CN109280540A - It is a kind of using graphene aerogel as energy storage material of matrix and preparation method thereof - Google Patents
It is a kind of using graphene aerogel as energy storage material of matrix and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of using graphene aerogel as the energy storage material of matrix and preparation method, belongs to new energy materials field.The present invention introduces rich hydroxyl chain polyvinyl alcohol and links graphene sheet layer, be conducive to the opening and transmission of passage of heat using graphene oxide as raw material；Spontaneous assembling between the graphene oxide and pyrrole monomer that handle through polyvinyl alcohol is improved energy storage efficiency by the present invention；The present invention is occurred graft reaction, increases the long-acting performance of energy storage by vacuum condition of ice bath from stream injection technology, amino and graphene aerogel oxygen-containing group is prolonged；The present invention obtains the energy storage activating agent of azobenzene using 5- amino isophthalic acid as raw material, and azobenzene molecule can be used for the long-term storage of solar energy highly effective；The present invention increases energy storage capacity finally using graphene aerogel as template.The present invention solves the problem of graphene aerogel materials'use crosslinking agent can make the structural unit of graphene oxide change, influence energy-storage property.
Description
Technical field
The invention belongs to new energy materials fields, and in particular to it is a kind of using graphene aerogel as the energy storage material of matrix and
Preparation method.
Background technique
Graphene is both most thin material, and most tough material, and breaking strength is 200 times higher than steel.While it
There is good elasticity again, stretch range can reach the 20% of own dimensions.Graphene most potential application at present is as silicon
Substitute manufactures ultra micro transistor npn npn, for producing following supercomputer.Replace silicon, computer processor with graphene
The speed of service will improve hundreds times.
Graphene is the new carbon with bi-dimensional cellular shape structure, has very high mechanical strength, and elasticity is thermally conductive
Property, electric conductivity and quantum hall effect etc. attract wide attention in recent years.Graphene enhances as a kind of nanoparticle
Epoxy resin composite material has been research hotspot, but graphene nano particle bad dispersibility, easily group in epoxy resin-base
It is poly-, cause the performance of composite material after resin modified not rise anti-drop in some aspects.
Aeroge is a kind of solid matter form, the smallest solid of world's upper density.Density can reach 3kg/m3.It is general normal
The aeroge seen is that silica aerogel was made in 1931.There are many type of aeroge, there is silicon systems, carbon system, sulphur system, metal oxide
System, metal system etc..Any substance aeroge can keep its shape invariance after drying and removing internal solvent substantially, and produce
Object has high porosity, low-density.
Aeroge includes a large amount of hole, and hole ratio is a kind of porous material with nanostructure 80% or more,
The aspects such as mechanics, acoustics, calorifics, optics show its peculiar property.They differ markedly from hole configurations in micron and milli
The porous material of rice magnitude, very thin nanostructure make the thermal conductivity of material extremely low, have great specific surface area airsetting
Glue is more much smaller than traditional porous material to the scattering of light, sound, these unique properties not only make the material in base
It is intriguing in plinth research, and contain broad application prospect in many fields.
Currently, sol-gel method preparation is usually used in aeroge, i.e., it is made wet solidifying first with the crosslinking feature of crosslinking agent
Glue (i.e. hydrogel), then by being dried to obtain.For graphene aerogel, some reports are using graphene oxide and hand over
Join agent mixing, so that the two is crosslinked reaction and obtain graphene oxide colloidal sol (i.e. hydrogel), is then obtained by dry, reduction
Graphene aerogel.But in this method, graphene oxide is crosslinked with crosslinking agent when reacting, the structure of graphene oxide
Unit is changed, and causes the script structure of graphene in graphene aerogel generated to change, to make graphite
The original conduction of alkene, mechanics, energy-storage property are affected.
Summary of the invention
The technical problems to be solved by the invention: can make to aoxidize stone for current graphene aerogel materials'use crosslinking agent
The problem of structural unit of black alkene changes, influences energy-storage property provides a kind of using graphene aerogel as the energy storage of matrix
Material and preparation method thereof.
