CN108539236A - A kind of cross-linked proton exchange membrane and preparation method thereof - Google Patents
A kind of cross-linked proton exchange membrane and preparation method thereof Download PDFInfo
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- CN108539236A CN108539236A CN201810302274.4A CN201810302274A CN108539236A CN 108539236 A CN108539236 A CN 108539236A CN 201810302274 A CN201810302274 A CN 201810302274A CN 108539236 A CN108539236 A CN 108539236A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
- H01M8/1018—Polymeric electrolyte materials
- H01M8/1041—Polymer electrolyte composites, mixtures or blends
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/10—Esters
- C08F120/12—Esters of monohydric alcohols or phenols
- C08F120/14—Methyl esters, e.g. methyl (meth)acrylate
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
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- H01M8/1069—Polymeric electrolyte materials characterised by the manufacturing processes
- H01M8/1072—Polymeric electrolyte materials characterised by the manufacturing processes by chemical reactions, e.g. insitu polymerisation or insitu crosslinking
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Abstract
The invention discloses a kind of cross-linked proton exchange membranes, it is made of the raw material of following weight parts：Crosslinking agent taic 12, polyphenylene oxide 110 120, activated silica 10 15, sodium carboxymethylcellulose 12, methyl methacrylate 20 30, initiator 0.6 0.7, stannous sulfide 0.1 0.2, Sucrose acetoisobutyrate 12, barium stearate 23, the present invention uses crosslinking agent taic for crosslinking agent, using the polyester liquid as reaction dissolvent, polyphenylene ether progress is cross-linking modified, effectively raises the mechanics and conductive stability of finished product exchange membrane.
Description
Technical field
The invention belongs to exchange membrane fields, and in particular to a kind of cross-linked proton exchange membrane and preparation method thereof.
Background technology
Proton exchange membrane is the core component of PEMFC, and PEM has any different with the diaphragm used in general electrochmical power source.Proton
Clean materials of the substitution power source as PEM that exchange film fuel battery has become gasoline internal combustion mechanomotive force most competitiveness is answered
This meets the following conditions：The permeability that the electro-osmotic effects of good proton conductivity, hydrone in film are small, gas is in film
It is as small as possible, electrochemical stability is good, dry and wet conversion performance is good, with certain mechanical strength, machinability is good, price is suitable
When；However, presently commercially available proton exchange film dynamic performance is poor, stability is relatively low.
Invention content
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of cross-linked proton exchange membrane and its systems
Preparation Method.
To achieve the above object, the present invention uses following technical scheme：
A kind of cross-linked proton exchange membrane, it is made of the raw material of following weight parts：
Crosslinking agent taic 1-2, polyphenylene oxide 110-120, activated silica 10-15, sodium carboxymethylcellulose 1-2, metering system
Sour methyl esters 20-30, initiator 0.6-0.7, stannous sulfide 0.1-0.2, Sucrose acetoisobutyrate 1-2, barium stearate 2-3.
The initiator is cumyl peroxide.
The preparation method of the activated silica, includes the following steps：
（1）The diethylenetriamine for taking 2-3 parts by weight is added in the absolute ethyl alcohol of 5-8 times of its weight, stirs evenly, it is molten to obtain alcohol
Liquid；
（2）The nano silicon dioxide of 30-40 parts by weight, the barium stearate mixing of 0.1-0.2 parts by weight are taken, is protected at 50-55 DEG C
Temperature stirring 10-20 minutes, is added above-mentioned alcoholic solution, stirs evenly, and ethyl alcohol is distilled off, and the oleic acid of 1-1.5 parts by weight is added, and rises
High-temperature be 65-70 DEG C, insulated and stirred 20-30 minute, filtering, will precipitation washing, air drying to get.
