CN103449414A - Preparation method of graphene having porous structure - Google Patents
Preparation method of graphene having porous structure Download PDFInfo
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- CN103449414A CN103449414A CN2012101765622A CN201210176562A CN103449414A CN 103449414 A CN103449414 A CN 103449414A CN 2012101765622 A CN2012101765622 A CN 2012101765622A CN 201210176562 A CN201210176562 A CN 201210176562A CN 103449414 A CN103449414 A CN 103449414A
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Abstract
The invention discloses a preparation method of graphene having a porous structure. The preparation method comprises the following steps of 1, adding graphite oxide, a reducing agent and a pore-forming agent into deionized water, and carrying out uniform mixing to obtain a mixed liquid, wherein a mass ratio of the graphite oxide, the reducing agent to the pore-forming agent is 1: (0.1-1): (0.2-0.5), 2, heating the mixed liquid to a temperature of 80-100 DEG C for a reduction reaction to obtain a graphene-pore-forming agent mixture, and 3, drying the graphene-pore-forming agent mixture at a temperature of 60-80 DEG C for 24-48h, heating the dried mixture to a temperature of 300-400 DEG C, carrying out heat preservation reaction for 3-5min, and cooling the mixture to a room temperature in a protective atmosphere to obtain the graphene having the porous structure. The preparation method has the simple processes, adopts the raw materials having wide sources and a low cost, has a low reaction temperature, can be controlled easily, and can realize batch production.
Description
Technical field
The present invention relates to the synthetic field of material, particularly a kind of preparation method with Graphene of vesicular structure.
Background technology
Graphene is a kind of Two-dimensional Carbon atomic crystal that the strong K of the peace moral of Univ Manchester UK in 2004 sea nurse (Andre K.Geim) etc. is found, and obtains the physics Nobel prize in 2010, again causes the carbon material research boom.Because its unique structure and photoelectric property make it become the study hotspot in the fields such as carbon material, nanotechnology, Condensed Matter Physics and functional materials, many scientific workers have been attracted.Single-layer graphene has good conduction, heat conductivility and low thermal expansivity, and its theoretical specific surface area is up to 2630m
2/ g(A Peigney, Ch Laurent, et al.Carbon, 2001,39,507), can be used for effect transistor, electrode materials, matrix material, liquid crystal display material, sensor.The place that the preparation method of traditional Graphene still comes with some shortcomings, be difficult to prepare the Graphene with specific morphology.And at present, the preparation method of porous graphene that had the investigator to provide, but its operation is too complicated, is difficult to control.
Summary of the invention
Given this, be necessary to provide a kind of simple to operate and more manageable preparation to there is the method for the Graphene of vesicular structure.
A kind of preparation method with Graphene of vesicular structure, comprise the steps:
Step 1: graphite oxide, reductive agent and pore-forming material are added in deionized water, mix, obtain mixed solution; Wherein, the mass ratio of described graphite oxide, reductive agent and pore-forming material is 1:(0.1 ~ 1): (0.2 ~ 0.5);
Step 2: described mixed solution is heated to 80 ℃ ~ 100 ℃, reduction reaction occurs, obtain the mixture of Graphene and described pore-forming material; And
Step 3: described mixture after dry 24 hours ~ 48 hours, is heated to 300 ℃ ~ 400 ℃ under 60 ℃ ~ 80 ℃, and insulation reaction, after 3 minutes ~ 5 minutes, in protection compression ring border, is cooled to room temperature, obtains the described Graphene with vesicular structure.
In embodiment, in step 1, described reductive agent is at least one in hydrazine, sodium borohydride, POTASSIUM BOROHYDRIDE and Trisodium Citrate therein.
In embodiment, in step 1, described pore-forming material is sodium bicarbonate or saleratus therein.
Therein in embodiment, in step 1, the blending means of described graphite oxide, described reductive agent, described pore-forming material and described deionized water is ultrasonic mixing 30 minutes ~ 60 minutes.
In embodiment, after step 2, also comprise the step that the product after described reduction reaction is filtered and cleans therein.
In embodiment, in step 3, described protection gas is at least one in hydrogen, argon gas and nitrogen therein.
Therein in embodiment, in step 3, the cooling speed of the product after described insulation reaction in described protection compression ring border is 30 ℃/min～50 ℃/min.
The above-mentioned preparation method with Graphene of vesicular structure, reductive agent is reduced into Graphene by graphite oxide, pore-forming material is prepared the Graphene with vesicular structure by high temperature decomposing, its preparation method is simple, and in preparation process, required raw material sources are wide and cost is low, temperature of reaction is low, is easy to control, thereby can realizes batch production.
The accompanying drawing explanation
Preparation method's schema of the Graphene with vesicular structure that Fig. 1 is an embodiment;
The scanning electron microscope (SEM) photograph (SEM) of the Graphene with vesicular structure that Fig. 2 is embodiment 1 preparation.
