CN110371958A - A kind of Microwave reduction method prepares molysite intercalated graphite alkene aeroge - Google Patents
A kind of Microwave reduction method prepares molysite intercalated graphite alkene aeroge Download PDFInfo
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- CN110371958A CN110371958A CN201910691679.6A CN201910691679A CN110371958A CN 110371958 A CN110371958 A CN 110371958A CN 201910691679 A CN201910691679 A CN 201910691679A CN 110371958 A CN110371958 A CN 110371958A
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- ferric trichloride
- intercalation
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- intercalated graphite
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
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Abstract
The present invention provides a kind of Microwave reduction method and prepares molysite intercalated graphite alkene aeroge.Oxygen-containing group layer and ferric trichloride alternating intercalated graphite material are prepared first, it is put into ultrasound removing in aqueous solution, obtain dispersible ferric trichloride intercalation graphene oxide in water, it is freeze-dried, obtain ferric trichloride intercalation graphite oxide aerogel, microwave treatment is carried out, molysite intercalated graphite alkene aeroge is obtained.The method of the present invention effectively mitigates graphene sheet layer structural damage, oxygen-containing group is efficiently removed using microwave, it avoids in reduction process using high temperature or reducing agent to tri-chlorination iron layer structural damage, ferric trichloride is evenly distributed on graphene film interlayer, effectively improves graphene aerogel electric conductivity, insulating refractory, silencing and damping performance, has broad application prospects, preparation process is simple, requirement to equipment is lower, is suitable for industry or laboratory operation, has huge application prospect.
Description
Technical field
The present invention relates to graphene aerogel preparation fields more particularly to a kind of Microwave reduction method to prepare molysite intercalated graphite
Alkene aeroge.
Background technique
Aeroge has many advantages, such as that density is low, thermal conductivity is small, hole is flourishing, fireclay insulating refractory, silencing and damping material,
Catalyst, dust acquirer, cleanser etc. have broad application prospects.Graphene aerogel refers to based on graphene
The three-dimensional porous network structure of body is imparted based on its unique globality structure, high-specific surface area and excellent conductivity
Its application prospect wide in fields such as electrode material, catalytic carrier and sea water desalinations, such as can be used as electrochemical double layer capacitor
The electrode of device, novel hydrogen storage materials etc..
Graphene intercalation compound is to form one layer of new intercalator between different atoms or molecule insertion graphene layer
The composite material of layer.The presence of intercalator increases interlamellar spacing, while different intercalator can also allow freely the carrying of graphene layer
Stream migrates, so that the compound with properties such as different electricity, calorifics and magnetics is obtained, for example, Britain's Ai Ke Saite
Professor Cracium of university describes the electric conductivity that can make graphene to graphene progress intercalation doping treatment using iron chloride
It improves to original ten times or more, and can keep stablizing for a long time in room temperature and atmospheric environment, show to utilize iron chloride pair
Graphene is doped the electric conductivity that can effectively improve graphene nanometer sheet.
Summary of the invention
The present invention provides a kind of Microwave reduction method and prepares molysite intercalated graphite alkene aeroge, different from traditional graphene gas
Gel is usually using graphene oxide as raw material and using redox graphene as three-dimensional porous network skeleton, present invention preparation
Oxygen content relatively low graphene intercalation compound, and construct skeleton with it can be with by microwave decomposition oxygen-containing functional group
The destruction of graphene sheet layer and molysite intercalation configuration is effectively reduced, materials conductive, insulating refractory, silencing and damping performance are improved.
The present invention adopts the following technical scheme:
A kind of Microwave reduction method prepares molysite intercalated graphite alkene aeroge, includes the following steps:
(1) anhydrous ferric trichloride and graphite Hybrid Heating are prepared into second order graphite intercalation compound with molte-salt synthesis；
(2) oxidation intercalation is carried out to second order graphene intercalation compound using oxidant and concentrated acid, obtains oxygen-containing group layer
With the material of ferric trichloride alternating intercalated graphite；
(3) oxygen-containing group layer and ferric trichloride alternating intercalated graphite are put into aqueous solution and are ultrasonically treated, remove oxygen-containing group
Group's layer obtains dispersible ferric trichloride intercalation graphene oxide in water；
(4) ferric trichloride intercalation graphene oxide dispersion is freeze-dried, obtains ferric trichloride intercalation oxidation stone
Black alkene aeroge；
(5) microwave treatment is carried out to ferric trichloride intercalation graphite oxide aerogel, obtains molysite intercalated graphite alkene airsetting
Glue.
