CN116024825A - Preparation method of novel microporous membrane for alkaline electrolyzed water, obtained product and application - Google Patents
Preparation method of novel microporous membrane for alkaline electrolyzed water, obtained product and application Download PDFInfo
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- CN116024825A CN116024825A CN202310028160.6A CN202310028160A CN116024825A CN 116024825 A CN116024825 A CN 116024825A CN 202310028160 A CN202310028160 A CN 202310028160A CN 116024825 A CN116024825 A CN 116024825A
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Abstract
The invention provides a preparation method of a novel microporous diaphragm for alkaline electrolyzed water, which uses polyvinylpyrrolidone, polyethylene glycol, N dimethylformamide, polysulfone and ZrO 2 、Y 2 O 3 And CeO 2 And (3) preparing film-making liquid, spraying the film-making liquid on the melt-blown cloth on two sides, and solidifying to obtain the novel microporous diaphragm. The diaphragm is applied to alkaline water electrolysis hydrogen production equipment. The diaphragm is modified by selecting proper inorganic materials, so that the diaphragm which meets the use conditions of the diaphragm of the alkaline water electrolysis cell and has simple and reliable preparation process is obtained. The inventive separatorThe membrane can resist alkali and high temperature, has good hydrophilic performance and mechanical performance, and has good air tightness, high ion conduction efficiency and stable chemical performance. When the electrolyte is applied to an alkaline water electrolysis system, the electric energy consumption per unit hydrogen is only 4.0 kW.h/m at the temperature of the electrolyte of 100 DEG C 3 The purity of the hydrogen can reach 99.98 percent, and other diaphragms in the prior art are more energy-saving and environment-friendly.
Description
[ field of technology ]
The invention relates to the technical field of hydrogen production by alkaline water electrolysis, in particular to a preparation method of a novel microporous membrane for an alkaline water electrolysis hydrogen production system.
[ background Art ]
The water electrolysis hydrogen production has the advantages of mature technology, high product purity, environmental protection and the like, and is an important technical means for producing hydrogen in a modern large scale. The alkaline water electrolyzer is a main device for producing hydrogen by water electrolysis, an anode and a cathode are respectively arranged in the electrolyzer by dividing the electrolyzer into a Yang Jixiao chamber and a cathode chamber through a diaphragm, 30% -40% KOH or NaOH solution is used as electrolyte in the electrolyzer, oxygen is obtained at the anode, hydrogen is obtained at the cathode, and the diaphragm arranged between the Yang Jixiao chamber and the cathode chamber is used for preventing the hydrogen and the oxygen from being mixed.
In this technique, the resistance of the membrane can affect the voltage of the electrolysis process, thus limiting the hydrogen production cost of the system. A membrane suitable for use in an alkaline water cell should possess the following properties: (1) Good air tightness is ensured, and hydrogen and oxygen molecules can not penetrate through the diaphragm; (2) good alkali resistance and corrosion resistance; (3) The mechanical strength is good, and the impact of electrolyte and generated gas can be born for a long time; (4) The porosity is higher, so that smaller surface resistance is obtained, and the energy consumption of the electrolytic cell is reduced; (5) Smaller average pore size to prevent permeation of bubbles and inhibit diffusion; (6) stable chemical properties; (7) The raw materials are easy to obtain, nontoxic and pollution-free, and the waste is easy to treat; (8) The physical and chemical properties of the raw materials are suitable for the requirements and conditions of the film-making process, and industrial production can be realized.
Commonly used separators may be classified into asbestos separators, inorganic separators, organic separators, and inorganic-organic composite separators. Asbestos diaphragm has larger impedance, unstable chemical property and cancerogenic risk, and is not an ideal diaphragm material; the inorganic or organic composite membrane is not suitable for the severe conditions of alkaline water electrolysis, so that the inorganic-organic composite membrane becomes the research direction of alkaline water electrolysis membranes.