Embodiment
Below main in conjunction with the drawings and the specific embodiments the preparation method of Graphene with vesicular structure is described in further detail.
As shown in Figure 1, the preparation method of the Graphene with vesicular structure of an embodiment comprises as step:
Step S1: graphite oxide, reductive agent and pore-forming material are added in deionized water, mix, obtain mixed solution.Wherein, the mass ratio of graphite oxide, reductive agent and pore-forming material is 1:(0.1 ~ 1): (0.2 ~ 0.5).
Wherein, graphite oxide is graphite oxide commonly used.
Wherein, the blending means of graphite oxide, reductive agent, pore-forming material and deionized water is ultrasonic mixing 30 minutes ~ 60 minutes.
Wherein, reductive agent is this area reductive agent commonly used, is preferably at least one in hydrazine, sodium borohydride, POTASSIUM BOROHYDRIDE and Trisodium Citrate.Reductive agent is reduced into Graphene by graphite oxide.
Wherein, pore-forming material is this area pore-forming material commonly used, is preferably sodium bicarbonate or saleratus.Pore-forming material can at high temperature decompose, release of carbon dioxide, thus staying abundant hole on Graphene, reaction formula is as follows:
The chemical equation of sodium bicarbonate pyrolytic decomposition:
The chemical equation of saleratus pyrolytic decomposition:
Step S2: mixed solution is heated to 80 ℃ ~ 100 ℃, reduction reaction occurs, obtain the mixture of Graphene and pore-forming material.
In the present embodiment, after step S2, also comprise the step that the product after reduction reaction is filtered and cleans.By filtering and cleaning, obtain purer Graphene and the mixture of pore-forming material.
Step S3: mixture after dry 24 hours ~ 48 hours, is heated to 300 ℃ ~ 400 ℃ under 60 ℃～80 ℃, and insulation reaction, after 3 minutes ~ 5 minutes, in protection compression ring border, is cooled to room temperature, obtains having the Graphene of vesicular structure.It is more complete that insulation reaction makes pore-forming material divide in 3 minutes ~ 5 minutes to solve.In the present embodiment; in protection, the cooling speed in the compression ring border is 30 ℃/min～50 ℃/min to product after insulation reaction; by cooling rapidly, thereby keep the hole stayed on Graphene after the pore-forming material decomposition not close, make Graphene there is the structure of porous.Wherein, protection gas is at least one in hydrogen, argon gas and nitrogen.While using sodium bicarbonate or saleratus as pore-forming material, after step S3, to the step of the cleaning of Graphene: add deionized water in Graphene, filter, until filtrate is neutral.By cleaning Graphene, remove sodium ion or potassium ion wherein.
The above-mentioned preparation method with Graphene of vesicular structure, reductive agent is reduced into Graphene by graphite oxide, pore-forming material is prepared the Graphene with vesicular structure by high temperature decomposing, its preparation method is simple, and in preparation process, required raw material sources are wide and cost is low, temperature of reaction is low, is easy to control, thereby can realizes batch production.And the Graphene that above-mentioned preparation method prepares has abundant hole, and oxygen level is low, can be applicable to noise reduction, sound-proof material, gas adsorption etc.
Be below the specific embodiment part:
Embodiment 1
(1) beaker that the selection capacity is 1L adds the deionized water of 1L in beaker, then 1g graphite oxide, 0.1g hydrazine and 0.2g sodium bicarbonate is added in deionized water, and ultrasonic mixing 30 minutes, obtain mixed solution.
(2) mixed solution is heated to 100 ℃, reduction reaction occurs, filter and clean, obtain the mixture of Graphene and sodium bicarbonate.
(3) mixture after dry 24 hours, is placed on quartz boat, and is heated to 300 ℃ in Reaktionsofen under 60 ℃, after insulation reaction 5 minutes, in hydrogen environment, be cooled to room temperature, rate of cooling is 30 ℃/min, open Reaktionsofen, collect solid product, add deionized water in solid product, filter, repeatedly add deionized water, filtration, until filtrate is neutral, obtain having the Graphene of vesicular structure.The scanning electron microscope (SEM) photograph (SEM) that Fig. 2 is the Graphene with vesicular structure for preparing of the present embodiment, as can be seen from the figure, Graphene with vesicular structure prepared by the present embodiment has abundant hole, the size of hole does not wait from 1nm～500nm, lamellar spacing is about 1nm～3nm, and the specific surface area that makes Graphene is 1270m
2/ g.
Embodiment 2
(1) beaker that the selection capacity is 1L adds the deionized water of 1L in beaker, then 1g graphite oxide, 1g sodium borohydride and 0.4g sodium bicarbonate is added in deionized water, and ultrasonic mixing 60 minutes, obtain mixed solution.
