CN105417531A - Method for preparing graphite at ultra-low temperature - Google Patents
Method for preparing graphite at ultra-low temperature Download PDFInfo
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- CN105417531A CN105417531A CN201510963367.8A CN201510963367A CN105417531A CN 105417531 A CN105417531 A CN 105417531A CN 201510963367 A CN201510963367 A CN 201510963367A CN 105417531 A CN105417531 A CN 105417531A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
Abstract
The invention relates to a method for preparing graphite at ultra-low temperature, and belongs to the technical field of expanded graphite. The method for preparing the expanded graphite at the ultra-low temperature is characterized in that a technical process for preparing the expanded graphite at the ultra-low temperature comprises the steps of soaking wet graphite oxide in an aqueous solution of non-volatile acid, and performing acid treatment; separating acidulated graphite oxide from an acid solution; performing heat treatment on the wet and acidulated graphite oxide under the ultra-low temperature of 50 to 110 DEG C to directly obtain a preliminary product, washing, and purifying to obtain the expended graphite. The method provided by the invention has the advantages that the process is simple, the operation is convenient, the production cost is lowered while the production efficiency is improved, and the like, and the method is extremely suitable for large scale production of the expanded graphite.
Description
Technical field
The invention belongs to expanded graphite technical field, particularly relate to a kind of method that very low temperature prepares expanded graphite.
Background technology
At present, graphite raw material is a kind of laminate structure, and the bonding force of interlayer is very weak, approximately only has 17KJ/mol.Space between the carbon atomic layer of graphite, the basic metal that easy insertion ionization energy is little and the large halogen of electron affinity energy, halogenide and acid etc., thus form compound between graphite layers (GICs), under GICs is placed in high temperature, the instantaneous vaporization of graphite layers inset produces thrust, graphite linings and layer are pushed open, macroscopically produces expansion, namely expansible black lead becomes expanded graphite.
Expanded graphite is a kind of loose porous vermiform material obtained through intercalation processing, washing, drying, high temperature puffing by natural flake graphite, is also worm graphite.And expanded graphite has following character: 1. possess the good characteristics such as heat-resisting, corrosion-resistant, the self-lubricating of natural graphite itself.2. also possessed the light soft that natural graphite does not possess, compressible, rebound resilience.3. pore structure is very abundant.Owing to having so unique character, thus it is made to have unique Application Areas: sealing material; Matrix material; Battery electrode material; Environment-friendly materials; Catalyzer; . graphite wave-absorbing and camouflage material; Biolith ink material is applied.
Wherein the primary process of the heat treating process of graphite oxide is: be raw material with graphite, utilizes Hummer method to carry out intercalation oxidation and obtains graphite oxide; Then under certain condition, graphite oxide is heat-treated, finally obtain expanded graphite.The representational work of most comprises: CN1239071A; CN1191196; JMaterSci2014,49,4989-4997; ACSNano, 2009,3,3730-3736; JMaterChem2011,21,5392-5397; JMaterChem2010,20,8467-8469; JMaterChemC, 2013,1,50-53; USPat.Pending, Ser.No.2013/0197256A1 (Aug.1,2013).This processing method thermal treatment temp is higher, and generally at 120-1100 DEG C, this constrains the large-scale production of expanded graphite to a certain extent.
Summary of the invention
The present invention provides a kind of very low temperature to prepare the method for expanded graphite for solving in known technology the technical problem that exists.
The object of this invention is to provide one and have technique simply, easy to operate, while enhancing productivity, can reduce production cost, the very low temperature being suitable for the features such as the large-scale production of expanded graphite prepares the method for expanded graphite.
The maximum difference of the present invention and traditional technology is that thermal treatment temp is extremely low, is 50-110 DEG C, greatly reduces energy expenditure, equipment requirements, working conditions etc., and therefore this technique is very suitable for the fairly large production of expanded graphite.
The graphite oxide of hygrometric state (not dry) soaks by the present invention in non-volatile aqueous acid, thus carry out acidification, the graphite oxide of acidifying is separated with acid solution, by hygrometric state and the graphite oxide of acidifying directly obtains preliminary product under the condition of ultralow temperature of 50-110 DEG C after Overheating Treatment, after washing, purifying, obtain expanded graphite.
The technical scheme that the method that very low temperature of the present invention prepares expanded graphite is taked is:
Very low temperature prepares a method for expanded graphite, is characterized in: the technological process that very low temperature prepares expanded graphite is that hygrometric state graphite oxide soaks in non-volatile aqueous acid, carries out acidification; The graphite oxide of acidifying is separated with acid solution; By hygrometric state and the graphite oxide of acidifying directly obtains preliminary product under the condition of ultralow temperature of 50-110 DEG C after Overheating Treatment, after washing, purifying, obtain expanded graphite.
