CN106397801B - A kind of doping load G8-2-8The preparation method of the modified fuel cell anionic membrane of the mesoporous silicon oxide polysulfones of/NaSal micelle volume - Google Patents
A kind of doping load G8-2-8The preparation method of the modified fuel cell anionic membrane of the mesoporous silicon oxide polysulfones of/NaSal micelle volume Download PDFInfo
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Abstract
The present invention relates to a kind of doping to load G8‑2‑8The preparation method of the modified fuel cell anionic membrane of the mesoporous silicon oxide polysulfones of/NaSal micelle volume.Using chloroform as solvent, polysulfones (PSF) particle is completely dissolved, as film base fluid.Using blending method, there is the mesoporous silicon oxide Uniform Doped of G8-2-8/NaSal micelle volume into the chloroform casting solution of polysulfones load.It pours film forming on a glass using the tape casting, then by the film immersion after drying in KOH solution, prepares hydroxide ion type composite membrane.Anionic membrane prepared by the present invention has low swelling, excellent high temperature alkali resistant stability, good mechanical performance, especially in the case where ion exchange capacity and not high moisture content, ion transfer efficiency is improved by orderly constructing the method for OH- transmission channel, and then improves conductivity.The problems such as solving graft modification means causes film to be excessively swollen, and alkali resistance is deteriorated.
Description
Technical field
The invention belongs to field of fuel cell technology, are related to the film electrolyte preparation skill of anion-exchange membrane fuel cells
A kind of art, and in particular to doping load G8-2-8The modified fuel cell yin of the mesoporous silicon oxide polysulfones of/NaSal micelle volume
The preparation method of ionic membrane.
Background technique
Core component of the anion-exchange membrane (AEMs) as anion-exchange membrane fuel cells (AEMFCs), in AEMFCs
In play important role.However, due to OH-Mobility be significantly lower than H+, cause the conductivity of AEMs relatively relatively low.At present
Generally use improve it is quaternized, season the grafting rate of the electropositive groups such as phosphine obtain higher ion exchange capacity, and then improve
The OH of film electrolyte-Conductivity.Such as triphenylphosphine by being grafted on the alkalinity synthesized on polyarylethersulfone polymer by Gu etc.
Membrane conductivity is 45mscm-1, but film forming is poor.Dalian Chemistry and Physics Institute Zhang Fengxiang etc. utilizes chloromethylation polyether sulfone and 1- methyl
Imidazoles, which reacts, is made chloromethylation degree of substitution (DCM) as 1.35 imidazole type anion-exchange membranes, and 20 DEG C of conductivity are about 21
ms·cm-1, but impregnate rear conductivity loss late for 24 hours in 60 DEG C of 3M NaOH aqueous solutions and be up to 23.3%, and film color change is bright
It is aobvious.In conclusion quaternary amines or season phosphine anion-exchange membrane are primarily present two problems: although (1) high grafting rate improves
Conductivity, but will definitely increase moisture content, this, which will will lead to film and excessively be swollen, substantially reduces high temperature alkali resistant stability
(Hoffmann degradation reaction, nucleophilic displacement of fluorine degradation reaction) and mechanical performance；(2) preparation process complicated and time consumption and need make
With carcinogenic compound --- iodomethane.So far, there are no a kind of satisfactory method, it can be improved the same of conductivity
When, the appropriateness swelling of film is kept, and then do not damage other correlated performances of its film excessively.
Summary of the invention
The present invention provides a kind of doping load G8-2-8The modified yin of the mesoporous silicon oxide polysulfones of/NaSal micelle volume from
The preparation method of sub- film, by G8-2-8Surfactant is in Organic counter-ion salicylate (Sal-) be self-assembly of under induction
Positive micelle volume causes polymerization under initiator (KPS) effect in mesoporous silicon oxide duct, utilizes micella outer surface cloth
Annular water conservation chamber is collectively formed in the silicone hydroxyl of full quaternary ammonium cation and silicon hole road inner wall, to construct OH-Ionic conducting path.
Positive micelle forma-tion process above-mentioned is transplanted in the casting solution of polysulfones and is completed, thus constructs suitable by the means of in-situ polymerization
The anion-exchange membrane of fuel cell.
