CN107265445A - A kind of green high-efficient of high-quality graphene prepares method - Google Patents
A kind of green high-efficient of high-quality graphene prepares method Download PDFInfo
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- CN107265445A CN107265445A CN201710545843.3A CN201710545843A CN107265445A CN 107265445 A CN107265445 A CN 107265445A CN 201710545843 A CN201710545843 A CN 201710545843A CN 107265445 A CN107265445 A CN 107265445A
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Abstract
The present invention provides a kind of green high-efficient preparation method of high-quality graphene.Mainly comprise the following steps that：1. pair graphite powder carries out thermal expansion processing expanded graphite is made.2. the same methyl pyrrolidone of obtained expanded graphite (NMP) reagent is mixed, addition sodium taurocholate is as surfactant, then is placed in progress high speed shear processing under the high-speed emulsifying machine of laboratory.Raw material after shearing is collected by centrifugal filtration.The technological process is simple to operation, process stabilization is with low cost, and batch preparation can be carried out in a short time, the scheme of graphene is prepared there is provided a kind of efficient stable, the product graphene sheet layer structural integrity, with preferable electric conductivity, and preparation process is not added with the environmental contaminants such as soda acid, has broad application prospects in the green preparation field of graphene.
Description
Technical field
The present invention relates to the preparation technology that green high-efficient rate prepares high-quality graphene, belong to materials chemistry technology of preparing neck
Domain.
Background technology
Graphene is a kind of new carbon nanomaterial, with by the tightly packed bi-dimensional cellular shape of single layer of carbon atom
Crystal structure, perfect lattice structure makes it have excellent and unique mechanics, optically and thermally electricity, characteristic, including hyperpyrexia
The electron mobility of conductance, at room temperature superelevation, high theoretical specific surface area etc., make the quantum devices such as its scene effect transistor, collection
Potentiality are had a wide range of applications in terms of into circuit, functional composite material, energy storage material, catalyst carrier.In graphene
In science and education research work, prepared by the high-volume of the graphene raw material of topmost restraining factors, high-quality macroscopic view.Current laboratory
The main preparation methods of middle graphene have oxidation-reduction method and chemical vapour deposition technique.Two kinds of preparation methods have respective advantage
And shortcoming.
It is to be peeled off graphene using oxidant mode of intercalation between graphite that oxidation-reduction method, which prepares graphene, its advantage
It is that can prepare graphene on a large scale in laboratory scope, but the graphene defect that this method is prepared is more, to stone
The performances such as electricity, the calorifics of black alkene have than more serious restriction.In addition, needing to use strong acid and poisonous reduction in preparation process
Agent, therefore environmental pressure is heavier.Process for preparing graphenes by chemical vapour deposition is then to deposit the small molecule of carbon on tinsel
So as to prepare single-layer graphene.Its advantage is that the graphene defect prepared is few, better performances, but graphite prepared by single
Alkene amount is seldom, and single preparation time is longer, and efficiency is low, and cost is high.Therefore find it is a kind of it is new, can be while taking into account high-quality
The method that amount, efficient and green prepare graphene is particularly important for the research and application of graphene.
It is that the graphene that newly rises recent years prepares method that liquid phase method, which prepares graphene, be characterized in using liquid phase substance as
Medium, is acted on to generate graphene by carrying out mechanical force, chemical reaction etc. to graphite.It is at present to use supercritical ultrasonics technology more, with super
Sound wave effect carries out local high energy concussion to graphite and prepares graphene to peel off.Can be in lower energy using mechanical shear stress
Consumption is lower to carry out graphene preparation, more meets the requirement of energy-conserving and environment-protective instantly.
The present invention is using methyl pyrrolidone (NMP) reagent as phase is prepared, and sodium taurocholate is surface catalyst, by a high speed
The graphite progress high speed shear of expansion process is handled to prepare graphene in laboratory homomixer.It is efficient, green there is provided one kind
Color prepares the new way of high-quality graphene.
The content of the invention
Technical problem：The invention provides a kind of green high-efficient preparation method of high-quality graphene.This method by
High speed shear processing is carried out in reagent to thermal expansion graphite shearing graphene is made.This method cost is low, simple to operate, effect
Rate is high, can largely prepare, and preparation process does not have the addition of the chemical reagent such as soda acid, beneficial to environmental protection.It is super with common liquid phase
Sound stripping method prepares graphene and compared, and the shearing preparation power consumption low and cycle is short, is more suitable for the preparation of mass industrial production.