A kind of preparation method of cross-linked proton exchange membrane, includes the following steps：
（1）Sodium carboxymethylcellulose is taken, is added in the deionized water of 16-20 times of its weight, stirs evenly, obtain aqueous dispersions；
（2）Stannous sulfide, activated silica mixing are taken, insulated and stirred 30-40 minutes at 60-65 DEG C, is added to mixture
It in the deionized water of 10-15 times of weight, stirs evenly, obtains nano dispersion fluid；
（3）Initiator is taken, is added in the absolute ethyl alcohol of 10-18 times of its weight, stirs evenly, obtain alcoholic solution；
（4）Above-mentioned aqueous dispersions, nano dispersion fluid mixing are taken, stirs evenly, methyl methacrylate is added, stirs evenly, send
Enter into reaction kettle, is passed through nitrogen, it is 65-70 DEG C to adjust temperature of reaction kettle, is added above-mentioned alcoholic solution, insulated and stirred 4-5 hours,
Discharging cooling, obtains polymer dispersion liquid；
（5）Crosslinking agent taic is taken, is added in above-mentioned polymer dispersion liquid, stirs evenly, Sucrose acetoisobutyrate is added, is risen
High-temperature is 80-90 DEG C, and polyphenylene oxide, insulated and stirred 100-130 minutes is added, and precipitation is washed in filtering, at 50-55 DEG C of vacuum
It is 1-2 hours dry, it is cooled to room temperature, obtains Noryl；
（6）Barium stearate, Noryl mixing are taken, is added in the dimethylformamide of 17-20 times of mixture weight, ultrasound
It 1-2 hours, pours into culture dish, is put into vacuum drying chamber, be dried in vacuo 20-30 hours at 70-85 DEG C, after film molding,
It is put into 95-105 DEG C of thermostatic drying chamber to handle 1-2 hours, takes off film, film water is washed, air drying is handed over to get the crosslinking proton
Change film.
Advantages of the present invention：
The present invention improves silica with stearate processing silica by the surface adsorption property of stearate
Then surface-active uses the amidation process of diethylenetriamine and oleic acid, further improves its reactivity, the present invention with
Methyl methacrylate is monomer, using activated silica aqueous solution as reaction dissolvent, polymerize under initiator effect, obtains nanometer
Then modified polyester liquid uses crosslinking agent taic for crosslinking agent, using the polyester liquid as reaction dissolvent, polyphenylene ether carries out
It is cross-linking modified, effectively raise the mechanics and conductive stability of finished product exchange membrane.
Specific implementation mode
Embodiment 1
A kind of cross-linked proton exchange membrane, it is made of the raw material of following weight parts：
Crosslinking agent taic 1, polyphenylene oxide 110, activated silica 10, sodium carboxymethylcellulose 1, methyl methacrylate 20, draw
Send out agent 0.6, stannous sulfide 0.1, Sucrose acetoisobutyrate 1, barium stearate 2.
The initiator is cumyl peroxide.
The preparation method of the activated silica, includes the following steps：
（1）The diethylenetriamine for taking 2 parts by weight is added in the absolute ethyl alcohol of 5 times of its weight, stirs evenly, obtain alcoholic solution；
（2）The nano silicon dioxide of 30 parts by weight, the barium stearate mixing of 0.1 parts by weight are taken, insulated and stirred 10 is divided at 50 DEG C
Clock is added above-mentioned alcoholic solution, stirs evenly, and ethyl alcohol is distilled off, and the oleic acid of 1 parts by weight is added, and it is 65 DEG C to increase temperature, heat preservation
Stirring 20 minutes, filtering, will precipitation washing, air drying to get.
A kind of preparation method of cross-linked proton exchange membrane, includes the following steps：
（1）Sodium carboxymethylcellulose is taken, is added in the deionized water of 16 times of its weight, is stirred evenly, obtain aqueous dispersions；
（2）Stannous sulfide, activated silica mixing are taken, insulated and stirred 30 minutes at 65 DEG C are added to mixture weight 10
In deionized water again, stirs evenly, obtain nano dispersion fluid；
（3）Initiator is taken, is added in the absolute ethyl alcohol of 10 times of its weight, is stirred evenly, obtain alcoholic solution；
（4）Above-mentioned aqueous dispersions, nano dispersion fluid mixing are taken, stirs evenly, methyl methacrylate is added, stirs evenly, send
Enter into reaction kettle, be passed through nitrogen, it is 65 DEG C to adjust temperature of reaction kettle, and above-mentioned alcoholic solution, insulated and stirred 4 hours, discharging is added
It is cooling, obtain polymer dispersion liquid；
（5）Crosslinking agent taic is taken, is added in above-mentioned polymer dispersion liquid, stirs evenly, Sucrose acetoisobutyrate is added, is risen
High-temperature is 80 DEG C, and polyphenylene oxide, insulated and stirred 100 minutes is added, and precipitation is washed in filtering, 1 hour dry at 50 DEG C of vacuum,
It is cooled to room temperature, obtains Noryl；
（6）Barium stearate, Noryl mixing are taken, is added in the dimethylformamide of 17 times of mixture weight, ultrasound 1 is small
When, it pours into culture dish, is put into vacuum drying chamber, be dried in vacuo 20 hours at 70 DEG C, after film molding, be put into 95-105 DEG C
Thermostatic drying chamber handle 1 hour, take off film, film water washed, air drying is to get the cross-linked proton exchange membrane.
