CN102765782B - Method for preparing hierarchical porous carbon capacitive deionization electrode - Google Patents
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Abstract
The invention relates to a method for preparing a hierarchical porous carbon capacitive deionization electrode and belongs to the field of preparation of capacitive deionization electrodes. According to the method, a silica template is immersed in a precursor solution of a mesoporous carbon material, the carbon material with a hierarchical pore structure is formed on silica spheres by the processes of low temperature volatilization, high temperature curing, carbonization in inert atmosphere and the like, and the porous carbon material with macropores, meso pores and micropores is obtained by hydrofluoric acid etching. The porous carbon material, acetylene black and teflon emulsion are mixed uniformly to be smeared on graphite paper, and the graphite paper onto which a mixture of the porous carbon material, the acetylene black and the teflon emulsion is smeared is dried after the night to form the hierarchical porous carbon capacitive deionization electrode. The method is easy to operate and has potential application prospect in the aspect of capacitive deionization which is low in energy consumption and cost and high in efficiency; conditions are easy to control; and the obtained electrode is large in specific surface, high in electrical conductivity and high in deionization performance.
Description
Technical field
The present invention relates to a kind of preparation method of multi-stage porous carbon structure capacitance desalination electrode.The desalination electrode of the present invention's preparation has the desalting performance of high-level efficiency, less energy-consumption.Belong to the desalination that the present invention of electric desalting electrode manufacturing process technical field can be applicable to seawater and brackish water, for less energy-consumption, low cost, high-performance desalination provide new way.
Background technology
Water resources crisis is one of maximum resource crisis that this century, the whole world faced, and seawater and brackish water desalting are the important channels that solves this crisis.Existing desalting method mainly contains distillation method (comprising multistage flash evaporation, multistage evaporation and the distillation of calming the anger) and embrane method (comprising reverse osmosis and electrodialysis).But the distillation method service temperature is high, bird nest harm is serious, seriously corroded; Embrane method is strict to film properties, the film spoilage is high and somewhat expensive.In addition, all there is the shortcoming that energy consumption is high, cost is large in these desalting method.Reduce desalinating cost so employ new technology is the most important developing goal of desalination technology always.Therefore, research and development energy consumption desalting technology application prospect low, that cost is low is very bright.Structure capacitance desalination (Capacitive Deionization; CDI) be based on the brand-new desalting technology of electric double layer capacitance principle.Compare with traditional desalting method, the method has that cost is low, desalting efficiency is high, processing unit is simple, easy to implement, there is no secondary pollution, environment amenable advantage simultaneously, for high-level efficiency, low energy, low-cost desalting technology provide new approach.
Principle based on CDI can find out, the key that obtains high CDI performance is electrode materials, requires electrode materials to have the characteristics such as specific surface area is large, space is flourishing, good conductivity.Porous carbon materials has that high specific surface area, good conductive capability, unique chemical stability, good formability, relative low price, raw material sources are abundant, production technique also the advantage such as comparative maturity application is very widely arranged aspect electrode materials.Up to now, the porous carbon materials as the CDI electrode mainly comprises gac, charcoal-aero gel, carbon nanofiber, carbon nanotube, Graphene and mesoporous carbon.Wherein gac is because specific surface area is large, simple, the cheap electrode materials that becomes present widespread use of preparation, but its desalting efficiency is lower, is mainly that existence due to a large amount of micropores is unfavorable for that the infiltration of ion and absorption cause lower, the unordered pore structure of specific surface area utilization ratio, and higher internal resistance.In order to address the above problem, the meso-porous carbon material that mesoporous carbon has high specific surface area, highly homogeneous pore size distribution, large pore volume and high mechanical stability has caused the great interest of investigator.The people such as Zou study ordered mesopore carbon (Zou L, Li LX, Song HH, the Morris G that finds to have high-specific surface area; Water Research, 2008,42,2340-2348) or through meso-porous carbon material (the Li LX of Ni finishing, Zou L, Song HH, Morris G, Carbon 2009,47,775-781) with respect to traditional activated carbon electrodes, all have higher desalination capacity.But it is to be noted the ratio capacitance of meso-porous carbon material when the desalination electrode of current preparation well below the theoretical value of carbon material, is mainly for example relatively high internal resistance and lower surface-area utilization ratios of some shortcomings of existing due to material.Therefore in order to address the above problem, prepare novel more high surface area, high conductivity, the space prosperity, the more much higher level of surperficial utilization ratio hole (macropore, mesoporous and micropore) carbon electrode material, for the desalination of high-performance, high-level efficiency, less energy-consumption provides new way.