(2) mixed solution is heated to 90 ℃, reduction reaction occurs, filter and clean, obtain the mixture of Graphene and sodium bicarbonate.
(3) mixture after dry 36 hours, is placed on quartz boat, and is heated to 400 ℃ in Reaktionsofen under 80 ℃, after insulation reaction 3 minutes, in ar gas environment, be cooled to room temperature, rate of cooling is 50 ℃/min, open Reaktionsofen, collect solid product, add deionized water in solid product, filter, repeatedly add deionized water, filtration, until filtrate is neutral, obtain having the Graphene of vesicular structure.
Embodiment 3
(1) beaker that the selection capacity is 1L adds the deionized water of 1L in beaker, then 1g graphite oxide, 0.8g POTASSIUM BOROHYDRIDE and 0.3g saleratus is added in deionized water, and ultrasonic mixing 40 minutes, obtain mixed solution.
(2) mixed solution is heated to 95 ℃, reduction reaction occurs, filter and clean, obtain the mixture of Graphene and saleratus.
(3) mixture after dry 30 hours, is placed on quartz boat, and is heated to 400 ℃ in Reaktionsofen under 70 ℃, after insulation reaction 4 minutes, in nitrogen environment, be cooled to room temperature, rate of cooling is 40 ℃/min, open Reaktionsofen, collect solid product, add deionized water in solid product, filter, repeatedly add deionized water, filtration, until filtrate is neutral, obtain having the Graphene of vesicular structure.
Embodiment 4
(1) beaker that the selection capacity is 1L adds the deionized water of 1L in beaker, then 1g graphite oxide, 0.5g Trisodium Citrate and 0.5g saleratus is added in deionized water, and ultrasonic mixing 50 minutes, obtain mixed solution.
(2) mixed solution is heated to 80 ℃, reduction reaction occurs, filter and clean, obtain the mixture of Graphene and saleratus.
(3) mixture after dry 48 hours, is placed on quartz boat, and is heated to 350 ℃ in Reaktionsofen under 65 ℃, after insulation reaction 5 minutes, in the gas mixture environment of hydrogen and argon gas, be cooled to room temperature, rate of cooling is 45 ℃/min, open Reaktionsofen, collect solid product, add deionized water in solid product, filter, repeatedly add deionized water, filtration, until filtrate is neutral, obtain having the Graphene of vesicular structure.
Embodiment 5
(1) beaker that the selection capacity is 1L adds the deionized water of 1L in beaker, then 1g graphite oxide, 0.2g hydrazine and 0.2g saleratus is added in deionized water, and ultrasonic mixing 60 minutes, obtain mixed solution.
(2) mixed solution is heated to 95 ℃, reduction reaction occurs, filter and clean, obtain the mixture of Graphene and saleratus.
(3) mixture after dry 35 hours, is placed on quartz boat, and is heated to 320 ℃ in Reaktionsofen under 70 ℃, after insulation reaction 5 minutes, in the gas mixture environment of hydrogen, argon gas and nitrogen, be cooled to room temperature, rate of cooling is 35 ℃/min, open Reaktionsofen, collect solid product, add deionized water in solid product, filter, repeatedly add deionized water, filtration, until filtrate is neutral, obtain having the Graphene of vesicular structure.
Embodiment 6
(1) beaker that the selection capacity is 1L adds the deionized water of 1L in beaker, then 1g graphite oxide, 0.8g sodium borohydride and 0.3g saleratus is added in deionized water, and ultrasonic mixing 50 minutes, obtain mixed solution.
(2) mixed solution is heated to 85 ℃, reduction reaction occurs, filter and clean, obtain the mixture of Graphene and saleratus.
(3) mixture after dry 45 hours, is placed on quartz boat, and is heated to 400 ℃ in Reaktionsofen under 65 ℃, after insulation reaction 3 minutes, in the gas mixture environment of hydrogen and nitrogen, be cooled to room temperature, rate of cooling is 40 ℃/min, open Reaktionsofen, collect solid product, add deionized water in solid product, filter, repeatedly add deionized water, filtration, until filtrate is neutral, obtain having the Graphene of vesicular structure.
Embodiment 7
(1) beaker that the selection capacity is 1L adds the deionized water of 1L in beaker, then 1g graphite oxide, 1g POTASSIUM BOROHYDRIDE and 0.5g sodium bicarbonate is added in deionized water, and ultrasonic mixing 40 minutes, obtain mixed solution.
(2) mixed solution is heated to 100 ℃, reduction reaction occurs, filter and clean, obtain the mixture of Graphene and sodium bicarbonate.
