours;
and 5.3, finishing soaking, and finally, sequentially carrying out ultrasonic cleaning in acetone and deionized water for 10 minutes to prepare the bipolar plate with the porous structure on both sides.
For the middle polypropylene cyano carbon fiber graphite felt/ring of the prepared bipolar plateThe oxygen resin compact layer is subjected to performance test, and the conductivity of the conductive plate is 2.4 multiplied by 102S/cm; the bending strength is 61 MPa; the corrosion rate is 0.3 mu A/cm2。
| Conductivity (S/cm) | Flexural Strength (MPa) | Corrosion Rate (. mu.A/cm 2) | |
| Example 1 | 2.3×102 | 64 | 0.2 |
| Example 2 | 1.9×102 | 63 | 0.44 |
| Example 3 | 2.1×102 | 66 | 0.17 |
| Example 4 | 1.6×102 | 64 | 0.11 |
| Example 5 | 2.4×102 | 61 | 0.3 |
TABLE 1
As can be seen from table 1: the electric conductivity, the bending strength and the corrosion rate of the polypropylene cyano carbon fiber graphite felt/epoxy resin compact layer conductive plate of the embodiments 1 to 5 reach and are superior to the performance standard of the American energy department bipolar plate, namely, the electric conductivity is more than 100S/cm, the bending strength is more than 59MPa, and the corrosion rate is less than 1 muA/cm2。
Claims (8)
1. A preparation method of a carbon fiber bipolar plate with a three-dimensional porous structure is characterized by comprising the following steps:
step 1, liquefying paraffin by using 110-grade 130 ℃ silicone oil to obtain paraffin liquid, wherein the paraffin is No. 90 microcrystalline wax; meanwhile, preparing epoxy resin glue solution;
step 2, preparing a polypropylene cyano carbon fiber graphite felt/epoxy resin prepreg by using the polypropylene cyano carbon fiber graphite felt;
step 3, preparing two same polypropylene cyano carbon fiber graphite felt/paraffin prepreg by using two same polypropylene cyano carbon fiber graphite felts;
step 4, pressing an electrode plate with two sides containing paraffin by using a polypropylene cyano carbon fiber graphite felt/epoxy resin prepreg and two same polypropylene cyano carbon fiber graphite felt/paraffin prepreg;
and 5, performing dewaxing treatment on the electrode plate with paraffin on two surfaces obtained in the step 4 to obtain the carbon fiber bipolar plate with a porous structure on two surfaces.
2. The method for preparing a carbon fiber bipolar plate with a three-dimensional porous structure according to claim 1, wherein the method for preparing the epoxy resin glue solution in the step 1 comprises the following steps:
mixing epoxy resin, cross-linking agent and catalyst, and magnetically stirring at 50-70 deg.c for 10-30 min to obtain the epoxy resin glue solution.
3. The method for preparing a carbon fiber bipolar plate with a three-dimensional porous structure as claimed in claim 1, wherein the step 2 is specifically performed according to the following steps:
step 2.1, completely soaking the polypropylene cyano carbon fiber graphite felt in the epoxy resin glue solution obtained in the step 1 for 1-5 minutes;
and 2.2, after the impregnation is finished, taking out the prepreg and placing the prepreg on silicone oil paper, and then adhering a layer of silicone oil paper on the surface of the prepreg to obtain the polypropylene cyano carbon fiber graphite/epoxy resin prepreg.
4. The method for preparing a carbon fiber bipolar plate with a three-dimensional porous structure as claimed in claim 3, wherein the step 3 is specifically performed according to the following steps:
step 3.1, flatly putting two same polypropylene cyano carbon fiber graphite felts into paraffin liquid, and soaking for 1-5 minutes;
and 3.2, after the impregnation is finished, taking out the prepreg and placing the prepreg on silicone oil paper, adhering a layer of silicone oil paper on the surface of the prepreg, and curing and sealing holes by paraffin at room temperature to obtain two same pieces of polypropylene cyano carbon fiber graphite felt/paraffin prepreg.
5. The method for preparing a carbon fiber bipolar plate with a three-dimensional porous structure as claimed in claim 4, wherein the step 4 is specifically performed according to the following steps:
step 4.1, after silicone oil paper on the surfaces of the three prepregs obtained in the steps 2 and 3 is removed, sequentially putting the three prepregs into a hot-pressing die, and placing the three prepregs in the middle to be in contact stacking with the upper and lower polypropylene cyano carbon fiber graphite felt/paraffin prepreg on the side without sealing holes with paraffin;
step 4.2, closing the grinding tool, then heating to 80 ℃ at the speed of 1-3 ℃/min, preserving the temperature for 180 minutes, and then gelling at the temperature of 100 ℃ and 150kgf/cm2Hot-press forming;
and 4.3, after forming, heating to 130 ℃ at the speed of 1-3 ℃/min, preserving the heat for 60-90 minutes, finally cooling to room temperature, releasing the pressure and taking out to obtain the electrode plate with paraffin on two sides.
6. The method for preparing a carbon fiber bipolar plate with a three-dimensional porous structure as claimed in claim 1, wherein the step 5 is specifically performed according to the following steps:
step 5.1, placing the electrode plate with paraffin on both sides obtained in the step 4 into 120-150 ℃ silicone oil to remove the paraffin, then placing the electrode plate into 40 mass percent NaOH aqueous solution, and soaking the electrode plate for 2-3 hours at 80-90 ℃;
step 5.2, taking out the mixture after soaking, and soaking the mixture in a boiling oxalic acid solution with the mass percentage of 15% for 2-3 hours;
and 5.3, finishing soaking, and finally, sequentially carrying out ultrasonic cleaning in acetone and deionized water for 8-10 minutes to obtain the carbon fiber bipolar plate with the porous structure on both sides.
7. The method for preparing a carbon fiber bipolar plate with a three-dimensional porous structure as claimed in claim 2, wherein the epoxy resin glue solution is prepared in step 1, and the weight percentages of the components are epoxy resin: a crosslinking agent: the catalyst is 100: 80-90: 0.1-0.3.
8. The method as claimed in claim 7, wherein the epoxy resin in step 1 is bisphenol A type with a molecular weight of 300-700; the catalyst is benzyldimethylamine.
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