Summary of the invention
The objective of the invention is for the problems referred to above, provide a kind of electric double layer capacitance type desalination process of applying to carry out the preparation method of the multi-stage porous carbon structure capacitance desalination electrode of sea water desaltination processing.With macropore, the multi-stage porous carbon material of the mesoporous and effective combination of micropore, can select the advantage of comprehensive various holes material,, due to its huge specific surface area, flourishing pore texture, the pore passage structure that is interconnected, make it at aspects such as diffusion, mass transfers, show and be better than single pore structure properties of materials simultaneously.The macropore that wherein is interconnected and the mesoporous hole of iontophoretic injection to depths that be conducive to, the effective rate of utilization of raising specific surface; Shorter ion the evolving path has also reduced the internal resistance of electrode materials simultaneously.Simultaneous micropore and mesoporously give desalination electrode higher specific surface area, be conducive to obtain higher CDI performance in addition.Macropore, mesoporous and micropore, effectively in conjunction with a kind of multi-stage porous carbon structure capacitance desalination electrode of preparation, had higher specific surface area, good electroconductibility and better desalting performance.
The objective of the invention is to reach by following technique means and measure.
The invention provides a kind of preparation method of multi-stage porous carbon structure capacitance desalination electrode, it is characterized in that following preparation process and step:
(1) preparation of electrode materials:
With monodisperse silica (SiO
2) the microballoon ultra-sonic dispersion is in a certain amount of ethanolic soln, 15 ~ 35
oThe C natural sediment, then high temperature sintering, obtain SiO
2Template; Be 20 wt% sodium hydroxide solutions to adding concentration in phenol, the rear concentration that slowly adds that stirs is 37 wt% formaldehyde solutions, is warming up to 65 ~ 75
oC reacts 1 ~ 2.5 h, is cooled to after room temperature with 0.6 M salt acid for adjusting pH to neutral, and the cryogenic vacuum underpressure distillation reduces water-content, then adds ethanol to stir and centrifugally after 10-12 h removes inorganic salt to obtain concentration be 20 wt% novolak resin precursor liquid solutions; The ethanolic soln of structure directing agent (concentration is 4.76 wt%) and novolak resin precursor liquid solution are uniformly mixed.Then SiO
2Template is impregnated in mixing solutions, and after the low temperature volatiling reaction, suction filtration is removed excessive solution, further low temperature volatilization hot setting, and then adding concentration in inert atmosphere after carbonization is that 10 wt% hydrofluoric acid solution stirring reactions are removed SiO
2Template, can obtain the multi-stage porous carbon material after fully washing drying; The preparation of multi-stage porous carbon structure capacitance desalination electrode:
With the multi-stage porous carbon material of step (1) preparation, acetylene black and ptfe emulsion are to be applied on the conductive substrates graphite paper after 80:10:10 ~ 90:5:5 is uniformly mixed according to mass ratio, subsequently 100 ~ 120
oThe C oven dry of spending the night; Finally make the multi-stage porous carbon structure capacitance desalination electrode.