Technical scheme：A kind of green high-efficient preparation method of high-quality graphene of the present invention is walked including following technique
Suddenly：
A. expanded graphite is prepared：Graphite powder is placed in ceramic crucible, high-temperature heat treatment is carried out to it, room temperature is cooled to i.e.
It can obtain thermal expansion graphite powder；
B. shearing method prepares graphene：Obtained thermal expansion graphite powder is dissolved in into methyl pyrrole with cholic acid natrium surfactant
In pyrrolidone NMP reagents, shear treatment is carried out to it under high-speed emulsifying machine；
C. removal and the sample cleanup of reagent are sheared：
1) sample reagent after shearing is filtered by vacuum, to remove reagent；
2) by step 1) in filtered material take out, centrifugal treating is to obtain purified product.
Wherein：
Described high-temperature heat treatment, its treatment temperature is 900 DEG C -1100 DEG C.
Described high-temperature heat treatment, its processing time is 15-30 minutes.
The rotating speed of described high-speed emulsifying machine shear treatment is 10000-16000rpm.
Described shear treatment, processing time is 1-5h.
Described thermal expansion graphite powder, cholic acid natrium surfactant, the ratio of methyl pyrrolidone NMP reagents are：(20-
30):1:(7000-8000)。
Described is filtered by vacuum to the sample reagent after shearing, and the number of times of suction filtration is more than 3 times.
Described centrifugal treating, the rotating speed of centrifuge is 5000-10000rpm.
Beneficial effect：Using the inventive method, low layer high-quality graphene, operation letter can efficiently, be stably prepared
It is single, and preparation process does not have the participation of the hazardous chemicals such as soda acid, and mass green production can be achieved and prepares.With common liquid
Mutually ultrasonic stripping method is compared, and innovative point of the invention is directly to use mechanical force to carry out shear treatment to graphite sample, prepares
It is simpler and consume energy relatively low.
Embodiment
Embodiment 1：
(1) prepares thermal expansion graphite powder：5-10g graphite powders are placed in ceramic crucible, in 950 DEG C of high temperature furnaces at heat
Reason 15-20 minutes, is cooled to room temperature.
(2) shearing methods prepare graphene：In the 1500-2500ml methyl pyrrolidones dissolved with 0.2-0.4g sodium taurocholates
(NMP) obtained thermal expansion graphite is dissolved in reagent, and 10000- is carried out to it using laboratory high-speed emulsifying machine
Stop shearing after 16000rpm shear treatment, 3-5h.
(3) reagents are removed：The sample reagent that step (2) is obtained is positioned over suction filtration 4-5 times repeatedly in suction filtration machine.
(4) takes out filtered material in step (3), and 4-6 times is centrifuged under the conditions of 7500-10000rpm and be can obtain
Purified product.
Embodiment 2：
(1) prepares thermal expansion graphite powder：2.5-7.5g graphite powders are placed in ceramic crucible, it is hot in 950 DEG C of high temperature furnaces
Processing 15-20 minutes, is cooled to room temperature..
(2) shearing methods prepare graphene：In the 750-2250ml methyl pyrrolidones dissolved with 0.1-0.3g sodium taurocholates
(NMP) obtained thermal expansion graphite is dissolved in reagent, and 13000- is carried out to it using laboratory high-speed emulsifying machine
16000rpm shear treatment, continues 2-4h.
(3) reagents are removed：The sample reagent that step (2) is obtained is positioned over suction filtration 3-5 times repeatedly in suction filtration machine.
(4) takes out filtered material in step (3), and being centrifuged 3-4 times under the conditions of 7000-10000rpm to obtain
To purified product.
Embodiment 3：
(1) prepares thermal expansion graphite powder：5-7.5g graphite powders are placed in ceramic crucible, in 950 DEG C of high temperature furnaces at heat
Reason 15-20 minutes, is cooled to room temperature.
(2) shearing methods prepare graphene：In the 1500-2250ml methyl pyrrolidones dissolved with 0.3-0.6g sodium taurocholates
(NMP) obtained thermal expansion graphite is dissolved in reagent, and 13000- is carried out to it using laboratory high-speed emulsifying machine
16000rpm shear treatment, continues 1-3h.
(3) reagents are removed：The sample reagent that step (2) is obtained is positioned over suction filtration 3-5 times repeatedly in suction filtration machine.
(4) takes out filtered material in step (3), and being centrifuged 3-4 times under the conditions of 8000-10000rpm to obtain
To purified product.
