CN107226464B - The preparation method of graphene aerogel based on emulsion method - Google Patents
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Abstract
The present invention provides one kind using graphene Pickering lotion as soft template, and the preparation method of gel is assembled under hydrothermal condition.Pickering lotion of the present invention, is made of the following components: according to parts by weight, 0.3~1 part of graphite oxide, 0~1.84 portion of salt, 0.00365~0.63 part of acid, 0.9~5 part of ascorbic acid, the vegetable oil of 100 parts of water and 0.2~1 times of water volume.Preparation method of the present invention is not necessarily to complex operations condition and strong corrosive material, and accurate porosity control may be implemented, may be implemented to prepare on a large scale；Graphene aerogel prepared by the present invention has good horizontal and vertical extruding resilience performance simultaneously, and cellular structure remains on pass, has superior adsorption capacity to petroleum-type product, has broad application prospects.
Description
Technical field
The invention belongs to Material Fields, and in particular to the preparation of graphene aerogel, more particularly to it is a kind of based on emulsion method
Graphene aerogel preparation method.
Background technique
Graphene aerogel is the graphene three-dimensional material that obtains by special operation using graphene oxide as raw material.Three
Tieing up graphene aerogel has superior surface area, pore volume abundant, ultralow density, carries in supercapacitor, catalyst
Body and environmental protection etc. have wide Research Prospects and application value.Flourishing hole knot inside graphene aerogel
Structure makes it with superior organic solvent adsorption capacity, general hundreds times up to own wt.Graphene aerogel is to having
The absorption of solvent is mainly physical absorption, and cellular structure and extruding resilience performance can be to the rate of adsorption, adsorbance, circulation benefits
With etc. have an impact.
Based on graphene aerogel in the wide application prospect of numerous areas, more and more research begins to focus on its preparation
Method.Wherein, patent of invention CN104250005A discloses a kind of method that high-energy ray radiation prepares amino aeroge, the party
Method can prepare the graphene aerogel of macropore.Patent of invention CN103213978A discloses hydro-thermal method and prepares graphene airsetting
Glue can regulate and control the duct of graphene aerogel by changing the cryogenic temperature in freeze-drying step.However, mesh
The preparation of preceding graphene aerogel still has following problems: (1) needing in water heating kettle mesohigh pyroreaction or special skill
The processing of art means；(2) the extruding resilience of graphene aerogel is bad, shows as longitudinal extruding resilience, transverse shear stress more
Resilience performance is poor；(3) graphene aerogel cellular structure and porosity can not simply and effectively be controlled, and certain
It is realized in range and porosity is accurately controlled, generally require severe operating conditions, such as cryogenic conditions.
For graphene aerogel, the control of porosity and cellular structure is particularly important.The hole of graphene aerogel
Diameter size uniform and ordered, then have excellent elasticity；Density is smaller, and porosity increases, to the adsorption capacity of the pollutants such as oil product
Increase therewith；Whether cellular structure is open cell type, influences the adsorption capacity of the interior diffusion rate and material in adsorption process；This
Outside, the cellular structure change of graphene aerogel can also change its electrochemical energy storage ability, play the part of weight in supercapacitor field
Want role.Currently, the cellular structure of graphene aerogel and the control of extruding resilience are mainly by changing graphene aerogel
Operating condition, reactant dosage, template etc. in preparation regulate and control porosity, the pore size etc. of graphene aerogel.
Xie etc. (Scientific reports, 2013,3,2117), which discloses, changes ice-crystal growth, control by adjusting cryogenic temperature
The method in aperture；However this method, to low temperature requirements height, range of temperature needs resistance to extremely low temperature from -170~-10 DEG C
Equipment and temperature control means.Huang etc. (Advanced Materials, 2012,24,4419-4423) is modified silicon ball
As template, the accurate control to graphene aerogel aperture is realized, but needs to perform etching using strong corrosive hydrofluoric acid,
Silicon ball is removed, cellular structure is obtained.Zhang etc. (Small, 2016,13,1702-1708) is using 3D orientation printing technique preparation
Graphene aerogel, aeroge density can be in 0.5~10mg/cm3It being controlled, longitudinal elasticity that squeezes can achieve 50%,
But this method needs 1000 DEG C of calcinings, squeezes resilience and is only showed only as longitudinal direction, laterally has no extruding resilience, cellular structure
In have more obturator-type.Therefore, how simply, mildly, green realization graphene aerogel porosity control, be provided simultaneously with
Horizontal and vertical excellent extrusion performance, and retain the more open cell type cellular structure of aeroge, it is the research emphasis of this field
One of.