In order to solve the above technical problems, the present invention is using technical solution as described below:
It is a kind of using graphene aerogel as the energy storage material of matrix, including graphene aerogel matrix object, energy storage activating agent；
The preparation method of the graphene aerogel matrix object, includes the following steps:
(1) it takes graphene oxide 1 ~ 3:30 in mass ratio ~ 50 to be added in deionized water, adds 6 ~ 9 times of graphene oxide quality
Polyvinyl alcohol, in 140 ~ 150 DEG C keep the temperature, be cooled to room temperature, cooled material taken to wash through deionized water, obtain washings, be passed through argon
Gas shielded takes washings to keep the temperature, and is cooled to room temperature, and obtains cooled material a；
(2) take cooled material a 1 ~ 3:10 in mass ratio ~ 20 that deionized water is added, ultrasonic disperse adds cooled material a mass 2 ~ 5%
Pyrroles, ultrasound stands 3 ~ 5 days in 25 ~ 30 DEG C, obtains standing object, takes and stands object 1 ~ 4:30 in mass ratio ~ 40 anhydrous second is added
Alcohol is stood, and dehydrated alcohol is removed in filtering, is repeated that dehydrated alcohol is added, is stood process 5 ~ 8 times, filtering takes final filtration cakes torrefaction, obtains
Dried object；
(3) it takes dimethyl silicone polymer 1 ~ 3:10 in mass ratio ~ 20 that n-hexane is added, is stirred, must mix in 25 ~ 30 DEG C
Liquid takes dried object 1 ~ 3:80 in mass ratio ~ 100 that mixed liquid dipping is added, and is prolonged stream injection naturally, and filtering is taken out and done after impregnating
Dry object is kept the temperature in 50 ~ 55 DEG C, is cooled to room temperature to get graphene aerogel matrix object.
The heat-retaining condition of washings in the step (1) are as follows: be warming up to 750 ~ 800 DEG C of 2 ~ 4h of heat preservation.
Naturally prolong the condition of stream injection in the step (3) are as follows: keep 4 ~ 6h in 2 ~ 4 DEG C, vacuum condition.
The energy storage activating agent the preparation method comprises the following steps:
S1. it takes 5- amino isophthalic acid 2 ~ 4:1 in mass ratio ~ 3:10 ~ 20 that sodium hydroxide, deionized water is added, is stirred in 2 ~ 4 DEG C
Mixing is mixed, the sodium nitrite of 5- amino isophthalic acid quality 40 ~ 60% is added, is stirred, obtains mixture, take mixture
1 ~ 4:5 ~ 9 are added dropwise in hydrochloric acid in mass ratio, are controlled 30 ~ 50min of time for adding, are stirred, obtain stirring mixture；
S2. it takes 3,5- dimethoxyaniline, 1 ~ 5:20 in mass ratio ~ 30 to be added in hydrochloric acid, is stirred, adds in 2 ~ 5 DEG C
The stirring mixture of 3,5- 1 ~ 3 times of dimethoxyaniline quality adjusts pH to 6 ~ 7, is passed through argon gas protection, keeps the temperature in 2 ~ 5 DEG C,
It filters, takes and filter slag through distillation water washing, vacuum drying obtains energy storage activating agent.
That mixture is stirred in the step S1 is stirred condition are as follows: is stirred 1 ~ 3h in -2 ~ 3 DEG C.
It is described using graphene aerogel as the preparation method of the energy storage material of matrix, include the following steps:
Take energy storage activating agent 1 ~ 5:0.2 in mass ratio ~ 0.5:50 ~ 60 that sodium nitrite, deionized water is added, it is stirred 20 ~
30min obtains mixture a, and the hydrochloric acid for adding deionized water quality 30 ~ 40% is stirred, and obtains mixed liquor, takes mixed liquor by matter
Graphene aerogel matrix object, deionized water is added than 40 ~ 50:1 ~ 4:80 ~ 100 in amount, in -4 ~ 1 DEG C of 2 ~ 5h of heat preservation, then at 25 ~
30 DEG C are stirred, and filtering takes filter cake through deionized water, acetone washing, rotary evaporation is to get using graphene aerogel as matrix
Energy storage material.
The mixed liquor is stirred condition are as follows: is stirred 1 ~ 3h in 2 ~ 5 DEG C.