Doping load G8-2-8The preparation method of the modified anionic membrane of the mesoporous silicon oxide polysulfones of/NaSal micelle volume
Specific step is as follows:
Step (1) weighs 1.2g mesoporous silicon oxide and is added to the water mesoporous silicon oxide aqueous solution is made, and thereto plus
Enter the G that a certain amount of purity is 33%8-2-8Type surfactant molecule makes it account for the mass fraction 5-20% of polysulfones system, to
G8-2-8After being completely dissolved, NaSal is added thereto, low speed magnetic rotor stirs under room temperature, and initiator is added every 30min
KPS, initiator KPS additional amount account for total mass fraction 1%, are added in three times, and after reaction carries out 3h, the mixing that reaction is obtained is molten
Liquid is filtered after being placed in a beaker static 1h with filter paper, obtains white much filtrate；
White much filtrate is impregnated in the KOH solution of 1M and carries out ion exchange by step (2), carries out primary mistake every 12h
Filter operates and replaces KOH solution, 3 times repeatedly, obtains white much filtrate；
Step (3) weighs 4g polysulfones particle, is added in the beaker of the chloroform solvent containing 30ml, carries out at normal temperature
Magnetic agitation continues to obtain casting film after stirring is sufficiently mixed until the white much filtrate that step (2) obtain is added in polysulfones after being completely dissolved
Liquid, using the tape casting in horizontal glass plate casting film, taken off after film natural air drying.
The preparation method of described step (1) the intermediary hole silica includes the following steps:
.A, 0.5g is weighed, 5.7mM cetyl trimethylammonium bromide and 0.28g sodium hydroxide are dissolved in 480mL deionized water
In, 7mL mesitylene is added later, is vigorously stirred and is heated to 80 DEG C, 5mL ethyl orthosilicate is added dropwise, continuation is acutely stirred
Mix 2h；After reaction, solution becomes white, and lower layer has precipitating to generate；Acquired solution is filtered, with excessive ethanol washing, and
It is dried in vacuo at 100 DEG C, obtains white powder；
B, it weighs 0.4g ammonium nitrate to be dissolved in the ethyl alcohol of 150mL 95%, the above-mentioned dried white powder of 1g is added later
In the mixed solution, and 5h being stirred at 60 DEG C, after reaction, sample being filtered, excess ethyl alcohol washing, room temperature in vacuo is done
It is dry to get arrive mesoporous silicon oxide.
The mass volume ratio of step (1) the intermediary hole silica and water is that 1.2g mesoporous silicon oxide is dissolved in
100mL water.
In the step (1), the amount and G of the substance of NaSal8-2-8The ratio between the amount of substance r be 10, i.e. r=nNaSal/
G8-2-8=10.
Anionic membrane material prepared by the present invention shows the conductance of the series membranes by the high-temp alkali-resistant test of 400h
The rate range of decrease is only 1.5% or so, and exterior appearance does not have significant change, embodies excellent high temperature alkali resistant stability.G8-2-8/
The introducing of NaSal micelle volume, makes OH-The transport efficiency of ion obtains in the case where ion exchange capacity and not high moisture content
It is higher to being obviously improved.In conclusion the composite membrane phase that anionic membrane prepared by the present invention is used with existing fuel cell
Than having the advantage that
(1) this research does not use the preparation method that traditional grafting means improve ion exchange capacity, but by G8-2-8/NaSal
Micelle volume introduces in polysulfones skeleton, makes anionic membrane the case where not increasing ion exchange capacity, conductivity is improved 50-
70%.
(2) for the series anionic film in the test of 400h high-temp alkali-resistant, the conductivity maximum range of decrease is only 1.5% or so,
And exterior appearance does not have significant change, shows excellent high temperature alkali resistant stability.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of anion-exchange membrane.
Fig. 2 is embodiment 1, embodiment 2, embodiment 3, the moisture content situation schematic diagram of 4 anion-exchange membrane of embodiment.
Fig. 3 is embodiment 1, embodiment 2, embodiment 3, the rate of water absorption and swellbility feelings of 4 anion-exchange membrane of embodiment
Condition schematic diagram.
Fig. 4 is embodiment 1, embodiment 2, embodiment 3, the conductivity variation with temperature of 4 anion-exchange membrane of embodiment
Situation schematic diagram.
Fig. 5 is embodiment 1, and embodiment 2, embodiment 3, it is molten that 4 anion-exchange membrane of embodiment is soaked in 60 DEG C of 3M NaOH
The alkali stability schematic diagram of 400h in liquid.