(3) mixture after dry 24 hours, is placed on quartz boat, and is heated to 380 ℃ in Reaktionsofen under 80 ℃, after insulation reaction 5 minutes, in the gas mixture environment of argon gas and nitrogen, be cooled to room temperature, rate of cooling is 45 ℃/min, open Reaktionsofen, collect solid product, add deionized water in solid product, filter, repeatedly add deionized water, filtration, until filtrate is neutral, obtain having the Graphene of vesicular structure.
Embodiment 8
(1) beaker that the selection capacity is 1L adds the deionized water of 1L in beaker, then 1g graphite oxide, 0.3g Trisodium Citrate and 0.4g saleratus is added in deionized water, and ultrasonic mixing 30 minutes, obtain mixed solution.
(2) mixed solution is heated to 80 ℃, reduction reaction occurs, filter and clean, obtain the mixture of Graphene and saleratus.
(3) mixture after dry 48 hours, is placed on quartz boat, and is heated to 330 ℃ in Reaktionsofen under 75 ℃, after insulation reaction 3 minutes, in hydrogen environment, be cooled to room temperature, rate of cooling is 50 ℃/min, open Reaktionsofen, collect solid product, add deionized water in solid product, filter, repeatedly add deionized water, filtration, until filtrate is neutral, obtain having the Graphene of vesicular structure.
Embodiment 9
(1) beaker that the selection capacity is 1L adds the deionized water of 1L in beaker, then 1g graphite oxide, 0.5g hydrazine, 0.2g sodium borohydride and 0.2g saleratus is added in deionized water, and ultrasonic mixing 60 minutes, obtain mixed solution.
(2) mixed solution is heated to 95 ℃, reduction reaction occurs, filter and clean, obtain the mixture of Graphene and saleratus.
(3) mixture after dry 45 hours, is placed on quartz boat, and is heated to 300 ℃ in Reaktionsofen under 60 ℃, after insulation reaction 5 minutes, in nitrogen environment, be cooled to room temperature, rate of cooling is 30 ℃/min, open Reaktionsofen, collect solid product, add deionized water in solid product, filter, repeatedly add deionized water, filtration, until filtrate is neutral, obtain having the Graphene of vesicular structure.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (7)
1. the preparation method with Graphene of vesicular structure, is characterized in that, comprises the steps:
Step 1: graphite oxide, reductive agent and pore-forming material are added in deionized water, mix, obtain mixed solution; Wherein, the mass ratio of described graphite oxide, reductive agent and pore-forming material is 1:(0.1 ~ 1): (0.2 ~ 0.5);
Step 2: described mixed solution is heated to 80 ℃ ~ 100 ℃, reduction reaction occurs, obtain the mixture of Graphene and described pore-forming material; And
Step 3: described mixture after dry 24 hours ~ 48 hours, is heated to 300 ℃ ~ 400 ℃ under 60 ℃～80 ℃, and insulation reaction, after 3 minutes ~ 5 minutes, in protection compression ring border, is cooled to room temperature, obtains the described Graphene with vesicular structure.
2. according to the preparation method of the Graphene with vesicular structure described in claim 1, it is characterized in that, in step 1, described reductive agent is at least one in hydrazine, sodium borohydride, POTASSIUM BOROHYDRIDE and Trisodium Citrate.
3. according to the preparation method of the Graphene with vesicular structure described in claim 1, it is characterized in that, in step 1, described pore-forming material is sodium bicarbonate or saleratus.
4. according to the preparation method of the Graphene with vesicular structure described in claim 1, it is characterized in that, in step 1, the blending means of described graphite oxide, described reductive agent, described pore-forming material and described deionized water is ultrasonic mixing 30 minutes ~ 60 minutes.
5. according to the preparation method of the Graphene with vesicular structure described in claim 1, it is characterized in that, after step 2, also comprise the step that the product after described reduction reaction is filtered and cleans.
6. according to the preparation method of the Graphene with vesicular structure described in claim 1, it is characterized in that, in step 3, described protection gas is at least one in hydrogen, argon gas and nitrogen.
7. according to the preparation method of the Graphene with vesicular structure described in claim 1, it is characterized in that, in step 3, the cooling speed of the product after described insulation reaction in described protection compression ring border is 30 ℃/min～50 ℃/min.
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| CN106395802A (en) * | 2016-09-08 | 2017-02-15 | 山东理工大学 | Method for preparing graphene porous membrane |
| CN108584927A (en) * | 2018-05-24 | 2018-09-28 | 浙江农业商贸职业学院 | A kind of preparation method of porous graphene powder for automotive alloys material |
| CN114497513A (en) * | 2022-03-05 | 2022-05-13 | 青岛泰达华润新能源科技有限公司 | Graphene negative electrode material for lithium ion battery and preparation method thereof |
| US11450487B2 (en) | 2016-07-15 | 2022-09-20 | Nanotek Instruments Group, Llc | Humic acid-based supercapacitors |
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