Molten-salt growth method reaction temperature in step (1) is 400 DEG C, and the reaction time is 4-6 hours, anhydrous ferric trichloride and graphite
Mass ratio is 5: 1.
Oxidant in step (2) includes chlorate, perchlorate, permanganate, bichromate, sodium peroxide, concentrated acid
For the concentrated sulfuric acid or the mixture of the concentrated sulfuric acid and concentrated nitric acid, the oxidation intercalation time is 4-48h, and temperature is 0-80 DEG C.
Ultrasonic time in step (3) is 0.5-2h.
Freeze-drying temperature in step (4) is < -30 DEG C, vacuum degree < 20Pa, drying time 12-72h.
Microwave power in step (5) is 500-1000W, and microwave frequency 915MHz-2450MHz, the microwave time is 5-
1800s。
The present invention has the advantage that
(1) graphite flake in the material for oxygen-containing group layer and ferric trichloride the alternating intercalated graphite that the method for the invention obtains
Layer single side oxidation, amount of oxidation reduce half, effectively mitigate graphene sheet layer structural damage, reduce graphite oxide method bring
The variation drawback such as electric conductivity and mechanical property.
(2) the method for the invention efficiently removes oxygen-containing group using microwave, avoid in reduction process using high temperature or
Reducing agent is evenly distributed on graphene film interlayer to tri-chlorination iron layer structural damage, ferric trichloride, effectively improves graphene gas
Gel electric conductivity, insulating refractory, silencing and damping performance.
(3) the novel molysite intercalated graphite alkene aeroge prepared in the method for the invention is in electrode material, catalytic carrier
And the fields such as sea water desalination have broad application prospects.
(4) the method for the invention preparation process is simple, and the requirement to equipment is lower, is suitable for industry or laboratory operation,
With huge application prospect.
Detailed description of the invention
Fig. 1 is the structural schematic diagram that the method for the present invention prepares second order graphite intercalation compound.
Fig. 2 is that oxidant and concentrated acid carry out oxidation intercalation to second order ferric trichloride graphite intercalation compound in the method for the present invention
Structural schematic diagram.
Fig. 3 is the structural schematic diagram that the method for the present invention prepares ferric trichloride intercalation graphene oxide.
Fig. 4 is the structural schematic diagram that the method for the present invention prepares molysite intercalated graphite alkene aeroge.
Specific embodiment
Of the invention for ease of understanding, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is used only for helping to understand the present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1
(1) 300mg anhydrous ferric trichloride is uniformly mixed with 60mg expanded graphite, is vacuumized, be enclosed within 50mL vial
In, 400 DEG C of heating 4h prepare pure second order graphite intercalation compound, graphite intercalation compound are dissolved in dilute hydrochloric acid solution, take out
Filter drying.
(2) graphite intercalation compound is added in the mixed solution of the 20mL concentrated sulfuric acid and the concentrated nitric acid of 10mL, in ice water
(0 DEG C) is stirred 0.5 hour, and 360mg sodium chlorate is put into solution, stirs 12 hours at room temperature, product eccentric cleaning obtains
Replace intercalated graphite to oxygen-containing group layer and ferric trichloride.
(3) oxygen-containing group layer and ferric trichloride alternating intercalated graphite are put into aqueous solution and are ultrasonically treated 1h, obtain to divide
Dissipate ferric trichloride intercalation graphene oxide in water.
(4) ferric trichloride intercalation graphene oxide dispersion is freeze-dried, freeze-drying temperature is -70 DEG C, very
Reciprocal of duty cycle is 10Pa, and drying time is for 24 hours, to obtain ferric trichloride intercalation graphite oxide aerogel.
(5) microwave treatment, microwave power 700W, microwave frequency are carried out to ferric trichloride intercalation graphite oxide aerogel
For 2450MHz, the microwave time is 120s, obtains molysite intercalated graphite alkene aeroge.