Embodiment 2
A kind of cross-linked proton exchange membrane, it is made of the raw material of following weight parts：
Crosslinking agent taic 2, polyphenylene oxide 120, activated silica 15, sodium carboxymethylcellulose 2, methyl methacrylate 30, draw
Send out agent 0.7, stannous sulfide 0.2, Sucrose acetoisobutyrate 2, barium stearate 3.
The initiator is cumyl peroxide.
The preparation method of the activated silica, includes the following steps：
（1）The diethylenetriamine for taking 3 parts by weight is added in the absolute ethyl alcohol of 8 times of its weight, stirs evenly, obtain alcoholic solution；
（2）The nano silicon dioxide of 40 parts by weight, the barium stearate mixing of 0.2 parts by weight are taken, insulated and stirred 20 is divided at 55 DEG C
Clock is added above-mentioned alcoholic solution, stirs evenly, and ethyl alcohol is distilled off, and the oleic acid of 1.5 parts by weight is added, and it is 70 DEG C to increase temperature, is protected
Temperature stirring 30 minutes, filtering, will precipitation washing, air drying to get.
A kind of preparation method of cross-linked proton exchange membrane, includes the following steps：
（1）Sodium carboxymethylcellulose is taken, is added in the deionized water of 20 times of its weight, is stirred evenly, obtain aqueous dispersions；
（2）Stannous sulfide, activated silica mixing are taken, insulated and stirred 40 minutes at 65 DEG C are added to mixture weight 15
In deionized water again, stirs evenly, obtain nano dispersion fluid；
（3）Initiator is taken, is added in its heavy 18 times absolute ethyl alcohol, is stirred evenly, obtain alcoholic solution；
（4）Above-mentioned aqueous dispersions, nano dispersion fluid mixing are taken, stirs evenly, methyl methacrylate is added, stirs evenly, send
Enter into reaction kettle, be passed through nitrogen, it is 65-70 DEG C to adjust temperature of reaction kettle, above-mentioned alcoholic solution is added, insulated and stirred 5 hours goes out
Material cooling, obtains polymer dispersion liquid；
（5）Crosslinking agent taic is taken, is added in above-mentioned polymer dispersion liquid, stirs evenly, Sucrose acetoisobutyrate is added, is risen
High-temperature is 90 DEG C, and polyphenylene oxide, insulated and stirred 130 minutes is added, and precipitation is washed in filtering, 2 hours dry at 55 DEG C of vacuum,
It is cooled to room temperature, obtains Noryl；
（6）Barium stearate, Noryl mixing are taken, is added in the dimethylformamide of 20 times of mixture weight, ultrasound 2 is small
When, it pours into culture dish, is put into vacuum drying chamber, be dried in vacuo 30 hours at 85 DEG C, after film molding, be put into 95-105 DEG C
Thermostatic drying chamber handle 2 hours, take off film, film water washed, air drying is to get the cross-linked proton exchange membrane.
Performance test：
Performance measurement is carried out to the cross-linked proton exchange membrane that embodiment 1-2 is prepared, film dynamic performance is according to GB4456-1996
Test；
The proton conductivity of the cross-linked proton exchange membrane of embodiment 1 is 3.01 × 10-2Scm-1, mechanical mechanics property 25.0Mpa；
The proton conductivity of the cross-linked proton exchange membrane of embodiment 2 is 3.06 × 10-2Scm-1, mechanical mechanics property 26.1Mpa；
The proton conductivity of commercially available polyphenylene oxide proton exchange membrane is 2-2.5 × 10-2Scm-1Mechanical mechanics property 10-15Mpa.