The present invention is compared with other methods, and advantageous effects are:
(1) for the present invention using graphene oxide as raw material, addition polyvinyl alcohol is additive, during the three-dimensional assembling of graphene
It introduces rich hydroxyl chain polyvinyl alcohol and links graphene sheet layer, effectively reduce the π-π overlapping of piece interlayer, obtaining has uniqueness
The bigger serface three-dimension layer secondary aperture carbon of pore system, it is logical that the three-dimensional porous system of the graphene being mutually communicated provides smooth mass transfer
Road and excellent electron-transport network, as the base structure of graphene aerogel, be conducive to passage of heat opening and
Transmission；
(2) present invention is by the spontaneous assembling between the graphene oxide and pyrrole monomer that handle through polyvinyl alcohol, without adding it
His Oxidizing and Reducing Agents prepares composite hydrogel at room temperature, also based on the oxidation between graphene oxide and pyrrole monomer
Original reaction, pyrroles play the role of crosslinking agent, and surface contains weak electropositive pyrroles's phase in electronegative graphene oxide and surface
Mutually attract, is self-assembly of gel through reduction, while pyridine monomer is oxidized graphene oxidation polymerization and forms polypyridine, aoxidizes stone
Conjugation between black alkene lamella makes its gelation, in the case where not changing graphene oxide structural unit, to graphene
It carries out being cross-linked to form gel, is conducive to good thermally conductive, energy-storage property the preservation that graphene this body structure has, improve energy storage
Efficiency；
(3) dimethyl silicone polymer is introduced graphene aerogel by vacuum condition of ice bath from stream injection technology is prolonged by the present invention,
Graft reaction occurs for the amino and graphene aerogel oxygen-containing group of dimethyl silicone polymer, is formed and orderly stablizes π-π connection, protects
It demonstrate,proves three-dimensional grapheme aeroge network skeleton completely to stablize with microcosmic combination interface, so that graphene aerogel internal sheets layer unit
It further regularization and is completely embedded, the complete long-acting holding maintained conducive to capable transport channel of structural framework increases
The long-acting performance of energy storage；
(4) present invention carries out diazo-reaction under the action of sodium nitrite, adds using 5- amino isophthalic acid as raw material
3,5- dimethoxyanilines carry out coupling reaction, obtain the energy storage activating agent of azobenzene, even containing electrophilic carboxyl
Pyridine molecule has different absorption characteristics in cis and trans configuration, its generation can be excited trans- to π * by π by ultraviolet light
Become cis-, and visible light by n to π * excite its it is cis- become trans-, pushed away simultaneous with the azobenzene derivatives molecule of carboxyl
It draws electronic structure and faces a methoxyl group and contraposition/meta position carboxyl functional group's effect, there is biggish isomerisation degree
With longer reply half-life period, is conducive to improve it to the absorption intensity and efficiency of solar energy and keeps good storage steady simultaneously
It is qualitative, it can be used for the long-term storage of solar energy highly effective；
(5) present invention orderly carries energy storage activating agent, improves the energy of azobenzene molecule finally using graphene aerogel as template
Metric density and half-life period, using diazonium salt radical reaction, by azobenzene molecule covalence graft to redox graphene surface,
The optical Response of energy storage is improved, energy storage capacity is increased.
Specific embodiment
Graphene aerogel matrix object the preparation method comprises the following steps:
(1) it takes graphene oxide 1 ~ 3:30 in mass ratio ~ 50 to be added in deionized water, adds 6 ~ 9 times of graphene oxide quality
Polyvinyl alcohol be cooled to room temperature in 140 ~ 150 DEG C of 4 ~ 6h of heat preservation, cooled material taken to wash through deionized water, obtain washings, lead to
Enter argon gas protection, takes washings to be warming up to 750 ~ 800 DEG C of 2 ~ 4h of heat preservation, be cooled to room temperature, obtain cooled material a；
(2) take cooled material a 1 ~ 3:10 in mass ratio ~ 20 that deionized water is added, 30 ~ 40min of ultrasonic disperse adds cooled material a
The pyrroles of quality 2 ~ 5%, 5 ~ 10min of ultrasound stand 3 ~ 5 days in 25 ~ 30 DEG C, obtain standing object, take and stand object 1 ~ 4:30 in mass ratio
~ 40 are added dehydrated alcohol, stand 5 ~ 7h, and dehydrated alcohol is removed in filtering, repeat that dehydrated alcohol is added, stand process 5 ~ 8 times, filtering,
Final filtration cakes torrefaction is taken, dried object is obtained；
(3) it takes dimethyl silicone polymer 1 ~ 3:10 in mass ratio ~ 20 that n-hexane is added, is stirred 30 ~ 40min in 25 ~ 30 DEG C,
Mixed liquor is obtained, takes dried object 1 ~ 3:80 in mass ratio ~ 100 that mixed liquid dipping is added, is prolonged naturally under 2 ~ 4 DEG C, vacuum condition
Stream keeps 4 ~ 6h, and filtering is taken out dried object after impregnating and is cooled to room temperature in 50 ~ 55 DEG C of 10 ~ 12h of heat preservation to get graphene airsetting
Matrix body object.