Above-mentioned single SiO that disperses
2The diameter of microballoon is 100 ~ 400 nm; Above-mentioned SiO
2In the alcohol dispersion liquid of microballoon, the solid content of microballoon is 1% ~ 10%.The silicon dioxide microsphere dispersion liquid of certain grain size and density can form quality formwork structure preferably; When undersized or density was too low, sedimentation velocity was excessively slow, and dispersion liquid can exist with the dispersion system of balance, can cause very difficult formation template or formation time long; When oversize the or dispersion liquid density of microballoon was too high, sedimentation velocity was too fast, and the colloid micro ball that concentrates on container bottom has little time to experience changing and causing the template quality that obtains poor mutually from disorder to order.
Above-mentioned structure directing agent is F127(PEO
106-PPO
70-PEO
106), P123(PEO
20-PPO
70-PEO
20) or both mixing.In addition, the mol ratio of phenol, formaldehyde, sodium hydroxide and structure directing agent is 1:2:0.1:0.005 ~ 0.025.The water-wet side at triblock copolymer PEO-PPO-PEO two ends and novolak resin precursor body have stronger hydrogen bond action, have guaranteed good dispersiveness, for further polymerization pyrolytic reaction provides possibility; Secondly the PEO-PPO-PEO template has a large amount of Sauerstoffatoms and lower decomposition temperature, be easy to remove, and be the good template for preparing porous carbon materials.
SiO after above-mentioned presoma dipping
2Template need to be through low temperature volatilization hot setting two-step reaction, and wherein the temperature of low temperature volatilization is 30 ~ 60
oC； The temperature of hot setting is 100 ~ 140
oC。Low temperature volatilization, hot setting make resol further volatilize after polymerization and form the macromolecular scaffold with rigidity.The too low resol polycondensation of temperature is slower, is unfavorable for being completed into the macromolecular scaffold of rigidity.Owing to solidifying under aerobic conditions, during excess Temperature, resol oxidation blackout.
Above-mentioned carbonization process need to be by sectional temperature-controlled calcining realization in inert atmosphere, and controlling temperature rise rate is 1
oC/min, at first be warming up to 300 ~ 500
oC, insulation 1-4 hour, then be warming up to 500 ~ 1100 at this temperature
oC, insulation 1-6 hour at this temperature.Inert protective gas comprises nitrogen and argon gas, and gas flow rate is 80-140 mL/min.Carbonization process carries out under protection of inert gas, be conducive to keep the carbon skeleton structure, if, containing roasting under oxygen condition, can cause caving in of carbon skeleton.Carbonization process divides two sections to carry out roasting in addition, is degradable because in low temperature insulation for some time, be conducive to triblock copolymer; High temperature cabonization forms the stable carbon skeleton structure with certain degree of graphitization subsequently.
The novel porous carbon structure capacitance desalination electrode with hierarchy of the inventive method preparation has higher specific surface area, good electroconductibility and better simple, the easy handling of desalting performance, preparation process.Have potential application prospect aspect structure capacitance desalination.
Embodiment
After now specific embodiments of the invention being described in.