Chinese patent application CN113862821a discloses a polyphenylene sulfide fiber fabric type alkaline water electrolysis diaphragm, wherein the polyphenylene sulfide resin is modified by zirconia inorganic nano particles, zirconia modified polyphenylene sulfide fibers are obtained through melt spinning, and after spinning and weaving the fibers into cloth, the polyphenylene sulfide fiber fabric type alkaline water electrolysis diaphragm can be obtained through a water needling process. However, only the porosity, pore contact angle and elongation loss at break of the separator are described in this patent application, and the separator resistance properties are not analyzed.
Chinese patent application CN 114432906a discloses a high temperature resistant alkaline water electrolysis cell composite membrane, the support is a polyphenylene sulfide mesh, the composite membrane is a polysulfone-zirconia composite membrane, and contains metal salt or composite metal salt. Wherein the metal salt comprises magnesium oxide, aluminum oxide, zinc oxide, silicon dioxide, borax, lithium oxide, calcium oxide, magnesium sulfate, magnesium carbonate, aluminum carbonate, sodium carbonate, calcium phosphate and/or kaolin and composite salts thereof. However, for its performance, this application discloses only a current density of 6400A/m at 80℃for the diaphragm 2 Alkali loss amount<1, the tensile strength and elongation at break thereof are disclosed, but the separator resistance properties cannot be analyzed due to the insufficient conditions disclosed.
Chinese patent application CN 114432905a discloses a non-asbestos alkaline electrolytic water composite membrane, which is a polysulfone/zirconia composite membrane, comprising polysulfone polymer, high molecular reinforcing agent, pore-forming agent and hydrophilic modifier; the pore-forming agent is polyvinylpyrrolidone; the hydrophilic modifier is zirconium dioxide; the polymer reinforcing agent is natural rubber, styrene-butadiene rubber, hydrogenated nitrile-butadiene rubber, SEBS rubber, chloroprene rubber or fluororubber. Nor was the resistive properties of the diaphragm analyzed in this application.
[ invention ]
The invention aims to overcome the defects of the prior art, provides a diaphragm with better resistance performance, which is applied to an alkaline electrolytic water system, ensures that the obtained diaphragm can resist alkali and high temperature, has good hydrophilic performance and mechanical performance, and simultaneously has good air tightness, high ion conduction efficiency and stable chemical performance, and the preparation process is expected to be environment-friendly, the preparation method is simple and feasible, and the use condition of the diaphragm of the alkaline electrolytic water tank is met.
Based on the above, the invention provides a preparation method of a novel microporous membrane for alkaline electrolyzed water, which comprises the following steps:
(1) Preparation of materials
Weighing 10-15 parts by weight of polyvinylpyrrolidone, 5-10 parts by weight of polyethylene glycol, 40-50 parts by weight of N, N-dimethylformamide, 10-25 parts by weight of polysulfone and ZrO with particle size of 100-300nm 2 5-15 parts, particle size 100-300nm Y 2 O 3 1-5 parts and CeO with particle size of 100-300nm 2 1-5 parts of polyvinylpyrrolidone, polyethylene glycol, N-dimethylformamide and polysulfone are mixed at 50-80 ℃ and stirred until the mixture is uniform, and then ZrO is added at 50-80 ℃ respectively 2 、Y 2 O 3 And CeO 2 Stirring until the mixture is uniform, and carrying out negative pressure degassing to obtain a film-making liquid;
(2) Film forming
Spraying the film-making liquid on the two sides of the melt-blown cloth through coating equipment, then placing the film-making liquid into a coagulating bath at 60-70 ℃ for coagulation, and then collecting to obtain the novel microporous diaphragm.
According to a preferred embodiment, the meltblown is a Polyetheretherketone (PEEK) meltblown.
Meltblown webs are a type of meltblown nonwoven web formed by drawing a stream of polymer melt extruded through a die orifice with a high velocity stream of hot air to form ultrafine fibers and collecting the ultrafine fibers on a web curtain or drum to adhere to itself. In the selection of raw materials, in order to meet the use conditions of the alkaline water electrolysis cell diaphragm, the melt-blown cloth must be capable of adapting to alkaline environment and high temperature conditions, so that the melt-blown cloth must have good alkali resistance, corrosion resistance, good mechanical strength and stable physicochemical properties. Polyether ether ketone (PEEK) is a high-molecular material with high temperature resistance and chemical corrosion resistance, and meanwhile, the PEEK is excellent in mechanical property and stable in physical and chemical properties, and is very suitable for being used as a supporting layer. And other common melt-blown materials such as polypropylene are unsuitable for use as a substrate for alkaline water electrolyser diaphragms because of their poor weatherability, high water absorption and susceptibility to moisture, which would otherwise affect the service life of the product.