Energy storage activating agent the preparation method comprises the following steps:
S1. it takes 5- amino isophthalic acid 2 ~ 4:1 in mass ratio ~ 3:10 ~ 20 that sodium hydroxide, deionized water is added, is stirred in 2 ~ 4 DEG C
30 ~ 50min of mixing is mixed, the sodium nitrite of 5- amino isophthalic acid quality 40 ~ 60% is added, is stirred 50 ~ 60min, obtains
Mixture, taking mixture 1 ~ 4:5 ~ 9 to be in mass ratio added dropwise to concentration is to control 30 ~ 50min of time for adding in 1mol/L hydrochloric acid,
It is stirred 1 ~ 3h in -2 ~ 3 DEG C, obtains stirring mixture；
S2. taking 3,5- dimethoxyaniline, 1 ~ 5:20 in mass ratio ~ 30 that concentration is added is to stir in 1mol/L hydrochloric acid in 2 ~ 5 DEG C
30 ~ 40min is mixed, the stirring mixture of 1 ~ 3 times of 3,5- dimethoxyaniline quality is added, pH to 6 ~ 7 is adjusted, is passed through argon
Gas shielded is filtered in 2 ~ 5 DEG C of 1 ~ 3h of heat preservation, is taken and is filtered slag through distillation water washing, vacuum drying obtains energy storage activating agent.
It is a kind of using graphene aerogel as the preparation method of the energy storage material of matrix, include the following steps:
Take energy storage activating agent 1 ~ 5:0.2 in mass ratio ~ 0.5:50 ~ 60 that sodium nitrite, deionized water is added, it is stirred 20 ~
30min obtains mixture a, and the concentration for adding deionized water quality 30 ~ 40% is 1mol/L hydrochloric acid, it is stirred 1 in 2 ~ 5 DEG C ~
3h obtains mixed liquor, takes mixed liquor 40 ~ 50:1 in mass ratio ~ 4:80 ~ 100 that graphene aerogel matrix object, deionized water is added,
In -4 ~ 1 DEG C of 2 ~ 5h of heat preservation, it is stirred 12 ~ 18h then at 25 ~ 30 DEG C, is filtered, takes filter cake through deionized water, acetone washing, rotation
Turn evaporation to get using graphene aerogel as the energy storage material of matrix.
Embodiment 1
Graphene aerogel matrix object the preparation method comprises the following steps:
(1) it takes graphene oxide 1:30 to be in mass ratio added in deionized water, adds 6 times of graphene oxide quality of polyethylene
Alcohol is cooled to room temperature in 140 DEG C of heat preservation 4h, cooled material is taken to wash through deionized water, obtain washings, is passed through argon gas protection, takes and wash
It washs object and is warming up to 750 DEG C of heat preservation 2h, be cooled to room temperature, obtain cooled material a；
(2) take cooled material a 1:10 in mass ratio that deionized water is added, ultrasonic disperse 30min adds cooled material a mass 2%
Pyrroles, ultrasonic 5min stand 3 days in 25 DEG C, obtain standing object, take and stand object 1:30 in mass ratio addition dehydrated alcohol, stand 5h,
Dehydrated alcohol is removed in filtering, repeats that dehydrated alcohol is added, stands process 5 times, filtering takes final filtration cakes torrefaction, obtains dried object；
(3) it takes dimethyl silicone polymer 1:10 in mass ratio that n-hexane is added, is stirred 30min in 25 DEG C, obtains mixed liquor, take
Mixed liquid dipping is added in dried object 1:80 in mass ratio, is prolonged stream naturally under 2 DEG C, vacuum condition and keeps 4h, leaching is taken out in filtering
Dried object is cooled to room temperature in 50 DEG C of heat preservation 10h to get graphene aerogel matrix object after bubble.