Embodiment 4：
(1) prepares thermal expansion graphite powder：10-10g graphite powders are placed in ceramic crucible, in 950 DEG C of high temperature furnaces at heat
Reason 15-20 minutes, is cooled to room temperature.
(2) shearing methods prepare graphene：In the 3000-5000ml methyl pyrrolidones dissolved with 0.4-0.8g sodium taurocholates
(NMP) obtained thermal expansion graphite is dissolved in reagent, and 14000- is carried out to it using laboratory high-speed emulsifying machine
17000rpm shear treatment, continues 2-5h.
(3) reagents are removed：The sample reagent that step (2) is obtained is positioned over suction filtration 3-5 times repeatedly in suction filtration machine.
(4) takes out filtered material in step (3), and being centrifuged 4-6 times under the conditions of 6000-10000rpm to obtain
To purified product.
Claims (8)
1. the green high-efficient preparation method of a kind of high-quality graphene, it is characterised in that this method comprises the following steps：
A. expanded graphite is prepared：Graphite powder is placed in ceramic crucible, high-temperature heat treatment is carried out to it, being cooled to room temperature can obtain
To thermal expansion graphite powder；
B. shearing method prepares graphene：Obtained thermal expansion graphite powder is dissolved in into crassitude with cholic acid natrium surfactant
In ketone NMP reagents, shear treatment is carried out to it under high-speed emulsifying machine；
C. removal and the sample cleanup of reagent are sheared：
1) sample reagent after shearing is filtered by vacuum, to remove reagent；
2) by step 1) in filtered material take out, centrifugal treating is to obtain purified product.
2. the green high-efficient preparation method of high-quality graphene according to claim 1, it is characterised in that described high temperature
Heat treatment, its treatment temperature is 900 DEG C -1100 DEG C.
3. the green high-efficient preparation method of high-quality graphene according to claim 1 or 2, it is characterised in that described
High-temperature heat treatment, its processing time is 15-30 minutes.
4. the green high-efficient preparation method of high-quality graphene according to claim 1, it is characterised in that described high speed
The rotating speed of mulser shear treatment is 10000-16000rpm.
5. the green high-efficient preparation method of the high-quality graphene according to claim 1 or 4, it is characterised in that described
Shear treatment, processing time is 1-5h.
6. the green high-efficient preparation method of high-quality graphene according to claim 1, it is characterised in that described is hot swollen
Swollen graphite powder, cholic acid natrium surfactant, the ratio of methyl pyrrolidone NMP reagents are：(20-30):1:(7000-8000).
7. the green high-efficient preparation method of high-quality graphene according to claim 1, it is characterised in that described to cutting
Sample reagent after cutting is filtered by vacuum, and the number of times of suction filtration is more than 3 times.
8. the green high-efficient preparation method of high-quality graphene according to claim 1, it is characterised in that described centrifugation
Processing, the rotating speed of centrifuge is 5000-10000rpm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108862259A (en) * | 2018-08-13 | 2018-11-23 | 深圳天元羲王材料科技有限公司 | A kind of graphene production method and device |
| CN110042284A (en) * | 2019-05-08 | 2019-07-23 | 东南大学 | A kind of preparation method of high-strength aluminum alloy |
| CN113371699A (en) * | 2020-03-09 | 2021-09-10 | 中国科学院上海硅酸盐研究所 | Green method for preparing high-quality graphene powder in large scale and at ultralow cost |
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| CN105585004A (en) * | 2014-10-24 | 2016-05-18 | 江阴碳谷科技有限公司 | A production device of graphene and a preparing method |
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| CN104059616A (en) * | 2014-06-26 | 2014-09-24 | 燕山大学 | Solid-liquid phase change heat exchange working medium for power generation by oceanic thermal energy and preparation method of working medium |
| CN105585004A (en) * | 2014-10-24 | 2016-05-18 | 江阴碳谷科技有限公司 | A production device of graphene and a preparing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108862259A (en) * | 2018-08-13 | 2018-11-23 | 深圳天元羲王材料科技有限公司 | A kind of graphene production method and device |
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| CN110042284A (en) * | 2019-05-08 | 2019-07-23 | 东南大学 | A kind of preparation method of high-strength aluminum alloy |
| CN113371699A (en) * | 2020-03-09 | 2021-09-10 | 中国科学院上海硅酸盐研究所 | Green method for preparing high-quality graphene powder in large scale and at ultralow cost |
| CN113371699B (en) * | 2020-03-09 | 2024-02-06 | 中国科学院上海硅酸盐研究所 | Green method for preparing high-quality graphene powder in large scale and ultra-low cost |
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Application publication date: 20171020 |