As a preferred embodiment, the meltblown webs used in the present invention have a weight per unit area of from 20 to 40g/m 2 。
In the present invention, it is desirable to improve the performance of the membrane by adding some materials to the membrane-making liquid. On the one hand, it is desirable that the added materials act to reduce the resistance of the film, and on the other hand, it is desirable that these materials increase the hydrophilicity of the product. The inventors examined ZrO 2 、Y 2 O 3 And CeO 2 They can be used as ion conducting materials of the electrolytic alkaline hydrogen production diaphragm, and have the function of reducing resistance; in addition, all three inorganic materials have hydrophilicity, so that the hydrophilicity of PSF can be improved. However, if one of the materials is used alone, e.g. ZrO 2 The thermal expansion coefficient is high, the thermal shock resistance is poor, and when the thermal expansion coefficient is used alone, the volume effect can be caused by phase change in the heating or cooling process. In order to overcome the defect, the invention is matched with Y 2 O 3 And CeO 2 The nano particles can relieve thermal stress at high temperature to a great extent and stabilize ZrO 2 Cracking problems of the article. Thus, zrO is finally selected 2 /Y 2 O 3 /CeO 2 The inorganic particles are added as composite inorganic particles to the film forming liquid.
In the invention, the polyethylene glycol in the film-forming liquid is PEG8000 which is used as a macromolecular additive, so that the product is easier to generate a pore structure in the phase inversion process, thereby improving the porosity, being beneficial to reducing the resistance and improving the conduction rate.
In the present invention, the coagulation bath used in step (2) is a water bath. Those skilled in the art can also select an appropriate coagulation bath as an alternative in light of the teachings of the prior art.
According to a preferred embodiment, the coating apparatus of step (2) is a slot coating apparatus.
In the present invention, the slot coating apparatus refers to an apparatus for performing slot-die coating, which can precisely coat a feed liquid onto a substrate surface through a slot die (slot head), such as an HPSDC slot coater sold by hanpan technology limited, hangzhou.
The spraying speed adopted by the invention is 8-12m/min by a melt-spraying cloth moving speed meter, the spraying amount of the film-making liquid is 10-15g/min, and the width of the melt-spraying cloth is 30-50cm.
Preferably, the thickness of the novel microporous separator membrane of the present invention is 0.20 to 0.30mm.
The invention also provides application of the novel microporous membrane obtained by the preparation method in alkaline water electrolysis hydrogen production equipment
The diaphragm is modified by selecting proper inorganic materials, so that the diaphragm which meets the use conditions of the diaphragm of the alkaline water electrolysis cell and is simple, reliable and environment-friendly in preparation process is obtained. The polysulfone is used as a common membrane material, has excellent mechanical property, keeps excellent mechanical property at high temperature, has high thermal stability, is hydrolysis-resistant, nontoxic and acid and alkali corrosion-resistant, and is the best choice for the alkaline water electrolysis hydrogen production membrane; zrO (ZrO) 2 /Y 2 O 3 /CeO 2 The use of the composite inorganic particles can improve the hydrophilicity of polysulfone, and simultaneously, electrolyte can flow in the diaphragm more easily, so that the composite inorganic particles have the effects of improving the air tightness of the diaphragm and reducing the resistance; the polyether-ether-ketone has high performance of high temperature resistance and chemical corrosion resistance and excellent mechanical property, so that the polyether-ether-ketone melt-blown cloth is very suitable for being used as a supporting layer.