Pickering lotion is a kind of using solid particle as the lotion of stabilizer, and graphene oxide is because have hydrophily
Edge and hydrophobic substrate, thus can be used as a kind of stabilizer.Using graphene oxide as the Pickering of stabilizer cream
Liquid drop size can be controlled simply by adjustment oil-water ratio, graphene oxide water solution concentration, salt content etc., lotion
It is with good stability, it still keeps stablizing after storage 24 hours.However, in the prior art, graphene oxide is stabilizer
Pickering lotion there are following following problems: (1) generally use it is aromatic hydrocarbon as oily phase, due to aromatic hydrocarbon itself
Toxicity is big, can lead to the problem of in practical applications many；High concentration aromatic hydrocarbon will cause acute poisoning, anaesthetize the maincenter mind of people
Through in addition threat to life；Low concentration aromatic hydrocarbon then will lead to slow poisoning, have to the nervous system of human body, hematological system larger
Injury, or even leukaemia, carcinogenic etc. can be induced.(2) system stability is inadequate；This is because the hydrophily of graphene oxide compared with
By force, small volume is emulsified obtained in emulsion preparation process, and places emulsion droplet after a certain period of time and obvious fusion phenomenon occurs, even
It is demulsified.Currently, not having still studies have reported that preparing graphene aerogel using Pickering lotion.
Summary of the invention
Deficiency based on graphene aerogel preparation in terms of porosity control and longitudinal extruding elasticity, the present invention
Provide a kind of simple, mild, green graphene aerogel preparation method.The present invention is with graphene Pickering lotion work
For soft template, gel is assembled under hydrothermal condition, preparation process is not necessarily to complex operations condition and strong corrosive material, Ke Yishi
Now accurate porosity control, while there is good horizontal and vertical extruding resilience performance, cellular structure remains on pass,
Large scale preparation can be achieved, have broad application prospects.
The technical scheme is that
It is used to prepare the Pickering lotion of graphene aerogel, is made of the following components: according to parts by weight, 0.3~
1 part of graphite oxide, 0~1.84 portion of salt, 0.00365~0.63 part of acid, 0.9~5 part of ascorbic acid, 100 parts of water and 0.2~1
The vegetable oil of times water volume.
The preparation method of graphene aerogel based on emulsion method, comprising the following steps:
(1) appropriate graphite oxide is weighed, and ultrasonic disperse is in water, obtains graphene oxide water solution；
(2) appropriate ascorbic acid and salt are added in the graphene oxide water solution that step (1) obtains；Appropriate amount of acid is added
PH=1~3 are adjusted, appropriate vegetable oil is added, are stirred evenly to get stable Pickering lotion is arrived；
(3) the Pickering lotion by step (2) preparation carries out hydro-thermal reaction, obtains graphene water-setting after reaction
Glue；It is replaced by solvent and removes vegetable oil, freeze-drying obtains graphene aerogel.
Wherein, the mass concentration of step (1) described graphene oxide water solution is that 0.3~1 part of oxygen is added in every 100 parts of water
Graphite；The mass ratio of ascorbic acid described in step (2) and graphene oxide is 3:1~5:1；The mass concentration of the salt is
0~1.84 portion of salt is added in every 100 parts of graphene oxide solutions；Volume ratio 1:1~1:5 of the vegetable oil and water.Preferably
It is that the mass concentration of step (1) described graphene oxide water solution is that 0.3~0.6 part of graphite oxide is added in every 100 parts of water；
The mass ratio of ascorbic acid described in step (2) and graphene oxide is 4:1；The mass concentration of the salt is every 100 parts oxidations
0~0.5 portion of salt is added in graphene solution；Volume ratio 1:2~1:4 of the vegetable oil and water.