Energy storage activating agent the preparation method comprises the following steps:
S1. it takes 5- amino isophthalic acid 2:1:10 in mass ratio that sodium hydroxide, deionized water is added, is stirred in 2 DEG C
30min adds the sodium nitrite of 5- amino isophthalic acid quality 40%, is stirred 50min, obtains mixture, take mixture
It is to control time for adding 30min in 1mol/L hydrochloric acid, be stirred 1h in -2 ~ 3 DEG C, must stir that 1:5 in mass ratio, which is added dropwise to concentration,
Mix mixture；
S2. taking 3,5- dimethoxyaniline 1:20 in mass ratio that concentration is added is to be stirred in 1mol/L hydrochloric acid in 2 DEG C
30min adds the stirring mixture of 1 ~ 3 times of 3,5- dimethoxyaniline quality, adjusts pH to 6, argon gas protection is passed through, in 2
DEG C heat preservation 1h, filter, take filter slag through distill water washing, vacuum drying, obtain energy storage activating agent.
It is a kind of using graphene aerogel as the preparation method of the energy storage material of matrix, include the following steps:
It takes energy storage activating agent 1:0.2:50 in mass ratio that sodium nitrite, deionized water is added, is stirred 20min, obtains mixture
A, add deionized water quality 30% concentration be 1mol/L hydrochloric acid, be stirred 1h in 2 DEG C, obtain mixed liquor, take mixed liquor by
Mass ratio 40:1:80 is added graphene aerogel matrix object, deionized water and is stirred in -4 DEG C of heat preservation 2h then at 25 DEG C
12h, filtering, takes filter cake through deionized water, acetone washing, rotary evaporation is to get using graphene aerogel as the energy storage material of matrix
Material.
Embodiment 2
Graphene aerogel matrix object the preparation method comprises the following steps:
(1) it takes graphene oxide 2:40 to be in mass ratio added in deionized water, adds 7 times of graphene oxide quality of polyethylene
Alcohol is cooled to room temperature in 148 DEG C of heat preservation 5h, cooled material is taken to wash through deionized water, obtain washings, is passed through argon gas protection, takes and wash
It washs object and is warming up to 780 DEG C of heat preservation 3h, be cooled to room temperature, obtain cooled material a；
(2) take cooled material a 2:15 in mass ratio that deionized water is added, ultrasonic disperse 35min adds cooled material a mass 3%
Pyrroles, ultrasonic 8min stand 4 days in 28 DEG C, obtain standing object, take and stand object 3:35 in mass ratio addition dehydrated alcohol, stand 6h,
Dehydrated alcohol is removed in filtering, repeats that dehydrated alcohol is added, stands process 7 times, filtering takes final filtration cakes torrefaction, obtains dried object；
(3) it takes dimethyl silicone polymer 2:15 in mass ratio that n-hexane is added, is stirred 35min in 28 DEG C, obtains mixed liquor, take
Mixed liquid dipping is added in dried object 2:90 in mass ratio, is prolonged stream naturally under 3 DEG C, vacuum condition and keeps 5h, leaching is taken out in filtering
Dried object is cooled to room temperature in 54 DEG C of heat preservation 11h to get graphene aerogel matrix object after bubble.
Energy storage activating agent the preparation method comprises the following steps:
S1. it takes 5- amino isophthalic acid 3:2:15 in mass ratio that sodium hydroxide, deionized water is added, is stirred in 3 DEG C
40min adds the sodium nitrite of 5- amino isophthalic acid quality 50%, is stirred 55min, obtains mixture, take mixture
It is to control time for adding 40min in 1mol/L hydrochloric acid, be stirred 2h in 1 DEG C, must stir that 3:8 in mass ratio, which is added dropwise to concentration,
Mixture；
S2. taking 3,5- dimethoxyaniline 3:25 in mass ratio that concentration is added is to be stirred in 1mol/L hydrochloric acid in 4 DEG C
35min adds the stirring mixture of 2 times of 3,5- dimethoxyaniline quality, adjusts pH to 6.5, argon gas protection is passed through, in 4
DEG C heat preservation 2h, filter, take filter slag through distill water washing, vacuum drying, obtain energy storage activating agent.
It is a kind of using graphene aerogel as the preparation method of the energy storage material of matrix, include the following steps:
It takes energy storage activating agent 4:0.3:55 in mass ratio that sodium nitrite, deionized water is added, is stirred 25min, obtains mixture
A, add deionized water quality 35% concentration be 1mol/L hydrochloric acid, be stirred 2h in 4 DEG C, obtain mixed liquor, take mixed liquor by
Mass ratio 45:3:90 is added graphene aerogel matrix object, deionized water and is stirred in -1 DEG C of heat preservation 4h then at 28 DEG C
16h, filtering, takes filter cake through deionized water, acetone washing, rotary evaporation is to get using graphene aerogel as the energy storage material of matrix
Material.
