CN116083955B - High-temperature-resistant basalt modified diaphragm and preparation process thereof - Google Patents
High-temperature-resistant basalt modified diaphragm and preparation process thereof Download PDFInfo
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- CN116083955B CN116083955B CN202310378083.7A CN202310378083A CN116083955B CN 116083955 B CN116083955 B CN 116083955B CN 202310378083 A CN202310378083 A CN 202310378083A CN 116083955 B CN116083955 B CN 116083955B
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21F—PAPER-MAKING MACHINES; METHODS OF PRODUCING PAPER THEREON
- D21F11/00—Processes for making continuous lengths of paper, or of cardboard, or of wet web for fibre board production, on paper-making machines
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B13/00—Diaphragms; Spacing elements
- C25B13/04—Diaphragms; Spacing elements characterised by the material
- C25B13/05—Diaphragms; Spacing elements characterised by the material based on inorganic materials
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Chemical Kinetics & Catalysis (AREA)
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- Organic Chemistry (AREA)
- Paper (AREA)
- Diaphragms For Electromechanical Transducers (AREA)
Abstract
The invention provides aA high temperature resistant basalt modified diaphragm and a preparation process thereof relate to the field of diaphragm preparation and aim to solve the problem that the temperature resistance of the existing diaphragm can not meet the use requirement. The high-temperature-resistant basalt modified diaphragm comprises the following raw materials: basalt fiber, zirconia fiber, chopped carbon fiber, sepiolite fiber, and adhesive; the thickness of the high-temperature-resistant basalt modified diaphragm is 0.1-3 mm, and the surface resistance is 0.1-0.3 omega cm 2 (30 ℃) and the temperature resistance temperature range is 50-550 ℃ and the operation density is 2000-20000A/m 2 The bubble point pressure is more than 1bar, and the alkali absorption rate is 100% -500%. The invention modifies the diaphragm to make the diaphragm have the characteristics of small resistance, high temperature resistance, high operation density, good wettability and high mechanical strength. In addition, based on the same conception, the invention also provides a preparation process of the high-temperature-resistant basalt modified diaphragm.
Description
Technical Field
The invention relates to the technical field of diaphragm preparation, in particular to a high-temperature-resistant basalt modified diaphragm and a preparation process thereof.
Background
The separator serves to isolate the substance from the reaction of two adjacent substances. When conventional separators are used in electrochemical devices, heat dissipation of the separator or perforation of the separator by overheating may increase the risk of explosion. When the diaphragm is used in the electrolytic hydrogen production technology, the diaphragm has poor temperature resistance, and can be vitrified or aged after running for a period of time at the temperature of more than 100 ℃, so that the diaphragm can not play a role in isolating hydrogen and oxygen. It is known that the temperature resistance of the conventional separator cannot meet the use requirements.
Disclosure of Invention
The invention provides a high-temperature-resistant basalt modified diaphragm, which aims to solve the problem that the use requirement of the conventional diaphragm cannot be met by the temperature resistance of the diaphragm. Based on the same inventive concept, the invention also provides a preparation process of the high-temperature-resistant basalt modified diaphragm.
The technical scheme adopted by the invention is as follows:
the high temperature resistant basalt modified diaphragm comprises the following raw materials in percentage by weight:
20-60% of basalt fiber, 30-50% of zirconia fiber, 0-5% of chopped carbon fiber, 0-20% of sepiolite fiber and 0-10% of adhesive;
wherein, the basalt fiber is long-cut fiber or short-cut fiber;
the thickness of the modified diaphragm is 0.1-3 mm, and the surface resistance is 0.1-0.3 ohm cm 2 (30 ℃) and the temperature resistance temperature range is 50-550 ℃ and the operation density is 2000-20000A/m 2 The bubble point pressure is more than 1bar, and the alkali absorption rate is 100% -500%.
Optionally, the length of the zirconia fiber is 3-5 μm or 800 nm-1 μm.
Optionally, the length of the chopped carbon fiber is 3-5 mm.
Optionally, the adhesive is one of polyimide glue, polyvinylidene fluoride, phenolic resin glue, heat-resistant epoxy glue, hydroxybutyronitrile latex, polytetrafluoroethylene glue, epoxy resin glue, polyvinyl chloride glue or organic silica gel.
Optionally, when the basalt fiber is a chopped fiber, the length of the zirconia fiber is 800 nm-1 μm, and the adhesive is polyvinylidene fluoride.
Optionally, when the basalt fiber is a chopped fiber, the length of the zirconia fiber is 3-5 μm.
Optionally, when the basalt fiber is a chopped fiber, the length of the zirconia fiber is 3-5 μm, and the adhesive is hydroxybutyronitrile latex.