Embodiment 2
(1) 300mg anhydrous ferric trichloride is uniformly mixed with 60mg expanded graphite, is vacuumized, be enclosed within 50mL vial
In, 400 DEG C of heating 4h prepare pure second order graphite intercalation compound, graphite intercalation compound are dissolved in dilute hydrochloric acid solution, take out
Filter drying.
(2) graphite intercalation compound is added in 20mL concentrated sulfuric acid solution, is stirred 0.5 hour for (0 DEG C) in ice water, it will
360mg potassium permanganate is put into solution, is stirred 12 hours at room temperature, by product eccentric cleaning, is obtained oxygen-containing group layer and three
Iron chloride replaces intercalated graphite.
(3) oxygen-containing group layer and ferric trichloride alternating intercalated graphite are put into aqueous solution and are ultrasonically treated 1h, obtain to divide
Dissipate ferric trichloride intercalation graphene oxide in water.
(4) ferric trichloride intercalation graphene oxide dispersion is freeze-dried, freeze-drying temperature is -70 DEG C, very
Reciprocal of duty cycle is 10Pa, and drying time is for 24 hours, to obtain ferric trichloride intercalation graphite oxide aerogel.
(5) microwave treatment, microwave power 700W, microwave frequency are carried out to ferric trichloride intercalation graphite oxide aerogel
For 2450MHz, the microwave time is 120s, obtains molysite intercalated graphite alkene aeroge.
Embodiment 3
(1) 300mg anhydrous ferric trichloride is uniformly mixed with 60mg expanded graphite, is vacuumized, be enclosed within 50mL vial
In, 400 DEG C of heating 4h prepare pure second order graphite intercalation compound, graphite intercalation compound are dissolved in dilute hydrochloric acid solution, take out
Filter drying.
(2) graphite intercalation compound is added in the mixed solution of the 20mL concentrated sulfuric acid and the concentrated nitric acid of 10mL, in ice water
(0 DEG C) is stirred 0.5 hour, and 360mg sodium chlorate is put into solution, stirs 12 hours at room temperature, product eccentric cleaning obtains
Replace intercalated graphite to oxygen-containing group layer and ferric trichloride.
(3) oxygen-containing group layer and ferric trichloride alternating intercalated graphite are put into aqueous solution and are ultrasonically treated 1h, obtain to divide
Dissipate ferric trichloride intercalation graphene oxide in water.
(4) ferric trichloride intercalation graphene oxide dispersion is freeze-dried, freeze-drying temperature is -70 DEG C, very
Reciprocal of duty cycle is 2Pa, drying time 12h, obtains ferric trichloride intercalation graphite oxide aerogel.
(5) microwave treatment, microwave power 700W, microwave frequency are carried out to ferric trichloride intercalation graphite oxide aerogel
For 2450MHz, the microwave time is 120s, obtains molysite intercalated graphite alkene aeroge.
Embodiment 4
(1) 300mg anhydrous ferric trichloride is uniformly mixed with 60mg expanded graphite, is vacuumized, be enclosed within 50mL vial
In, 400 DEG C of heating 4h prepare pure second order graphite intercalation compound, graphite intercalation compound are dissolved in dilute hydrochloric acid solution, take out
Filter drying.
(2) graphite intercalation compound is added in the mixed solution of the 20mL concentrated sulfuric acid and the concentrated nitric acid of 10mL, in ice water
(0 DEG C) is stirred 0.5 hour, and 360mg sodium chlorate is put into solution, stirs 12 hours at room temperature, product eccentric cleaning obtains
Replace intercalated graphite to oxygen-containing group layer and ferric trichloride.
(3) oxygen-containing group layer and ferric trichloride alternating intercalated graphite are put into aqueous solution and are ultrasonically treated 1h, obtain to divide
Dissipate ferric trichloride intercalation graphene oxide in water.
(4) ferric trichloride intercalation graphene oxide dispersion is freeze-dried, freeze-drying temperature is -70 DEG C, very
Reciprocal of duty cycle is 10Pa, and drying time is for 24 hours, to obtain ferric trichloride intercalation graphite oxide aerogel.