Embodiment 3
Graphene aerogel matrix object the preparation method comprises the following steps:
(1) it takes graphene oxide 3:50 to be in mass ratio added in deionized water, adds 9 times of graphene oxide quality of polyethylene
Alcohol is cooled to room temperature in 150 DEG C of heat preservation 6h, cooled material is taken to wash through deionized water, obtain washings, is passed through argon gas protection, takes and wash
It washs object and is warming up to 800 DEG C of heat preservation 4h, be cooled to room temperature, obtain cooled material a；
(2) take cooled material a 3:20 in mass ratio that deionized water is added, ultrasonic disperse 40min adds cooled material a mass 5%
Pyrroles, ultrasonic 10min stand 5 days in 30 DEG C, obtain standing object, take and stand object 4:40 in mass ratio addition dehydrated alcohol, stand
Dehydrated alcohol is removed in 7h, filtering, repeats that dehydrated alcohol is added, stands process 8 times, filtering takes final filtration cakes torrefaction, obtains dried object；
(3) it takes dimethyl silicone polymer 3:20 in mass ratio that n-hexane is added, is stirred 40min in 30 DEG C, obtains mixed liquor, take
Mixed liquid dipping is added in dried object 3:100 in mass ratio, is prolonged stream naturally under 4 DEG C, vacuum condition and keeps 6h, filtered, taken out
Dried object is cooled to room temperature in 55 DEG C of heat preservation 12h to get graphene aerogel matrix object after immersion.
Energy storage activating agent the preparation method comprises the following steps:
S1. it takes 5- amino isophthalic acid 4:3:20 in mass ratio that sodium hydroxide, deionized water is added, is stirred in 4 DEG C
50min adds the sodium nitrite of 5- amino isophthalic acid quality 60%, is stirred 60min, obtains mixture, take mixture
It is to control time for adding 50min in 1mol/L hydrochloric acid, be stirred 3h in 3 DEG C, must stir that 4:9 in mass ratio, which is added dropwise to concentration,
Mixture；
S2. taking 3,5- dimethoxyaniline 5:30 in mass ratio that concentration is added is to be stirred in 1mol/L hydrochloric acid in 5 DEG C
40min adds the stirring mixture of 3 times of 3,5- dimethoxyaniline quality, adjusts pH to 7, argon gas protection is passed through, in 5 DEG C
3h is kept the temperature, is filtered, takes and filters slag through distillation water washing, vacuum drying obtains energy storage activating agent.
It is a kind of using graphene aerogel as the preparation method of the energy storage material of matrix, include the following steps:
It takes energy storage activating agent 5:0.5:60 in mass ratio that sodium nitrite, deionized water is added, is stirred 30min, obtains mixture
A, add deionized water quality 40% concentration be 1mol/L hydrochloric acid, be stirred 3h in 5 DEG C, obtain mixed liquor, take mixed liquor by
Mass ratio 50:4:100 is added graphene aerogel matrix object, deionized water and is stirred in 1 DEG C of heat preservation 5h then at 30 DEG C
18h, filtering, takes filter cake through deionized water, acetone washing, rotary evaporation is to get using graphene aerogel as the energy storage material of matrix
Material.
Comparative example 1: it is essentially identical with the preparation method of embodiment 3, it has only the difference is that lacking graphene aerogel matrix
Object.
Comparative example 2: it is essentially identical with the preparation method of embodiment 3, it has only the difference is that lacking energy storage activating agent.
Comparative example 3: the graphene aerogel of company of Wuhan City production is the energy storage material of matrix.
It is the energy storage material of matrix according to GB/T34336-017, GB/ by embodiment and comparative example gained graphene aerogel
T 22473-2008 standard is tested, and test result is as shown in table 1.
Table 1:
In summary, graphene aerogel of the invention is that the energy storage material of matrix is more preferable compared to commercial product effect, is worth
It widelys popularize.