Table 1. is the mesoporous SiO for loading G8-2-8/NaSal micelle volume2Particle adsorption desorption result parameter.
Table 2. be NaSal be added front and back embodiment 1, embodiment 2, embodiment 3, the conductivity of 4 anionic membrane of embodiment and
Ion exchange capacity.
Table 3. be 4 anion-exchange membrane of embodiment be separately immersed in 60 DEG C of 3M and 10M NaOH solutions mechanical performance and from
Sub- exchange capacity.
Specific embodiment
Method of the invention is further illustrated by the following examples.
Embodiment 1
(1) it weighs in 1.2g mesoporous silicon oxide addition 100mL water and mesoporous silicon oxide aqueous solution is made, and add thereto
Enter the G that a certain amount of purity is 33%8-2-8Type surfactant molecule makes it account for the mass fraction of polysulfones system 5%, to
G8-2-8After being completely dissolved, NaSal is added thereto, the amount and G of the substance of NaSal8-2-8The ratio between the amount of substance r be 10, i.e. r
=nNaSal/G8-2-8=10, low speed magnetic rotor stirs under room temperature, and initiator KPS is added every 30min, and initiator KPS adds
Enter amount and account for total mass fraction 1%, be added in three times, after reaction carries out 3h, the mixed solution that reaction obtains is placed in a beaker quiet
It is only filtered after 1h with filter paper, obtains white much filtrate.
(2) white much filtrate is impregnated in the KOH solution of 1M and carries out ion exchange, carry out primary filtering behaviour every 12h
Make and replace KOH solution, 3 times repeatedly, obtains white much filtrate.
(3) 4g polysulfones particle is weighed, is added in the beaker of the chloroform solvent containing 30ml, magnetic force is carried out at normal temperature and stirs
It mixes, until the white much filtrate that step (2) obtain is added in polysulfones after being completely dissolved, continues to obtain casting solution after stirring is sufficiently mixed, adopt
With the tape casting in horizontal glass plate casting film, taken off after film natural air drying.
Embodiment 2
(1) it weighs in a certain amount of water of 1.2g mesoporous silicon oxide addition and mesoporous silicon oxide aqueous solution is made, and thereto
The G that a certain amount of purity is 33% is added8-2-8Type surfactant molecule makes it account for the mass fraction of polysulfones system 10%, to
G8-2-8After being completely dissolved, NaSal is added thereto, the amount and G of the substance of NaSal8-2-8The ratio between the amount of substance r be 10, i.e. r
=nNaSal/G8-2-8=10, low speed magnetic rotor stirs under room temperature, and initiator KPS is added every 30min, and initiator KPS adds
Enter amount and account for total mass fraction 1%, be added in three times, after reaction carries out 3h, the mixed solution that reaction obtains is placed in a beaker quiet
It is only filtered after 1h with filter paper, obtains white much filtrate.
(2) white much filtrate is impregnated in the KOH solution of 1M and carries out ion exchange, carry out primary filtering behaviour every 12h
Make and replace KOH solution, 3 times repeatedly, obtains white much filtrate.
(3) 4g polysulfones particle is weighed, is added in the beaker of the chloroform solvent containing 30ml, magnetic force is carried out at normal temperature and stirs
It mixes, until the white much filtrate that step (2) obtain is added in polysulfones after being completely dissolved, continues to obtain casting solution after stirring is sufficiently mixed, adopt
With the tape casting in horizontal glass plate casting film, taken off after film natural air drying.
Embodiment 3
(1) it weighs in a certain amount of water of 1.2g mesoporous silicon oxide addition and mesoporous silicon oxide aqueous solution is made, and thereto
The G that a certain amount of purity is 33% is added8-2-8Type surfactant molecule makes it account for the mass fraction of polysulfones system 15%, to
G8-2-8After being completely dissolved, NaSal is added thereto, the amount and G of the substance of NaSal8-2-8The ratio between the amount of substance r be 10, i.e. r
=nNaSal/G8-2-8=10, low speed magnetic rotor stirs under room temperature, and initiator KPS is added every 30min, and initiator KPS adds
Enter amount and account for total mass fraction 1%, be added in three times, after reaction carries out 3h, the mixed solution that reaction obtains is placed in a beaker quiet
It is only filtered after 1h with filter paper, obtains white much filtrate.