Embodiment 1
Be the monodisperse silica microspheres ultra-sonic dispersion (massfraction is 1 wt%) in ethanolic soln of 150 nm with diameter, then 20
oC deposits 1-2 week rear 600
oC sintering 1.5 h, make SiO
2Template.Be 20 wt% sodium hydroxide solutions to adding 0.13 g concentration in the phenol of 0.61 g melting, the rear 1.05 g concentration that slowly add that stir are 37 wt % formaldehyde solutions, are warming up to 65
oC reacts 2 h, is cooled to after room temperature and regulates PH to neutral with 0.6 M hydrochloric acid, and the cryogenic vacuum decompression dehydration, to sticky, then adds ethanolic soln to stir 10 h, finally centrifugally removes inorganic salt to obtain concentration be 20 wt% novolak resin precursor liquid solutions.With 1 g F127(PEO
106PPO
70PEO
106) join in 20 g ethanol after stirring and dissolving, add precursor solution to be uniformly mixed.Wherein the mol ratio of phenol, formaldehyde, sodium hydroxide and structure directing agent is 1:2:0.1:0.012.Then with 0.5 g SiO
2Template adds in above-mentioned mixing solutions, and 30
oIt is sticky that C evaporates into solution, and suction filtration is removed excessive solution further rear further 30
oC volatilization self-assembly 8 h, 100
oC solidifies 24 h and is placed in tube furnace, is under the nitrogen protection of 100 mL/min at gas flow rate, and controlling temperature rise rate is 1
oC/min, at first be warming up to 350
oC, 350
oC is incubated 2h, then is warming up to 800
oC, 800
oC is incubated 4 h.To be cooled is that 10 wt% hydrofluoric acid solution stirred overnight are removed SiO to adding concentration after room temperature
2Template, namely obtain the multi-stage porous carbon material after fully washing drying.With the multi-stage porous carbon material of gained, acetylene black and ptfe emulsion are to be applied on graphite paper after 80:10:10 mixes according to mass ratio, subsequently 100
oC ~ 120
oThe C oven dry of spending the night.Finally make the multi-stage porous carbon desalination electrode.
Test the ratio electric capacity of above-mentioned multi-stage porous carbon desalination electrode.Use CHI 660D type electrochemistry electrochemical workstation, ionogen is 1 M sodium chloride solution, and scanning speed is 10 mV/s, and voltage range is-0.5 V ~ 0.5 V; Record the ratio electric capacity of this electrode its desalting performance of electrode test greater than the 120 above-mentioned preparations of F/g., in the salt solution of 600 ppm, its desalting efficiency is greater than 90%.
Embodiment 2
Be the monodisperse silica microspheres ultra-sonic dispersion (massfraction is 3 wt%) in ethanolic soln of 250 nm with diameter, then 25
oC deposits 1-2 week rear 600
oC sintering 1.5 h, make SiO
2Template.Be 20 wt% sodium hydroxide solutions to adding 0.26 g concentration in the phenol of 1.22 g meltings, the rear 2.1 g concentration that slowly add that stir are 37 wt % formaldehyde solutions, are warming up to 70
oC reacts 1.5 h, is cooled to after room temperature and regulates PH to neutral with 0.6 M hydrochloric acid, and the cryogenic vacuum decompression dehydration, to sticky, then adds ethanol to stir 12 h, finally centrifugally removes inorganic salt to obtain concentration be 20 wt% novolak resin precursor liquid solutions.With 1.5 g P123(PEO
20-PPO
70-PEO
20) join in 30 g ethanol after stirring and dissolving, add precursor solution to be uniformly mixed.Wherein the mol ratio of phenol, formaldehyde, sodium hydroxide and structure directing agent is 1:2:0.1:0.02.Then with 2 g SiO
2Template adds in above-mentioned mixing solutions, and 45
oIt is sticky that C evaporates into solution, and suction filtration removes after excessive solution further 45
oC volatilization self-assembly 5 h, 120
oC solidifies 20 h and is placed in tube furnace, is under the nitrogen protection of 80 mL/min at gas flow rate, and controlling temperature rise rate is 1
oC/min, at first be warming up to 400
oC, 400
oC is incubated 2 .5h, then is warming up to 600
oC, 600
oC is incubated 4 h.To be cooled is that 10 wt% hydrofluoric acid solution stirred overnight are removed SiO to adding concentration after room temperature
2Template, namely obtain the multi-stage porous carbon material after fully washing drying.With the multi-stage porous carbon material of gained, acetylene black and ptfe emulsion are to be applied on graphite paper after 85:10:5 mixes according to mass ratio, subsequently 100
oC ~ 120
oThe C oven dry of spending the night.Finally make the multi-stage porous carbon desalination electrode.