The alkaline electrolytic water system diaphragm prepared by the invention can resist alkali and high temperature, has good hydrophilic performance and mechanical performance, and has good air tightness, high ion conduction efficiency and stable chemical performance. When the diaphragm is applied to an alkaline water electrolysis system, the electric energy consumption per unit hydrogen is only 4.0kW DEG at the temperature of the electrolyte of 100 DEG Ch/m 3 The purity of the hydrogen can reach 99.98 percent, and other diaphragms in the prior art are more energy-saving and environment-friendly.
[ description of the drawings ]
FIG. 1 is an electron micrograph of a microporous separator membrane of example 1;
FIG. 2 is an electron micrograph of the microporous membrane of example 2;
FIG. 3 is a graph of membrane resistance versus temperature for the microporous membrane of example 1 in 30% KOH aqueous solution;
FIG. 4 is a graph of membrane resistance versus temperature for the microporous membrane of example 2 in 30% KOH aqueous solution;
FIG. 5 is a schematic diagram of the structure of an alkaline water electrolysis cell of example 4.
[ detailed description ] of the invention
The following examples serve to illustrate the technical solution of the invention without limiting it.
In the present invention, unless otherwise specified,% for specifying concentration is weight percent, "parts" for specifying amount is weight part ": "is the weight ratio.
Example 1 preparation of novel microporous separator membranes
Weighing 10 parts by weight of polysulfone, 10 parts by weight of polyvinylpyrrolidone and 5 parts by weight of polyethylene glycol in 50 parts by weight of N, N dimethylformamide, mechanically stirring for 4 hours at 50 ℃ until the polysulfone, the polyvinylpyrrolidone and the polyethylene glycol are completely dissolved and uniformly mixed.
Adding ZrO one by one at 50deg.C 2 (particle size 100-300 nm) 15 parts, Y 2 O 3 (particle diameter 100-300 nm) 5 parts and CeO 2 (particle size 100-300 nm) for 5 parts, stirring continuously for 1h until the mixture is uniform, and then degassing for 1h under negative pressure to obtain film-forming liquid.
Pouring the film-making liquid into a trough of a slit coater, and spraying on the two sides of the polyether-ether-ketone melt-blown cloth through a slot-die quantitative coating process. The spraying parameters are 10g/min, the moving speed is 10m/min, and the breadth is 30cm.
Then, the sample was put into a coagulation bath in a water bath at 60℃and subjected to mass exchange with the aqueous phase, and collected by a roller, to obtain a membrane sample 1.
Example 2 preparation of novel microporous separator membranes
A separator sample 2 was prepared in the same manner as in example 1 except that the raw materials for the film-forming liquid were polysulfone 25 parts, polyvinylpyrrolidone 15 parts, polyethylene glycol 10 parts, N dimethylformamide 40 parts, zrO 2 5 parts, Y 2 O 3 3 parts of CeO 2 2 parts, wherein the temperature used in the preparation process is 80 ℃, the spraying parameter is 15g/min, the moving speed is 10m/min, the breadth is 50cm, and the water bath coagulation bath temperature is 70 ℃, so that the diaphragm sample 2 is obtained.
Example 3 diaphragm Performance test
The membrane samples 1 and 2 were each observed under an electron microscope as shown in fig. 1-2.
From fig. 1 and 2, it can be seen that the membrane surface has a uniform distribution of small holes, which provide channels for gas exchange; meanwhile, inorganic particles can be seen to be attached to the surface of the diaphragm, so that the hydrophilicity and conductivity of the diaphragm are increased, and the hydrogen production energy consumption is reduced; the PEEK melt-blown cloth is taken as a supporting layer, the PEEK melt-blown cloth is wrapped by high polymer resin, and the resin section presents a finger-shaped hole structure, so that an effective channel is provided for gas exchange.
The thickness, pore size, porosity, weight density, surface contact angle, tensile strength, alkali absorption, alkali vector, electrical resistance, and dimensional stability of the separator samples 1 and 2 were measured, respectively. The measurement method is as follows:
(1) Thickness: the thickness of the diaphragm is measured by referring to the national electronic industry standard SJ-T10171.1-1991 method for testing diaphragm thickness of alkaline storage battery diaphragm, and the average value measured by 3 pieces of samples is taken as a measurement result.