(2) white much filtrate is impregnated in the KOH solution of 1M and carries out ion exchange, carry out primary filtering behaviour every 12h
Make and replace KOH solution, 3 times repeatedly, obtains white much filtrate.
(3) 4g polysulfones particle is weighed, is added in the beaker of the chloroform solvent containing 30ml, magnetic force is carried out at normal temperature and stirs
It mixes, until the white much filtrate that step (2) obtain is added in polysulfones after being completely dissolved, continues to obtain casting solution after stirring is sufficiently mixed, adopt
With the tape casting in horizontal glass plate casting film, taken off after film natural air drying.
Embodiment 4
(1) it weighs in a certain amount of water of 1.2g mesoporous silicon oxide addition and mesoporous silicon oxide aqueous solution is made, and thereto
The G that a certain amount of purity is 33% is added8-2-8Type surfactant molecule makes it account for the mass fraction of polysulfones system 20%, to
G8-2-8After being completely dissolved, NaSal is added thereto, the amount and G of the substance of NaSal8-2-8The ratio between the amount of substance r be 10, i.e. r
=nNaSal/G8-2-8=10, low speed magnetic rotor stirs under room temperature, and initiator KPS is added every 30min, and initiator KPS adds
Enter amount and account for total mass fraction 1%, be added in three times, after reaction carries out 3h, the mixed solution that reaction obtains is placed in a beaker quiet
It is only filtered after 1h with filter paper, obtains white much filtrate.
(2) white much filtrate is impregnated in the KOH solution of 1M and carries out ion exchange, carry out primary filtering behaviour every 12h
Make and replace KOH solution, 3 times repeatedly, obtains white much filtrate.
(3) 4g polysulfones particle is weighed, is added in the beaker of the chloroform solvent containing 30ml, magnetic force is carried out at normal temperature and stirs
It mixes, until the white much filtrate that step (2) obtain is added in polysulfones after being completely dissolved, continues to obtain casting solution after stirring is sufficiently mixed, adopt
With the tape casting in horizontal glass plate casting film, taken off after film natural air drying.
In above-described embodiment 1-4, the preparation method of the step (1) intermediary hole silica includes the following steps:
.A, 0.5g is weighed, 5.7mM cetyl trimethylammonium bromide and 0.28g sodium hydroxide are dissolved in 480mL deionized water
In, 7mL mesitylene is added later, is vigorously stirred and is heated to 80 DEG C, 5mL ethyl orthosilicate is added dropwise, continuation is acutely stirred
Mix 2h；After reaction, solution becomes white, and lower layer has precipitating to generate；Acquired solution is filtered, with excessive ethanol washing, and
It is dried in vacuo at 100 DEG C, obtains white powder；
B, it weighs 0.4g ammonium nitrate to be dissolved in the ethyl alcohol of 150mL 95%, the above-mentioned dried white powder of 1g is added later
In the mixed solution, and 5h being stirred at 60 DEG C, after reaction, sample being filtered, excess ethyl alcohol washing, room temperature in vacuo is done
It is dry to get arrive mesoporous silicon oxide.
Table .1 loads G8-2-8The mesoporous SiO of/NaSal micelle volume2Particle adsorption desorption result parameter
The conductivity and ion exchange capacity of front and back anionic membrane is added in table .2 NaSal
Anionic membrane prepared by table .3 embodiment 4 is separately immersed in the mechanical performance in 60 DEG C of 3M and 10M NaOH solutions
And ion exchange capacity
[a]Theoretical IEC value:0.64mmol·g-1。
Claims (4)
1. a kind of doping loads G8-2-8The modified fuel cell anion of the mesoporous silicon oxide polysulfones of/NaSal micelle volume
The preparation method of film, it is characterised in that steps are as follows:
Step (1) weighs 1.2 g mesoporous silicon oxides and is added to the water mesoporous silicon oxide aqueous solution is made, and is added thereto
A certain amount of purity is the G of 33 %8-2-8Type surfactant molecule makes it account for the mass fraction 5-20 % of polysulfones system, to
G8-2-8After being completely dissolved, NaSal is added thereto, low speed magnetic rotor stirs under room temperature, and initiator is added every 30 min
KPS, initiator KPS additional amount account for total mass fraction 1%, are added in three times, and after reaction carries out 3 h, the mixing that reaction is obtained is molten
Liquid is filtered after being placed in a beaker static 1 h with filter paper, obtains white much filtrate；
The polysulfones system are as follows: weigh 4 g polysulfones particles, be added in the beaker of the chloroform solvent containing 30 ml, in room temperature
Lower carry out magnetic agitation, obtains polysulfones system；
White much filtrate is impregnated in the KOH solution of 1 M and carries out ion exchange by step (2), is once filtered every 12 h
KOH solution is operated and replaced, 3 times repeatedly, obtains white much filtrate；
The white that step (2) obtain is added in the polysulfones in polysulfones system in step (3), the step (1) after being completely dissolved
Much filtrate, continue stirring be sufficiently mixed after casting solution, using the tape casting in horizontal glass plate casting film, to film natural wind
It is taken off after dry.