Optionally, when the basalt fiber is a long cut fiber, the length of the zirconia fiber is 800nm to 1 μm.
The high-temperature-resistant basalt modified diaphragm disclosed by the technical scheme has the advantages of small resistance, high temperature resistance, high operation density, good wettability and high mechanical strength, and can completely meet the performance requirements after being tested and used by the inventor.
Based on the modified diaphragm disclosed by the invention, the invention also discloses a process method for preparing the modified diaphragm, which specifically comprises the following steps:
s1, taking quantitative basalt fibers and desalted water, stirring and fluffing to enable the slurry concentration to be 1-5%;
s2, adding one or more of zirconia fiber, carbon fiber or sepiolite fiber, and uniformly stirring to obtain suspension;
s3, adding an adhesive into the suspension to obtain slurry;
s4, the slurry is made into a paper machine for suction filtration and dehydration, and the wet paper web is obtained after dehydration;
s5, drying the wet paper web to obtain the basalt modified diaphragm.
The drying temperature in the step S5 is 40-100 ℃, and the drying time is 12-24 hours.
Compared with the prior art, the invention has the beneficial effects that:
1. the basalt modified diaphragm has the advantages of small resistance, high temperature resistance, high operation density, high alkali absorption rate, good wettability and high mechanical strength.
2. The size and weight of a single tank can be reduced or the productivity of the industrial alkaline electrolytic tank can be improved, and the direct current power consumption can be reduced.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic structural diagram of a process flow of a preparation process of a high-temperature-resistant basalt modified diaphragm.
Detailed Description
Hereinafter, only certain exemplary embodiments are briefly described. As will be recognized by those of skill in the pertinent art, the described embodiments may be modified in various different ways without departing from the spirit or scope of the present invention. Accordingly, the drawings and description are to be regarded as illustrative in nature and not as restrictive.
The following disclosure provides many different embodiments, or examples, for implementing different features of the invention. In order to simplify the present disclosure, components and arrangements of specific examples are described below. They are, of course, merely examples and are not intended to limit the invention. Furthermore, the present invention may repeat reference numerals and/or letters in the various examples, which are for the purpose of brevity and clarity, and which do not themselves indicate the relationship between the various embodiments and/or arrangements discussed.
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
The embodiment of the invention provides a high-temperature-resistant basalt modified diaphragm, which comprises the following raw materials in percentage by weight:
20-60% of basalt fiber, 30-50% of zirconia fiber, 0-5% of chopped carbon fiber, 0-20% of sepiolite fiber and 0-10% of adhesive;
wherein, the basalt fiber is long-cut fiber or short-cut fiber; the length of the zirconia fiber is 3-5 μm or 800 nm-1 μm; the length of the chopped carbon fiber is 3-5 mm; the adhesive is one of polyimide glue, polyvinylidene fluoride, phenolic resin glue, heat-resistant epoxy glue, hydroxybutyronitrile emulsion, polytetrafluoroethylene glue, epoxy resin glue, polyvinyl chloride glue or organic silica gel.
The application also provides a preparation process of the film, as shown in fig. 1, comprising the following steps:
s1, taking quantitative basalt fibers and desalted water, stirring and fluffing to enable the slurry concentration to be 1-5%;
s2, adding one or more of zirconia fiber, carbon fiber or sepiolite fiber, and uniformly stirring to obtain suspension;
s3, adding an adhesive into the suspension to obtain slurry;
s4, the slurry is made into a paper machine for suction filtration and dehydration, and the wet paper web is obtained after dehydration;
s5, drying the wet paper web to obtain the basalt modified diaphragm; the drying temperature is 40-100 ℃, and the drying time is 12-24 hours.
The following is illustrative:
example 1: weighing 5g of basalt chopped fiber, 5g of 800 nm-1 mu m zirconia fiber, 0.3g of carbon fiber and 0.8g of polyvinylidene fluoride. Adding basalt chopped fibers into desalted water, stirring and fluffing, and adding zirconia fibers and carbon fibers and stirring after stirring and fluffing to obtain suspension; adding the dissolved adhesive polyvinylidene fluoride into the suspension to obtain slurry; and adding the slurry into a paper machine for suction filtration and dehydration, discharging after dehydration to obtain a wet paper web, and putting the wet paper web into a vacuum oven for drying at 50 ℃ for 24 hours, and taking out to obtain the basalt modified diaphragm.