(2) Pore diameter: 30 wells were randomly measured on a membrane electron micrograph and the average was taken as the membrane pore size.
(3) Porosity measurement: the porosity of the diaphragm is the percentage of the pore volume of the diaphragm to the volume of the diaphragm, the pore volume V hole of the diaphragm is determined according to the change of the weight of the diaphragm before and after soaking purified water, the skeleton volume of the material can obtain V bone through the density and the dry weight of raw materials, and the porosity of the porous material can be calculated by adopting the following formula:
the average value of the measurement of 3 specimens was taken as the measurement result.
(4) Weight density: the diaphragm weight density refers to the weight of a sample of unit size by cutting the diaphragm sample to 1cm 3 The measurement was performed by a weighing method, and an average value of the measurement of 3 samples was taken as a measurement result.
(5) Surface contact angle: the contact angle of pure water on the surface of the diaphragm was measured by using a DSA100 video optical contact angle measuring instrument, and the average value of measurements of 3 specimens was taken as a measurement result.
(6) Tensile strength: the tensile strength of the diaphragm refers to the tensile force per unit sectional area of the diaphragm, expressed in N/mm 2 The tensile strength of the membrane was measured by using an XLD type electronic tensile tester with reference to the national electronic industry Standard SJ-T10171.4-91, and the average value of the measurement of 3 samples was taken as a measurement result.
(7) Alkali absorption rate: the alkali absorption rate may represent the relative change in mass of the diaphragm after immersion in KOH solution, expressed as a percentage of the increase in mass to the mass of the original sample. The method is carried out by referring to the national electronic industry standard SJ-T10171.7-91 'determination of diaphragm alkali absorption rate', and an average value of 3 sample measurements is taken as a measurement result.
(8) Alkali vector: the diaphragm alkali vector is a measure of the relative change in mass of the diaphragm after immersion in a potassium hydroxide solution at a certain temperature. The measurement is carried out by referring to the national electronic industry standard SJ/T10171.6-1991 'determination of alkali resistance loss of diaphragm of alkaline storage battery diaphragm Performance test method', and the average value of 3 sample measurements is taken as a test result.
(9) Resistance: the resistance of the diaphragm reflects the conductivity of the diaphragm immersed in the electrolyte, the electrochemical impedance under different temperature conditions is measured by an electrochemical workstation, and the average value of the measurement of 3 samples is taken as a test result.
(10) Dimensional stability: the dimensional stability of the diaphragm is that a sample with unit size is placed in a water bath with the temperature of 100 ℃ for 15min, the shrinkage rate of the diaphragm size is calculated, and the average value measured by 3 samples is taken as a test result.
(11) Maximum operating temperature: the highest temperature which can be born by the equipment during operation is referred to, and exceeding the highest operating temperature can influence the stability of the physicochemical property of the diaphragm and the purity of the hydrogen.
(12) Air permeability: refers to the permeability of gas to high molecular materials such as films, coatings, fabrics and the like. And measuring the volume of gas permeating through the diaphragm per square centimeter in unit time by using a chemical sensor by adopting an isobaric method, and taking the average value of measurement of 3 samples as a test result.
The results obtained are shown in Table 1:
TABLE 1 basic Properties of separator
As shown in table 1 and fig. 3-4, each of the membrane samples 1 and 2 had a microporous structure, which had good tensile strength, alkali absorption rate and alkali vector, and the membrane resistance decreased with increasing temperature at 20-100 ℃ under the condition of 30% by mass concentration of KOH aqueous solution, and was substantially linear. Wherein the resistance of the diaphragm sample 1 at 100 ℃ can reach 0.05Ω & cm 2 While the resistance of the diaphragm sample 2 at 100 ℃ can reach 0.06 omega cm 2 The performance is excellent.
Example 4 use of the separator obtained in example 1
An alkaline water electrolysis cell as shown in fig. 5 was constructed. At a volume of 0.5m 3 The cell body of (2) is divided into 3 compartments by a diaphragm sample 1, anodes or cathodes are arranged in each compartment, and all the anodes and cathodes are staggered and connected in parallel. The anode and the cathode are all 500g/m 2 The foam nickel with surface density is electrolyzed under the conditions of 100-500A current and 1-3V voltage.