The method that very low temperature of the present invention prepares expanded graphite can also adopt following technical scheme:
Described very low temperature prepares the method for expanded graphite, is characterized in: graphite oxide is for having graphite laminate structural carbon material.
Described very low temperature prepares the method for expanded graphite, is characterized in: graphite laminate structural carbon material is synthetic graphite, natural graphite, crystalline flake graphite, graphite nano micro-flake.
Described very low temperature prepares the method for expanded graphite, is characterized in: non-volatile acid is sulfuric acid, perchloric acid, hypochlorous acid, permanganic acid, phosphoric acid; The mass percent concentration of aqueous acid is 3%-50%.
The advantage that the present invention has and positively effect are:
Very low temperature prepares the method for expanded graphite owing to have employed the brand-new technical scheme of the present invention, and compared with prior art, thermal expansion condition adjusts extremely gentle by technique of the present invention, obtains amorphous expanded graphite meterial.While enhancing productivity, reduce production cost, be very suitable for the large-scale production of expanded graphite.
Accompanying drawing explanation
Fig. 1 is the XRD test curve that embodiment 1 obtains expanded graphite;
Fig. 2 is the SEM photo that embodiment 1 obtains expanded graphite;
Fig. 3 is the nitrogen suction/desorption curve (its specific surface area included) that embodiment 1 obtains expanded graphite.
Embodiment
For summary of the invention of the present invention, Characteristic can be understood further, hereby exemplify following examples, and coordinate accompanying drawing to be described in detail as follows:
Accompanying drawings 1, Fig. 2 and Fig. 3.
Embodiment 1
Very low temperature prepares a method for expanded graphite, take crystalline flake graphite as raw material, utilizes Hummers method to obtain graphite oxide.The graphite oxide of hygrometric state (not dry) is soaked in sulphur aqueous acid (concentration 3%), thus carry out acidification, the graphite oxide of acidifying is separated with acid solution, by hygrometric state and the graphite oxide of acidifying directly obtains preliminary product under the condition of ultralow temperature of 70 DEG C after Overheating Treatment, after washing, purifying, obtain expanded graphite.
Embodiment 2
Very low temperature prepares a method for expanded graphite, take synthetic graphite as raw material, utilizes Hummers method to obtain graphite oxide.The graphite oxide of hygrometric state (not dry) is soaked in sulphur aqueous acid (concentration 50%), thus carry out acidification, the graphite oxide of acidifying is separated with acid solution, by hygrometric state and the graphite oxide of acidifying directly obtains preliminary product under the condition of ultralow temperature of 50 DEG C after Overheating Treatment, after washing, purifying, obtain expanded graphite.
Embodiment 3
Very low temperature prepares a method for expanded graphite, take natural graphite as raw material, utilizes Hummers method to obtain graphite oxide.The graphite oxide of hygrometric state (not dry) is soaked in the aqueous solution (concentration 10%) of perchloric acid, thus carry out acidification, the graphite oxide of acidifying is separated with acid solution, by hygrometric state and the graphite oxide of acidifying directly obtains preliminary product under the condition of ultralow temperature of 110 DEG C after Overheating Treatment, after washing, purifying, obtain expanded graphite.
Embodiment 4
Very low temperature prepares a method for expanded graphite, take graphite nano micro-flake as raw material, utilizes Hummers method to obtain graphite oxide.The graphite oxide of hygrometric state (not dry) is soaked in the hypochlorous aqueous solution (concentration 10%), thus carry out acidification, the graphite oxide of acidifying is separated with acid solution, by hygrometric state and the graphite oxide of acidifying directly obtains preliminary product under the condition of ultralow temperature of 90 DEG C after Overheating Treatment, after washing, purifying, obtain expanded graphite.
Embodiment 5
Very low temperature prepares a method for expanded graphite, take crystalline flake graphite as raw material, utilizes Hummers method to obtain graphite oxide.The graphite oxide of hygrometric state (not dry) is soaked in the aqueous solution (concentration 10%) of permanganic acid, thus carry out acidification, the graphite oxide of acidifying is separated with acid solution, by hygrometric state and the graphite oxide of acidifying directly obtains preliminary product under the condition of ultralow temperature of 60 DEG C after Overheating Treatment, after washing, purifying, obtain expanded graphite.