Test the ratio electric capacity of above-mentioned multi-stage porous carbon desalination electrode.Use CHI 660D type electrochemistry electrochemical workstation, ionogen is 1 M sodium chloride solution, and scanning speed is 10 mV/s, and voltage range is-0.5V ~ 0.5V; Record the ratio electric capacity of this electrode its desalting performance of electrode test greater than the 95 above-mentioned preparations of F/g., in the salt solution of 800 ppm, its desalting efficiency is greater than 85%.
Embodiment 3
Be the monodisperse silica microspheres ultra-sonic dispersion (massfraction is 6 wt%) in ethanolic soln of 400 nm with diameter, then 28
oC deposits 1-2 week rear 600
oC sintering 1.5 h, make SiO
2Template.Be 20 wt% sodium hydroxide solutions to adding 0.13 g concentration in the phenol of 0.61 g melting, the rear 1.05 g concentration that slowly add that stir are 37 wt % formaldehyde solutions, are warming up to 75
oC reacts 1.5 h, is cooled to after room temperature and regulates PH to neutral with 0.6 M hydrochloric acid, and the cryogenic vacuum decompression dehydration, to sticky, then adds ethanol to stir 10 h, finally centrifugally removes inorganic salt to obtain concentration be 20 wt% novolak resin precursor liquid solutions.With 0.5 g F127(PEO
106PPO
70PEO
106) and 0.5 g P123(PEO
20-PPO
70-PEO
20) join in 20 g ethanol after stirring and dissolving, add precursor solution to be uniformly mixed.Wherein the mol ratio of phenol, formaldehyde, sodium hydroxide and structure directing agent is 1:2:0.1:0.017.Then with 4 g SiO
2Template adds in above-mentioned mixing solutions, and 55
oIt is sticky that C evaporates into solution, and suction filtration removes after excessive solution further 55
oC volatilization self-assembly 5 h, 100
oC solidifies 24 h and is placed in tube furnace, is under the nitrogen protection of 130 mL/min at gas flow rate, and controlling temperature rise rate is 1
oC/min, at first be warming up to 500
oC, 500
oC is incubated 3 h, then is warming up to 1000
oC, 1000
oC is incubated 2 h.To be cooled is that 10 wt% hydrofluoric acid solution stirred overnight are removed SiO to adding concentration after room temperature
2Template, namely obtain the multi-stage porous carbon material after fully washing drying.With the multi-stage porous carbon material of gained, acetylene black and ptfe emulsion are to be applied on graphite paper after 90:5:5 mixes according to mass ratio, subsequently 100
oC ~ 120
oThe C oven dry of spending the night.Finally make the multi-stage porous carbon desalination electrode.
Test the ratio electric capacity of above-mentioned multi-stage porous carbon desalination electrode.Use CHI 660D type electrochemistry electrochemical workstation, ionogen is 1 M sodium chloride solution, and scanning speed is 10 mV/s, and voltage range is-0.5 V ~ 0.5 V; Record the ratio electric capacity of this electrode its desalting performance of electrode test greater than the 80 above-mentioned preparations of F/g., in the salt solution of 300 ppm, its desalting efficiency is greater than 80%.
Claims (7)
1. the preparation method of multi-stage porous carbon structure capacitance desalination electrode is characterized in that comprising the following steps:
(1) preparation of electrode materials: with monodisperse silica (SiO
2) the microballoon ultra-sonic dispersion is in a certain amount of ethanolic soln, 15 ~ 35
oThe C natural sediment, then high temperature sintering, obtain SiO
2Template; Be 20 wt% sodium hydroxide solutions to adding concentration in phenol, the rear concentration that slowly adds that stirs is 37 wt% formaldehyde solutions, is warming up to 65 ~ 75
oC reacts 1 ~ 2.5 h, is cooled to after room temperature with 0.6 M salt acid for adjusting pH to neutral, and the cryogenic vacuum underpressure distillation reduces water-content, then adds ethanol to stir and centrifugally after 10-12 h removes inorganic salt to obtain concentration be 20 wt% novolak resin precursor liquid solutions; The ethanolic soln and the novolak resin precursor liquid solution that are 4.76 wt% structure directing agents with concentration are uniformly mixed; Then SiO
2Template is impregnated in mixing solutions, and after the low temperature volatiling reaction, suction filtration is removed excessive solution, further low temperature volatilization hot setting, and then adding concentration in inert atmosphere after carbonization is that 10 wt% hydrofluoric acid solution stirring reactions are removed SiO
2Template, can obtain the multi-stage porous carbon material after fully washing drying;
(2) preparation of structure capacitance desalination electrode: with the multi-stage porous carbon material of step (1) preparation, acetylene black and ptfe emulsion are to be applied on the conductive substrates graphite paper after 80:10:10 ~ 90:5:5 is uniformly mixed according to mass ratio, subsequently 100 ~ 120
oThe C oven dry of spending the night; Finally make the multi-stage porous carbon structure capacitance desalination electrode.