Claims (7)
1. a kind of using graphene aerogel as the energy storage material of matrix, which is characterized in that including graphene aerogel matrix object, storage
It can activating agent；
The preparation method of the graphene aerogel matrix object, includes the following steps:
(1) it takes graphene oxide 1 ~ 3:30 in mass ratio ~ 50 to be added in deionized water, adds 6 ~ 9 times of graphene oxide quality
Polyvinyl alcohol, in 140 ~ 150 DEG C keep the temperature, be cooled to room temperature, cooled material taken to wash through deionized water, obtain washings, be passed through argon
Gas shielded takes washings to keep the temperature, and is cooled to room temperature, and obtains cooled material a；
(2) take cooled material a 1 ~ 3:10 in mass ratio ~ 20 that deionized water is added, ultrasonic disperse adds cooled material a mass 2 ~ 5%
Pyrroles, ultrasound stands 3 ~ 5 days in 25 ~ 30 DEG C, obtains standing object, takes and stands object 1 ~ 4:30 in mass ratio ~ 40 anhydrous second is added
Alcohol is stood, and dehydrated alcohol is removed in filtering, is repeated that dehydrated alcohol is added, is stood process 5 ~ 8 times, filtering takes final filtration cakes torrefaction, obtains
Dried object；
(3) it takes dimethyl silicone polymer 1 ~ 3:10 in mass ratio ~ 20 that n-hexane is added, is stirred, must mix in 25 ~ 30 DEG C
Liquid takes dried object 1 ~ 3:80 in mass ratio ~ 100 that mixed liquid dipping is added, and is prolonged stream injection naturally, and filtering is taken out and done after impregnating
Dry object is kept the temperature in 50 ~ 55 DEG C, is cooled to room temperature to get graphene aerogel matrix object.
2. according to claim 1 using graphene aerogel as the energy storage material of matrix, which is characterized in that the step
(1) heat-retaining condition of washings in are as follows: be warming up to 750 ~ 800 DEG C of 2 ~ 4h of heat preservation.
3. according to claim 1 using graphene aerogel as the energy storage material of matrix, which is characterized in that the step
(3) prolong the condition of stream injection in naturally are as follows: keep 4 ~ 6h in 2 ~ 4 DEG C, vacuum condition.
4. according to claim 1 using graphene aerogel as the energy storage material of matrix, which is characterized in that the energy storage is living
Property agent the preparation method comprises the following steps:
S1. it takes 5- amino isophthalic acid 2 ~ 4:1 in mass ratio ~ 3:10 ~ 20 that sodium hydroxide, deionized water is added, is stirred in 2 ~ 4 DEG C
Mixing is mixed, the sodium nitrite of 5- amino isophthalic acid quality 40 ~ 60% is added, is stirred, obtains mixture, take mixture
1 ~ 4:5 ~ 9 are added dropwise in hydrochloric acid in mass ratio, are controlled 30 ~ 50min of time for adding, are stirred, obtain stirring mixture；
S2. it takes 3,5- dimethoxyaniline, 1 ~ 5:20 in mass ratio ~ 30 to be added in hydrochloric acid, is stirred, adds in 2 ~ 5 DEG C
The stirring mixture of 3,5- 1 ~ 3 times of dimethoxyaniline quality adjusts pH to 6 ~ 7, is passed through argon gas protection, keeps the temperature in 2 ~ 5 DEG C,
It filters, takes and filter slag through distillation water washing, vacuum drying obtains energy storage activating agent.
5. according to claim 4 using graphene aerogel as the energy storage material of matrix, which is characterized in that the step S1
Middle stirring mixture is stirred condition are as follows: is stirred 1 ~ 3h in -2 ~ 3 DEG C.
6. it is a kind of as described in claim 1 ~ 5 any one using graphene aerogel as the preparation side of the energy storage material of matrix
Method, which is characterized in that the preparation method includes the following steps:
Take energy storage activating agent 1 ~ 5:0.2 in mass ratio ~ 0.5:50 ~ 60 that sodium nitrite, deionized water is added, it is stirred 20 ~
30min obtains mixture a, and the hydrochloric acid for adding deionized water quality 30 ~ 40% is stirred, and obtains mixed liquor, takes mixed liquor by matter
Graphene aerogel matrix object, deionized water is added than 40 ~ 50:1 ~ 4:80 ~ 100 in amount, in -4 ~ 1 DEG C of 2 ~ 5h of heat preservation, then at 25 ~
30 DEG C are stirred, and filtering takes filter cake through deionized water, acetone washing, rotary evaporation is to get using graphene aerogel as matrix
Energy storage material.
7. according to claim 6 using graphene aerogel as the preparation method of the energy storage material of matrix, which is characterized in that
The mixed liquor is stirred condition are as follows: is stirred 1 ~ 3h in 2 ~ 5 DEG C.
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