Embodiment 6
Very low temperature prepares a method for expanded graphite, take natural graphite as raw material, utilizes Hummers method to obtain graphite oxide.The graphite oxide of hygrometric state (not dry) is soaked in phosphorus aqueous acid (concentration 5%), thus carry out acidification, the graphite oxide of acidifying is separated with acid solution, by hygrometric state and the graphite oxide of acidifying directly obtains preliminary product under the condition of ultralow temperature of 100 DEG C after Overheating Treatment, after washing, purifying, obtain expanded graphite.
Comparative embodiment
Comparative example 1
After graphite oxide washes clean will be obtained; air dry oven is utilized to carry out drying at 100 DEG C to sample; make sample fully dry; again graphite oxide powder pure for 0.2g is placed in tube furnace; tube furnace is carried out hydrogen shield, at 350 DEG C, carries out expansion process, thus make graphite oxide and hydrogen carry out vigorous reaction; and make it to expand, obtain expanded graphite.
This technique, then needs hydrogen environment in the preparation of expanded graphite and temperature is higher, thus makes graphite oxide and hydrogen generation intense reaction to realize the expansion of graphite oxide, therefore, amplifies more dangerous, need specific equipment by technique.
Comparative example 2
After graphite oxide washes clean will be obtained, air dry oven is utilized to carry out drying at 100 DEG C to sample, make sample fully dry, under an inert atmosphere pure graphite oxide powder is expanded at 1100 DEG C, thus make graphite oxide and hydrogen carry out vigorous reaction, and make it to expand, obtain expanded graphite.
This technique, in the preparation of expanded graphite, temperature is very high, therefore, amplifies more dangerous, need specific equipment by technique.
Claims (4)
1. very low temperature prepares a method for expanded graphite, it is characterized in that: the technological process that very low temperature prepares expanded graphite is that hygrometric state graphite oxide soaks in non-volatile aqueous acid, carries out acidification; The graphite oxide of acidifying is separated with acid solution; By hygrometric state and the graphite oxide of acidifying directly obtains preliminary product under the condition of ultralow temperature of 50-110 DEG C after Overheating Treatment, after washing, purifying, obtain expanded graphite.
2. very low temperature according to claim 1 prepares the method for expanded graphite, it is characterized in that: graphite oxide is for having graphite laminate structural carbon material.
3. very low temperature according to claim 2 prepares the method for expanded graphite, it is characterized in that: graphite laminate structural carbon material is synthetic graphite, natural graphite, crystalline flake graphite, graphite nano micro-flake.
4. very low temperature according to claim 1 prepares the method for expanded graphite, it is characterized in that: non-volatile acid is sulfuric acid, perchloric acid, hypochlorous acid, permanganic acid, phosphoric acid; The mass percent concentration of aqueous acid is 3%-50%.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102126719A (en) * | 2010-01-14 | 2011-07-20 | 河北农业大学 | Preparation method of expandable graphite with low starting expansion temperature |
| CN102424382A (en) * | 2011-09-16 | 2012-04-25 | 中国科学院宁波材料技术与工程研究所 | Method for preparing high-specific-surface-area graphene under conditions of normal pressure and low temperature |
| CN103449424A (en) * | 2012-08-28 | 2013-12-18 | 武汉大学 | Low temperature preparation method of graphene and graphene-based composite material |
| CN104512881A (en) * | 2013-09-27 | 2015-04-15 | 青岛市首胜实业有限公司 | Preparation technology of expandable graphite utilizing secondary inserting method |
| US9067794B1 (en) * | 2008-08-06 | 2015-06-30 | The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Adminstration | Highly thermal conductive nanocomposites |
-
2015
- 2015-12-17 CN CN201510963367.8A patent/CN105417531A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9067794B1 (en) * | 2008-08-06 | 2015-06-30 | The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Adminstration | Highly thermal conductive nanocomposites |
| CN102126719A (en) * | 2010-01-14 | 2011-07-20 | 河北农业大学 | Preparation method of expandable graphite with low starting expansion temperature |
| CN102424382A (en) * | 2011-09-16 | 2012-04-25 | 中国科学院宁波材料技术与工程研究所 | Method for preparing high-specific-surface-area graphene under conditions of normal pressure and low temperature |
| CN103449424A (en) * | 2012-08-28 | 2013-12-18 | 武汉大学 | Low temperature preparation method of graphene and graphene-based composite material |
| CN104512881A (en) * | 2013-09-27 | 2015-04-15 | 青岛市首胜实业有限公司 | Preparation technology of expandable graphite utilizing secondary inserting method |
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| 魏兴海 等: "HClO4-GIC的制备及其柔性石墨的性能", 《新型碳材料》 * |
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Application publication date: 20160323 |