Wherein, the reaction temperature of hydro-thermal reaction described in step (3) is 50~90 DEG C, and the reaction time is 5~20 hours；Institute
The temperature for stating freeze-drying is -20~-60 DEG C, and the time of freeze-drying is 12~48 hours.Preferably, step (3) is described
Hydro-thermal reaction reaction temperature be 70~80 DEG C, the reaction time be 5~10 hours；The temperature of the freeze-drying be -50~-
60 DEG C, the time of freeze-drying is 24~36 hours.
Wherein, the rate of step (2) described stirring is 2000~16000r/min, and the time of the stirring is 3-5min；
The time of step (1) described ultrasonic disperse is 0.5~2 hour.Preferably, the ultrasonic time is 1 hour.
Wherein, the vegetable oil be one of peanut oil, soybean oil, rapeseed oil, olive oil, castor oil and linseed oil or
It is several；The salt is one or more of sodium chloride, potassium chloride, magnesium chloride, sodium bromide, potassium bromide and magnesium bromide；The acid
For hydrochloric acid, sulfuric acid or nitric acid.Preferably, in the step (2), salt is sodium chloride or magnesium chloride；Vegetable oil is peanut
Oil, soybean oil or rapeseed oil；The acid is hydrochloric acid, pH=2；
Wherein, the specific steps of step (3) the solvent displacement are as follows: graphene hydrogel is put into built-in organic solvent
In container, organic solvent is made not have hydrogel, teetertotter container several times, is then allowed to stand 1~10 hour, solvent is poured out, it is complete
At primary displacement；Displacement 5~10 times until being mutually precipitated without obvious oil, then is replaced 3~5 times with water；The organic solvent be acetone,
Ethyl alcohol or n-hexane.Preferably, the organic solvent is acetone.
The present invention is based on principle: graphene oxide has hydrophilic edge and lipophilic substrate, can be directly as one
The good emulsion stabilizer of kind.And under conditions of pH=1~3, it is possible to reduce graphene oxide in graphene oxide water solution
Hydrophily, to enhance the stability of emulsion system.By concentration, oil-water ratio, the salt density etc. that adjust graphene oxide
It can be obtained by the graphene aerogel of different pore size.
Compared with prior art, beneficial effects of the present invention are as follows:
(1) preparation method of the present invention is simple, mild condition, without the harsh conditions such as low temperature, corrosive substance, cream
All components in liquid are environmentally protective substance；Therefore large scale preparation may be implemented, has wide application prospect.
(2) graphene aerogel porosity prepared by the present invention may be implemented accurately to control in 99~99.9% ranges
System；Density can achieve it is ultralight, be 2~20mg/cm-3；With good mechanical strength, transverse shear stress reaches 50%, can be complete
Full rebound；Cellular structure is open cell type.
(3) graphene aerogel prepared by the present invention has superior adsorption capacity to petroleum-type product, especially to emulsification
The absorption of oil, thus can be applied to the processing of marine oil spill, oily waste water.
Detailed description of the invention
Fig. 1 is the schematic diagram of preparation method of the present invention.
Fig. 2 is the scanning electron microscope (SEM) photograph of graphene aerogel prepared by the embodiment of the present invention 1.
Fig. 3 is that graphene aerogel transverse shear stress prepared by the embodiment of the present invention 1 springs back photo.
Fig. 4 is that graphene aerogel prepared by the embodiment of the present invention 1 longitudinally squeezes rebound photo.
Specific embodiment
The present invention will be further explained with reference to the examples below.
In following embodiment, graphite used is provided by Aladdin company, crystalline flake graphite used be 325 mesh, remaining raw material by
Sinopharm Chemical Reagent Co., Ltd. provides.