The measurement is as follows: the thickness of the diaphragm is 1mm, and the surface resistance is 0.1 omega cm 2 (30 ℃) and the diaphragm is dried in a muffle furnace at 550 ℃ and has 0 percent of thermal shrinkage, the bubble point pressure is 1.2bar, the alkali absorption rate is 450 percent, and the operation density is 20013A/m 2 The mass per unit area of the diaphragm is 0.1g/cm 2 。
Example 2: weighing 6g of basalt chopped fiber, 5g of zirconia fiber with the diameter of 3-5 mu m, 0.2g of carbon fiber and 2g of sepiolite fiber. Adding basalt chopped fibers into desalted water, stirring and fluffing, and adding zirconia fibers, carbon fibers and sepiolite fibers after stirring and fluffing, and stirring to obtain suspension; in this example, no adhesive is added, so that the suspension is directly added into a paper machine for suction filtration and dehydration, and the wet paper web is obtained after dehydration and is put into a vacuum oven for drying at 70 ℃ for 12 hours and is taken out to obtain the basalt modified diaphragm.
The measurement is as follows: the thickness of the diaphragm is 2mm, and the surface resistance is 0.2 omega cm 2 (30 ℃) and the muffle furnace drying shrinkage rate of the diaphragm at 550 ℃ is 0%, the bubble point pressure is 1.1bar, the alkali absorption rate is 500%, and the operation density is 18632A/m 2 The mass per unit area of the diaphragm is 0.22g/cm 2 。
Example 3: 6g of basalt chopped fiber, 6g of zirconia fiber with the diameter of 3-5 mu m, 0.05g of carbon fiber and 0.5g of hydroxybutyronitrile emulsion are weighed. Adding basalt chopped fibers into desalted water, stirring and fluffing, adding zirconia fibers and carbon fibers after stirring and fluffing, stirring to obtain a suspension, and adding the dissolved adhesive hydroxybutyronitrile emulsion into the suspension to obtain slurry; and adding the slurry into a paper machine, carrying out suction filtration and dehydration, carrying out dehydration, and then taking out to obtain a wet paper web, and putting the wet paper web into a vacuum oven for drying at 40 ℃ for 24 hours, and taking out to obtain the basalt modified diaphragm.
The measurement is as follows: the thickness of the diaphragm is 3mm, and the surface resistance is 0.24 ohm cm 2 (30 ℃) and the diaphragm is 550 ℃, the drying shrinkage rate of a muffle furnace is 0%, the bubble point pressure is 1.2bar, the alkali absorption rate is 400%, and the operation density is 16816A/m 2 The mass per unit area of the diaphragm is 3.3g/cm 2 。
Example 4: weighing 6g of basalt long cut fibers, 5g of 800 nm-1 mu m zirconia fibers and 2g of sepiolite fibers. Adding basalt chopped fibers into desalted water, stirring and fluffing, and adding zirconia fibers and sepiolite fibers and stirring after stirring and fluffing to obtain suspension; in this example, no adhesive was added, so that the suspension was directly added to a paper machine, and subjected to suction filtration and dehydration, after which the wet paper web was obtained by draining, and the wet paper web was put into a vacuum oven for drying at 100 ℃ for 8 hours, and was taken out to obtain a basalt modified diaphragm.
The measurement is as follows: the thickness of the diaphragm is 0.5mm, and the surface resistance is 0.3 omega cm 2 (30 ℃) and the muffle furnace drying shrinkage rate of the diaphragm at 550 ℃ is 0%, the bubble point pressure is 1.1bar, the alkali absorption rate is 500%, and the operation density is 15345A/m 2 The mass per unit area of the diaphragm is 0.8g/cm 2 。
The results of the comparison of the diaphragm data measured in the previous examples with conventional industrial diaphragms are as follows.
Table 1: data comparison table of diaphragm
| Separator type | Thickness of (L) | Surface resistance | Temperature resistance | Bubble point pressure | Alkali absorption rate | Operating electric seal |
| Basalt chopped fiber modified separator of example 1 | 1mm | 0.1Ω•cm 2 （30℃） | 550℃ | 1.2bar | 450% | 20013A/m 2 |
| Basalt chopped fiber modified separator of example 2 | 2mm | 0.2Ω•cm 2 （30℃） | 550℃ | 1.1bar | 500% | 18632A/m 2 |
| Example 3 basalt chopped fiber modified separator | 3mm | 0.24Ω•cm 2 （30℃） | 550℃ | 1.2bar | 400% | 16816A/m 2 |
| Basalt long cut fiber modified separator of example 4 | 0.5mm | 0.3Ω•cm 2 （30℃） | 550℃ | 1.1bar | 500% | 15345A/m 2 |
| Industrial diaphragm-01 | 1.0mm | 0.3Ω•cm 2 （30℃） | 110℃ | 1bar | 168% | 3151A/m 2 |
| Industrial diaphragm-02 | 1.0mm | 0.3Ω•cm 2 （30℃） | 110℃ | 1bar | 138% | 2850A/m 2 |
The comparison results show that:
the surface resistance of the industrial diaphragm is larger than that of the basalt chopped fiber modified diaphragm under the same thickness, and when the industrial diaphragm is subjected to temperature resistance test, the temperature resistance of the industrial diaphragm is lower than that of the basalt chopped fiber modified diaphragm, and the basalt modified diaphragm has better alkaline absorption performance than that of the industrial diaphragm.