The electrolyte was a 30% aqueous KOH solution charged to each compartment. In the electrolysis process, oxygen generated by the anode and hydrogen generated by the cathode are respectively collected, and the hydrogen and the oxygen are separated by the diaphragm sample 1, so that mixing is avoided.
The energy consumption and hydrogen purity per unit volume of hydrogen were measured by varying the temperature of the electrolyte in the electrolytic cell, and the results are shown in table 2.
TABLE 2 consumption of electric energy and purity of Hydrogen under different temperature conditions
The results showed that the energy consumption decreased with an increase in temperature, which corresponds to the trend of decrease in the separator resistance with an increase in temperature measured in example 2. In addition, the hydrogen purity increases as the electrolyte temperature increases.
When the temperature of the electrolyte is 100 ℃, the electric energy consumption per unit hydrogen is 4.0kW.h/m 3 The purity of the hydrogen reaches 99.98 percent.
Example 5 application of the separator obtained in example 2
The test was performed in the same procedure as in example 4, except that the separator was replaced with the separator obtained in example 2.
The test results are shown in Table 3.
TABLE 3 consumption of electric energy and purity of Hydrogen under different temperature conditions
The results showed that the trend of energy consumption and the trend of hydrogen purity were the same as those of example 4, and that the energy consumption was decreased with an increase in temperature, while the hydrogen purity was increased with an increase in electrolyte temperature.
When the temperature of the electrolyte is 100 ℃, the electric energy consumption per unit hydrogen is 4.1 kW.h/m 3 The purity of the hydrogen reaches 99.99 percent.
Claims (8)
1. A method for preparing a novel microporous membrane for alkaline electrolyzed water, which comprises the following steps:
(1) Preparation of materials
Weighing 10-15 parts by weight of polyvinylpyrrolidone, 5-10 parts by weight of polyethylene glycol, 40-50 parts by weight of N, N-dimethylformamide, 10-25 parts by weight of polysulfone and ZrO with particle size of 100-300nm 2 5-15 parts, particle size 100-300nm Y 2 O 3 1-5 parts and CeO with particle size of 100-300nm 2 1-5 parts of polyvinylpyrrolidone, polyethylene glycol, N-dimethylformamide and polysulfone are mixed at 50-80 ℃ and stirred until the mixture is uniform, and then ZrO is added at 50-80 ℃ respectively 2 、Y 2 O 3 And CeO 2 Stirring until the mixture is uniform, and carrying out negative pressure degassing to obtain a film-making liquid;
(2) Film forming
Spraying the film-making liquid on the two sides of the melt-blown cloth through coating equipment, then placing the film-making liquid into a coagulating bath at 60-70 ℃ for coagulation, and then collecting to obtain the novel microporous diaphragm.
2. The process of claim 1 wherein the meltblown web is a polyetheretherketone meltblown web having a weight per unit area of 20-40g/m 2 。
3. The process according to claim 1, wherein the polydiethanol in step (1) is PEG8000.
4. The method of claim 1, wherein the coagulation bath of step (2) is a water bath.
5. The production method according to claim 1, wherein the coating apparatus of step (2) is a slot-die coating apparatus.
6. The method according to claim 1, wherein the spraying speed in the step (2) is 8-12m/min by a melt-blown cloth moving speed meter, the spraying amount of the film-forming liquid is 10-15g/min, and the width of the melt-blown cloth is 30-50cm.
7. The method of claim 1, wherein the novel microporous membrane has a thickness of 0.20 to 0.30mm.
8. Use of a novel microporous membrane obtained by the preparation method according to any one of claims 1 to 7 in an alkaline water electrolysis hydrogen production plant.
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| CN202310028160.6A CN116024825A (en) | 2023-01-09 | 2023-01-09 | Preparation method of novel microporous membrane for alkaline electrolyzed water, obtained product and application |
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| CN202310028160.6A CN116024825A (en) | 2023-01-09 | 2023-01-09 | Preparation method of novel microporous membrane for alkaline electrolyzed water, obtained product and application |
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