Embodiment 1:
Prepare graphite oxide using improved Hummers method: graphite powder 2g, 98% sulfuric acid 92ml, sodium nitrate 2g are added to
500ml round-bottomed flask stirs 2 hours at 0~10 DEG C, while being slowly added to potassium permanganate 12g, is warming up to 35 DEG C and continues stirring 1
Hour, add 160ml deionized water and be warming up to 95 DEG C, reaction 30 minutes is added 30% hydrogen peroxide of 10ml and removes extra permanganic acid
Potassium.Dialysis one week, freeze-drying obtained graphite oxide powder.
The preparation method of graphene aerogel based on emulsion method, comprising the following steps:
(1) it prepares graphene oxide solution: weighing the graphite oxide of 0.3gHummers method preparation, and ultrasound 1h makes its point
It is dispersed in 100g water, to obtain graphene oxide water solution；
(2) it prepares Pickering lotion: 0.9g ascorbic acid and 0.5g sodium chloride is added to the oxygen that step (1) obtains
In graphite aqueous solution；Appropriate hydrochloric acid is added and adjusts pH=2,20ml peanut oil is added, using the stirring rate of 8000r/min
Stirring 5min arrives stable homogeneous Pickering lotion to stirring evenly；
(3) prepare graphene aerogel: by step (2) preparation Pickering lotion under the conditions of 80 DEG C of temperature into
Row hydro-thermal reaction, reaction time are 10 hours, obtain graphene hydrogel after reaction；Graphene hydrogel is put into built-in
In the container of acetone, it is made not have hydrogel, teetertotter container several times, be then allowed to stand 1 hour, solvent is poured out, completes one
Secondary displacement；Displacement 8 times until being mutually precipitated without obvious oil, then is replaced 5 times with water；It is freeze-dried for 24 hours under the conditions of -20 DEG C of temperature,
Obtain graphene aerogel.
Embodiment 2:
Unlike the first embodiment, the preparation method of the graphene aerogel based on emulsion method, comprising the following steps:
(1) it prepares graphene oxide solution: weighing the graphite oxide of 0.6g preparation, and ultrasound 2h makes it be dispersed in 100g water
In, to obtain graphene oxide water solution；
(2) it prepares Pickering lotion: 1.8g ascorbic acid and 1.0g potassium chloride is added to the oxygen that step (1) obtains
In graphite aqueous solution；Nitric acid is added and adjusts pH=3,25ml soybean oil is added, is stirred using the stirring rate of 16000r/min
3min is mixed to stirring evenly to get to stable homogeneous Pickering lotion；
(3) prepare graphene aerogel: by step (2) preparation Pickering lotion under the conditions of 90 DEG C of temperature into
Row hydro-thermal reaction, reaction time are 5 hours, obtain graphene hydrogel after reaction；Graphene hydrogel is put into built-in
In the container of acetone, it is made not have hydrogel, teetertotter container several times, be then allowed to stand 5 hours, solvent is poured out, completes one
Secondary displacement；Displacement 10 times until being mutually precipitated without obvious oil, then is replaced 3 times with water；It is freeze-dried under the conditions of -40 DEG C of temperature
48h obtains graphene aerogel.
Embodiment 3:
Unlike the first embodiment, the preparation method of the graphene aerogel based on emulsion method, comprising the following steps:
(1) it prepares graphene oxide solution: weighing the graphite oxide of 1g preparation, and ultrasound 0.5h makes it be dispersed in 100g water
In, to obtain graphene oxide water solution；
(2) it prepares Pickering lotion: 5.0g ascorbic acid and 1.5g magnesium chloride is added to the oxygen that step (1) obtains
In graphite aqueous solution；Hydrochloric acid is added and adjusts pH=1,50ml rapeseed oil is added, is stirred using the stirring rate of 2000r/min
5min arrives stable homogeneous Pickering lotion to stirring evenly；
(3) prepare graphene aerogel: by step (2) preparation Pickering lotion under the conditions of 50 DEG C of temperature into
Row hydro-thermal reaction, reaction time are 20 hours, obtain graphene hydrogel after reaction；Graphene hydrogel is put into built-in
In the container of ethyl alcohol, it is made not have hydrogel, teetertotter container several times, be then allowed to stand 10 hours, solvent is poured out, completes one
Secondary displacement；Displacement 5 times until being mutually precipitated without obvious oil, then is replaced 5 times with water；It is freeze-dried 12h under the conditions of -60 DEG C of temperature,
Obtain graphene aerogel.