Claims (4)
1. a kind of cross-linked proton exchange membrane, which is characterized in that it is made of the raw material of following weight parts：
Crosslinking agent taic 1-2, polyphenylene oxide 110-120, activated silica 10-15, sodium carboxymethylcellulose 1-2, metering system
Sour methyl esters 20-30, initiator 0.6-0.7, stannous sulfide 0.1-0.2, Sucrose acetoisobutyrate 1-2, barium stearate 2-3.
2. a kind of cross-linked proton exchange membrane according to claim 1, which is characterized in that the initiator is peroxidating two
Isopropylbenzene.
3. a kind of cross-linked proton exchange membrane according to claim 1, which is characterized in that the system of the activated silica
Preparation Method includes the following steps：
（1）The diethylenetriamine for taking 2-3 parts by weight is added in the absolute ethyl alcohol of 5-8 times of its weight, stirs evenly, it is molten to obtain alcohol
Liquid；
（2）The nano silicon dioxide of 30-40 parts by weight, the barium stearate mixing of 0.1-0.2 parts by weight are taken, is protected at 50-55 DEG C
Temperature stirring 10-20 minutes, is added above-mentioned alcoholic solution, stirs evenly, and ethyl alcohol is distilled off, and the oleic acid of 1-1.5 parts by weight is added, and rises
High-temperature be 65-70 DEG C, insulated and stirred 20-30 minute, filtering, will precipitation washing, air drying to get.
4. a kind of preparation method of cross-linked proton exchange membrane as described in claim 1, which is characterized in that include the following steps：
（1）Sodium carboxymethylcellulose is taken, is added in the deionized water of 16-20 times of its weight, stirs evenly, obtain aqueous dispersions；
（2）Stannous sulfide, activated silica mixing are taken, insulated and stirred 30-40 minutes at 60-65 DEG C, is added to mixture
It in the deionized water of 10-15 times of weight, stirs evenly, obtains nano dispersion fluid；
（3）Initiator is taken, is added in the absolute ethyl alcohol of 10-18 times of its weight, stirs evenly, obtain alcoholic solution；
（4）Above-mentioned aqueous dispersions, nano dispersion fluid mixing are taken, stirs evenly, methyl methacrylate is added, stirs evenly, send
Enter into reaction kettle, is passed through nitrogen, it is 65-70 DEG C to adjust temperature of reaction kettle, is added above-mentioned alcoholic solution, insulated and stirred 4-5 hours,
Discharging cooling, obtains polymer dispersion liquid；
（5）Crosslinking agent taic is taken, is added in above-mentioned polymer dispersion liquid, stirs evenly, Sucrose acetoisobutyrate is added, is risen
High-temperature is 80-90 DEG C, and polyphenylene oxide, insulated and stirred 100-130 minutes is added, and precipitation is washed in filtering, at 50-55 DEG C of vacuum
It is 1-2 hours dry, it is cooled to room temperature, obtains Noryl；
（6）Barium stearate, Noryl mixing are taken, is added in the dimethylformamide of 17-20 times of mixture weight, ultrasound
It 1-2 hours, pours into culture dish, is put into vacuum drying chamber, be dried in vacuo 20-30 hours at 70-85 DEG C, after film molding,
It is put into 95-105 DEG C of thermostatic drying chamber to handle 1-2 hours, takes off film, film water is washed, air drying is handed over to get the crosslinking proton
Change film.
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| CN201810302274.4A CN108539236A (en) | 2018-04-04 | 2018-04-04 | A kind of cross-linked proton exchange membrane and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113097548A (en) * | 2021-03-01 | 2021-07-09 | 吴丹 | Multi-fiber doped sulfonated polyphenyl ether proton exchange membrane and preparation method thereof |
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2018
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113097548A (en) * | 2021-03-01 | 2021-07-09 | 吴丹 | Multi-fiber doped sulfonated polyphenyl ether proton exchange membrane and preparation method thereof |
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Application publication date: 20180914 |