2. the preparation method of multi-stage porous carbon structure capacitance desalination electrode according to claim 1, is characterized in that described single SiO of dispersion
2The diameter of microballoon is 100 ~ 400 nm.
3. the preparation method of multi-stage porous carbon structure capacitance desalination electrode according to claim 1, is characterized in that described SiO
2In the ethanolic soln of microballoon, the massfraction of microballoon is 1 ~ 10%.
4. the preparation method of multi-stage porous carbon structure capacitance desalination electrode according to claim 1, is characterized in that described structure directing agent comprises F127(PEO
106-PPO
70-PEO
106) and P123(PEO
20-PPO
70-PEO
20) in a kind of or both mixing.
5. the preparation method of multi-stage porous carbon structure capacitance desalination electrode according to claim 1, is characterized in that in described preparation process, and the mol ratio of phenol, formaldehyde, sodium hydroxide and structure directing agent is 1:2:0.1:0.005 ~ 0.025.
6. the preparation method of multi-stage porous carbon structure capacitance desalination electrode according to claim 1, is characterized in that the SiO that described presoma floods
2Template need to be through low temperature volatilization and hot setting two-step reaction, and wherein the temperature of low temperature volatilization is 30 ~ 60
oC； The temperature of hot setting is 100 ~ 140
oC。
7. the preparation method of multi-stage porous carbon structure capacitance desalination electrode according to claim 1, is characterized in that the carbonization process in described inert atmosphere need to be realized by sectional temperature-controlled calcining, and controlling temperature rise rate is 1
oC/min, at first be warming up to 300 ~ 500
oC, insulation 1-4 h, then be warming up to 500 ~ 1100 at this temperature
oC, insulation 1-6 h at this temperature; Inert protective gas comprises nitrogen and argon gas, and gas flow rate is 80-140 mL/min.
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| CN104591120A (en) * | 2013-10-31 | 2015-05-06 | 无锡华臻新能源科技有限公司 | Preparation of rough-surface microspherical manganese dioxide and application to supercapacitors |
| WO2015165762A1 (en) * | 2014-04-30 | 2015-11-05 | Basf Se | Process for producing a monolithic body of a porous carbon material, monolithic bodies of special porous carbon materials and their use |
| CN105731609B (en) * | 2014-12-10 | 2018-03-30 | 吉林师范大学 | A kind of porous carbon electrodes based on metal-organic framework materials and preparation method thereof |
| CN105688897A (en) * | 2015-12-31 | 2016-06-22 | 北京化工大学 | Porous carbon net array Ag loaded catalyst with high catalytic activity and preparation method |
| CN111224189A (en) * | 2020-01-16 | 2020-06-02 | 东莞理工学院 | Activated carbon microsphere electrode material based on waste lithium ion battery negative electrode material and preparation and application thereof |
| CN112357905B (en) * | 2020-10-12 | 2022-07-12 | 广东药科大学 | Nitrogen-doped mesoporous carbon nanosphere material as well as preparation method and application thereof |
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