Embodiment 4:
Unlike the first embodiment, the preparation method of the graphene aerogel based on emulsion method, comprising the following steps:
(1) it prepares graphene oxide solution: weighing the graphite oxide of 0.8g preparation, and ultrasound 1.5h makes it be dispersed in 100g
In water, to obtain graphene oxide water solution；
(2) it prepares Pickering lotion: 2.8g ascorbic acid and 1.84g sodium bromide is added to the oxygen that step (1) obtains
In graphite aqueous solution；Nitric acid is added and adjusts pH=2,80ml olive oil is added, is stirred using the stirring rate of 5000r/min
4min arrives stable homogeneous Pickering lotion to stirring evenly；
(3) prepare graphene aerogel: by step (2) preparation Pickering lotion under the conditions of 60 DEG C of temperature into
Row hydro-thermal reaction, reaction time are 15 hours, obtain graphene hydrogel after reaction；Graphene hydrogel is put into built-in
In the container of organic solvent (acetone, ethyl alcohol or n-hexane), so that it was not had hydrogel, teetertotter container several times, be then allowed to stand 8
Hour, solvent is poured out, primary displacement is completed；Displacement 6 times until being mutually precipitated without obvious oil, then is replaced 4 times with water；At -30 DEG C
It is freeze-dried 30h under the conditions of temperature, obtains graphene aerogel.
Embodiment 5:
Unlike the first embodiment, the preparation method of the graphene aerogel based on emulsion method, comprising the following steps:
(1) it prepares graphene oxide solution: weighing the graphite oxide of 0.5g preparation, and ultrasound 1h makes it be dispersed in 100g water
In, to obtain graphene oxide water solution；
(2) prepare Pickering lotion: it is water-soluble that 2.0g ascorbic acid is added to the graphene oxide that step (1) obtains
In liquid；Sulfuric acid is added and adjusts pH=1,100ml linseed oil is added, is extremely stirred using the stirring rate stirring 3min of 12000r/min
Uniformly to get arrive stable homogeneous Pickering lotion；
(3) prepare graphene aerogel: by step (2) preparation Pickering lotion under the conditions of 70 DEG C of temperature into
Row hydro-thermal reaction, reaction time are 10 hours, obtain graphene hydrogel after reaction；Graphene hydrogel is put into built-in
In the container of n-hexane, it is made not have hydrogel, teetertotters container several times, is then allowed to stand 1~10 hour, solvent is poured out,
Complete primary displacement；Displacement 9 times until being mutually precipitated without obvious oil, then is replaced 4 times with water；It is freezed under the conditions of -50 DEG C of temperature dry
Dry 36h, obtains graphene aerogel.
The characterization result list of the graphene aerogel of 1 embodiment 1-5 of table preparation
| Density, mg/cm3 | Porosity, % | Toluene adsorption capacity, g/g | |
| Embodiment 1 | 9.423 | 99.57 | 127 |
| Embodiment 2 | 8.665 | 99.61 | 133 |
| Embodiment 3 | 14.29 | 99.35 | 89 |
| Embodiment 4 | 10.88 | 99.51 | 115 |
| Embodiment 5 | 6.201 | 99.72 | 151 |
According to table 1, the graphene aerogel of Examples 1 to 5 preparation, density are 6.201~14.29mg/cm3, hole
Gap rate is 99.35~99.72%, belongs to low-density, high porosity range.Using toluene as oily phase, the suction of graphene aerogel
Attached ability reaches 89~151g/g.It is apparent more that the SEM photograph of Fig. 2 shows that graphene aerogel prepared by embodiment 1 has
Pore structure, pore size is at 20~100 μm, and duct stacks orderly, and duct marginal texture is shown as open-celled structure.Fig. 3 and Fig. 4 is aobvious
Show, graphene aerogel prepared by the present invention has good extruding resilience, and longitudinal squeeze has and can reach with transverse shear stress
50%, without obvious deformation and breakage when rebound.In conclusion graphene aerogel prepared by the present invention can be adjusted effectively
Density and porosity, cellular structure open cell type is high to oily phase adsorption capacity, and excellent horizontal and vertical extruding resilience is conducive to
Absorption-recycling of oily phase.