2. a kind of doping according to claim 1 loads G8-2-8The mesoporous silicon oxide polysulfones of/NaSal micelle volume is modified
Fuel cell anionic membrane preparation method, it is characterised in that the preparation side of described step (1) the intermediary hole silica
Method includes the following steps:
A, 0.5 g is weighed, 5.7 mM cetyl trimethylammonium bromides and 0.28 g sodium hydroxide are dissolved in 480 mL deionized waters
In, 7 mL mesitylene are added later, are vigorously stirred and are heated to 80 C, 5 mL ethyl orthosilicates are added dropwise, continue violent
Stir 2 h；After reaction, solution becomes white, and lower layer has precipitating to generate；Acquired solution is filtered, with excessive ethanol washing,
And be dried in vacuo under 100 C, obtain white powder；
B, it weighs 0.4 g ammonium nitrate to be dissolved in the ethyl alcohol of 150 mL 95%, the above-mentioned dried white powder of 1 g is added later
In the mixed solution, and 5 h are stirred under 60 C, after reaction, sample is filtered, excess ethyl alcohol washing, room temperature in vacuo
It dries to get mesoporous silicon oxide is arrived.
3. a kind of doping according to claim 1 loads G8-2-8The mesoporous silicon oxide polysulfones of/NaSal micelle volume is modified
Fuel cell anionic membrane preparation method, it is characterised in that the matter of described step (1) the intermediary hole silica and water
Measuring volume ratio is that 1.2 g mesoporous silicon oxides are dissolved in 100 mL water.
4. a kind of doping according to claim 1 loads G8-2-8The mesoporous silicon oxide polysulfones of/NaSal micelle volume is modified
Fuel cell anionic membrane preparation method, it is characterised in that in the step (1), the amount of the substance of NaSal with
G8-2-8The ratio between the amount of substance r be 10, i.e. r=n(NaSal)/n(G8-2-8)=10.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102430349A (en) * | 2011-12-22 | 2012-05-02 | 中国海洋大学 | Reverse osmosis composite membrane and preparation method thereof |
| CN105170122A (en) * | 2015-10-09 | 2015-12-23 | 辽宁石油化工大学 | Preparation method and application of full-interpenetrating membrane based on quaternized polyvinyl alcohols |
| CN105280928A (en) * | 2015-09-17 | 2016-01-27 | 辽宁石油化工大学 | Preparation method of polysulfone modification based anionic membrane having ultralow aqueous solution swelling degree for fuel cell |
| CN105384955A (en) * | 2015-10-09 | 2016-03-09 | 辽宁石油化工大学 | Preparation method of anion exchange membrane capable of introducing surfactant molecules to be used as cationic sites |
Family Cites Families (1)
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| US20110071056A1 (en) * | 2009-09-24 | 2011-03-24 | Rajesh K Saini | Degradable Surfactants, Including Degradable Gemini Surfactants, and Associated Methods |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102430349A (en) * | 2011-12-22 | 2012-05-02 | 中国海洋大学 | Reverse osmosis composite membrane and preparation method thereof |
| CN105280928A (en) * | 2015-09-17 | 2016-01-27 | 辽宁石油化工大学 | Preparation method of polysulfone modification based anionic membrane having ultralow aqueous solution swelling degree for fuel cell |
| CN105170122A (en) * | 2015-10-09 | 2015-12-23 | 辽宁石油化工大学 | Preparation method and application of full-interpenetrating membrane based on quaternized polyvinyl alcohols |
| CN105384955A (en) * | 2015-10-09 | 2016-03-09 | 辽宁石油化工大学 | Preparation method of anion exchange membrane capable of introducing surfactant molecules to be used as cationic sites |
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