(5) microwave treatment, microwave power 1000W, Microwave Frequency are carried out to ferric trichloride intercalation graphite oxide aerogel
Rate is 2450MHz, and the microwave time is 30s, obtains molysite intercalated graphite alkene aeroge.
The Applicant declares that the present invention is explained by the above embodiments detailed process equipment and process flow of the invention,
But the present invention is not limited to the above detailed process equipment and process flow, that is, it is above-mentioned detailed not mean that the present invention must rely on
Process equipment and process flow could be implemented.It should be clear to those skilled in the art, any improvement in the present invention,
Addition, selection of concrete mode of equivalence replacement and auxiliary element to each raw material of product of the present invention etc., all fall within of the invention
Within protection scope and the open scope.
Claims (6)
1. a kind of Microwave reduction method prepares molysite intercalated graphite alkene aeroge, include the following steps:
(1) anhydrous ferric trichloride and graphite Hybrid Heating are prepared into second order graphite intercalation compound with molte-salt synthesis；
(2) oxidation intercalation is carried out to second order graphene intercalation compound using oxidant and concentrated acid, obtains oxygen-containing group layer and three
The material of iron chloride alternating intercalated graphite；
(3) oxygen-containing group layer and ferric trichloride alternating intercalated graphite are put into aqueous solution and are ultrasonically treated, remove oxygen-containing group layer
Obtain dispersible ferric trichloride intercalation graphene oxide in water；
(4) ferric trichloride intercalation graphene oxide dispersion is freeze-dried, obtains ferric trichloride intercalation graphene oxide
Aeroge；
(5) microwave treatment is carried out to ferric trichloride intercalation graphite oxide aerogel, obtains molysite intercalated graphite alkene aeroge.
2. preparation method according to claim 1, which is characterized in that the molten-salt growth method reaction temperature in step (1) is 400
DEG C, the reaction time is 4-6 hours, and anhydrous ferric trichloride and graphite quality ratio are 5: 1.
3. preparation method according to claim 1, which is characterized in that the oxidant in step (2) includes chlorate, high chlorine
Hydrochlorate, permanganate, bichromate, sodium peroxide, concentrated acid are the mixture of the concentrated sulfuric acid or the concentrated sulfuric acid and concentrated nitric acid, and oxidation is inserted
The layer time is 4-48h, and temperature is 0-80 DEG C.
4. preparation method according to claim 1, which is characterized in that the ultrasonic time in step (3) is 0.5-2h.
5. preparation method according to claim 1, which is characterized in that the freeze-drying temperature in step (4) is < -30
DEG C, vacuum degree < 20Pa, drying time 12-72h.
6. preparation method according to claim 1, which is characterized in that the microwave power in step (5) is 500-1000W,
Microwave frequency is 915MHz-2450MHz, and the microwave time is 5-1800s.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910691679.6A CN110371958A (en) | 2019-07-24 | 2019-07-24 | A kind of Microwave reduction method prepares molysite intercalated graphite alkene aeroge |
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| CN201910691679.6A CN110371958A (en) | 2019-07-24 | 2019-07-24 | A kind of Microwave reduction method prepares molysite intercalated graphite alkene aeroge |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023279356A1 (en) * | 2021-07-08 | 2023-01-12 | 苏州盛魅新材料科技有限公司 | Device for manufacturing intercalated graphene antimicrobial material |
| CN115974059A (en) * | 2022-09-09 | 2023-04-18 | 杭州高烯科技有限公司 | High-elasticity graphene composite aerogel and preparation method and application thereof |
-
2019
- 2019-07-24 CN CN201910691679.6A patent/CN110371958A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023279356A1 (en) * | 2021-07-08 | 2023-01-12 | 苏州盛魅新材料科技有限公司 | Device for manufacturing intercalated graphene antimicrobial material |
| CN115974059A (en) * | 2022-09-09 | 2023-04-18 | 杭州高烯科技有限公司 | High-elasticity graphene composite aerogel and preparation method and application thereof |
| CN115974059B (en) * | 2022-09-09 | 2023-09-05 | 杭州高烯科技有限公司 | High-elastic graphene composite aerogel and preparation method and application thereof |
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Application publication date: 20191025 |