Claims (7)
1. the preparation method of the graphene aerogel based on emulsion method, it is characterised in that: the following steps are included:
(1) appropriate graphite oxide is weighed, and ultrasonic disperse is in water, obtains graphene oxide water solution；The graphene oxide
The mass concentration of aqueous solution is that 0.3~1 part of graphite oxide is added in every 100 parts of water；
(2) appropriate ascorbic acid and salt are added in the graphene oxide water solution that step (1) obtains；Appropriate amount of acid is added to adjust
Appropriate vegetable oil is added in pH=1~3, stirs evenly to get stable Pickering lotion is arrived；The ascorbic acid and oxidation
The mass ratio of graphene is 3:1~5:1；The mass concentration of the salt is that 0~1.84 is added in every 100 parts of graphene oxide solutions
Part salt；Volume ratio 1:1~1:5 of the vegetable oil and water；
(3) the Pickering lotion by step (2) preparation carries out hydro-thermal reaction, obtains graphene hydrogel after reaction；It is logical
It crosses solvent displacement and removes vegetable oil, freeze-drying obtains graphene aerogel；The reaction temperature of the hydro-thermal reaction be 50~
90 DEG C, the reaction time is 5~20 hours；The cryogenic temperature of the freeze-drying is -20~-60 DEG C, and the time of freeze-drying is
12~48 hours.
2. the preparation method of the graphene aerogel according to claim 1 based on emulsion method, it is characterised in that: step
(1) mass concentration of the graphene oxide water solution is that 0.3~0.6 part of graphite oxide is added in every 100 parts of water；Step (2)
Described in the mass ratio of ascorbic acid and graphene oxide be 4:1；The mass concentration of the salt is that every 100 parts of graphene oxides are molten
0~0.5 portion of salt is added in liquid；Volume ratio 1:2~1:4 of the vegetable oil and water.
3. the preparation method of the graphene aerogel according to claim 1 based on emulsion method, it is characterised in that: step
(3) reaction temperature of the hydro-thermal reaction described in is 70~80 DEG C, and the reaction time is 5~10 hours；The temperature of the freeze-drying
It is -50~-60 DEG C, the time of freeze-drying is 24~36 hours.
4. the preparation method of the graphene aerogel according to claim 2 based on emulsion method, it is characterised in that: step
(2) rate of the stirring is 2000~16000r/min, and the time of the stirring is 3-5min；Step (1) ultrasound point
The scattered time is 0.5~2 hour.
5. the preparation method of the graphene aerogel according to claim 2 based on emulsion method, it is characterised in that: the plant
Object oil is one or more of peanut oil, soybean oil, rapeseed oil, olive oil, castor oil and linseed oil；The salt is chlorination
One or more of sodium, potassium chloride, magnesium chloride, sodium bromide, potassium bromide and magnesium bromide；The acid is hydrochloric acid, sulfuric acid or nitre
Acid.
6. the preparation method of the graphene aerogel according to claim 4 or 5 based on emulsion method, it is characterised in that: institute
It states in step (1), ultrasonic time 1 hour；In the step (2), salt is sodium chloride or magnesium chloride；Vegetable oil be peanut oil,
Soybean oil or rapeseed oil；The acid is hydrochloric acid, pH=2.
7. the preparation method of the graphene aerogel according to claim 1 based on emulsion method, it is characterised in that: step
(3) specific steps of the solvent displacement are as follows: graphene hydrogel is put into the container of built-in organic solvent, makes organic solvent
Hydrogel is not crossed, teetertotters container several times, is then allowed to stand 1~10 hour, solvent is poured out, completes primary displacement；Displacement 5~
It 10 times, until being mutually precipitated without obvious oil, then is replaced 3~5 times with water；The organic solvent is acetone, ethyl alcohol or n-hexane.
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