It should be noted that, the operation density in the data comparison table is the highest value obtained by testing the diaphragm in the testing process, and the operation density of the diaphragm in the actual use process can be lower than the highest value tested by the diaphragm.
The diaphragm with high temperature resistance and high operation density value is selected to improve the safety performance (avoid rupture of the diaphragm after the temperature rise caused by the over high operation density when the diaphragm is used) during the use, and simultaneously improve the productivity of the hydrogen production system.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. The high-temperature-resistant basalt modified diaphragm for the alkaline electrolytic tank is characterized by comprising the following raw materials in percentage by weight:
20-60% of basalt fiber, 30-50% of zirconia fiber, 300/111-5% of chopped carbon fiber, 0-20% of sepiolite fiber and 80/111-10% of adhesive;
wherein, the basalt fiber is long-cut fiber or short-cut fiber; the length of the zirconia fiber is 3-5 μm or 800 nm-1 μm;
when the basalt fiber is chopped fiber, the length of the zirconia fiber is 800 nm-1 mu m, and the adhesive is polyvinylidene fluoride;
when the basalt fiber is chopped fiber, the length of the zirconia fiber is 3-5 mu m, and the adhesive is hydroxybutyronitrile emulsion;
the thickness of the high temperature resistant basalt modified diaphragm is 0.1-3 mm, the surface resistance is 0.1-0.3 when the temperature is 30 ℃, the temperature resistance temperature interval is 50-550 ℃, and the operation density is 2000-20000A/m 2 The bubble point pressure is more than 1bar, and the alkali absorption rate is 100% -500%.
2. The high temperature resistant basalt modified diaphragm for alkaline electrolyzer of claim 1, wherein the length of the chopped carbon fiber is 3-5 mm.
3. A process for preparing a high temperature resistant basalt modified diaphragm for an alkaline electrolytic bath as claimed in any one of claims 1 to 2, comprising the steps of:
s1, taking quantitative basalt fibers and desalted water, stirring and fluffing to enable the slurry concentration to be 1-5%;
s2, adding one or more of zirconia fiber, carbon fiber or sepiolite fiber, and uniformly stirring to obtain suspension;
s3, adding an adhesive into the suspension to obtain slurry;
s4, the slurry is made into a paper machine for suction filtration and dehydration, and the wet paper web is obtained after dehydration;
s5, drying the wet paper web to obtain the basalt modified diaphragm.
4. The process for preparing the high-temperature-resistant basalt modified diaphragm for an alkaline electrolytic bath according to claim 3, wherein the drying temperature in the step S5 is 40-100 ℃ and the drying time period is 12-24 hours.
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| CN202310378083.7A CN116083955B (en) | 2023-04-11 | 2023-04-11 | High-temperature-resistant basalt modified diaphragm and preparation process thereof |
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| CN202310378083.7A CN116083955B (en) | 2023-04-11 | 2023-04-11 | High-temperature-resistant basalt modified diaphragm and preparation process thereof |
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| CN116083955B true CN116083955B (en) | 2023-06-30 |
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| BE1016238A3 (en) * | 2004-10-25 | 2006-05-02 | Frantschach Belcoat Nv | IMPROVED FIBER-REINFORCED FILM AND METHOD OF MAKING IT. |
| CN108511663A (en) * | 2018-03-27 | 2018-09-07 | 山东大学 | A kind of Zirconium oxide fibre paper mold battery diaphragm and preparation method thereof |
| CN108807799B (en) * | 2018-08-07 | 2020-04-28 | 吉林大学 | Expanded dickite modified lithium ion battery diaphragm and preparation method thereof |
| CN108929049A (en) * | 2018-08-21 | 2018-12-04 | 徐培培 | A method of Basalt fiber high-temperature resisting performance is promoted by surface modification |
| KR20210056053A (en) * | 2019-11-08 | 2021-05-18 | 경희대학교 산학협력단 | A graphene coated basalt fiber and a method for manufacturing the same |
| CN112397849B (en) * | 2020-10-28 | 2022-11-15 | 中国地质大学（北京） | High-temperature-resistant flame-retardant battery diaphragm and preparation method and application thereof |
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