CN108083273A - A kind of heat safe graphite material and preparation method thereof - Google Patents
A kind of heat safe graphite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of heat safe graphite material and preparation method thereof, during preparation, by graphite according to solid-to-liquid ratio 1g:4 6mL ratios add in the glycollic acid solution of 2 3mol/L, are heated to 80 DEG C, 80 90min of constant temperature, and mixture A is made；Ethyl orthosilicate and aminopropyl trimethoxysilane are added in mixture A, 65 75 DEG C of 0.8 1.2h of reaction is heated, filters, is washed to neutrality, vacuum drying obtains mixture B；Made mixture B is placed in hydrazine hydrate alcoholic solution, hydro-thermal reaction is carried out after stirring and evenly mixing, 1.5 1.8h are reacted at a temperature of 70 80 DEG C, is filtered, is washed to neutrality, vacuum drying puffing obtains graphite material.The present invention is the graphite material for handling graphite by glycolic, ethyl orthosilicate, aminopropyl trimethoxysilane, hydrazine hydrate, thermal weight loss is lower, with high high temperature resistance, service life is just grown, improve tensile strength, and puffing volume can be increased, many reprocessing processes are saved, reduce cost.
Description
Technical field
The present invention relates to graphite technology fields, are specifically a kind of heat safe graphite material and preparation method thereof.
Background technology
Graphite is a kind of allotrope of elemental carbon, and the periphery of each carbon atom links the other three carbon atom（Row
Row mode is in cellular multiple hexagons）With Covalent bonding together, covalent molecule is formed.Expanded graphite (Expanded
Graphite, abbreviation EG) be obtained by natural graphite scale through intercalation, washing, drying, high temperature puffing it is a kind of loose porous
Vermiform substance.EG also has in addition to possessing the excellent performances such as cold-hot, the corrosion-resistant, self-lubricating of native graphite in itself
The spies such as the unexistent softness of native graphite, compression resilience, adsorptivity, ecological environment harmony, biocompatibility, radiation resistance
Property.With the development of material science, the sealing material of high-temperature field is also required to make constant progress.In common hot environment
In, such as 200 DEG C or so, due to the bad mechanical strength of flexible graphite material, its application is affected, and in the higher ring of temperature
In border, flexible graphite material will oxidation weight loss, lose the sealing characteristics of compression resilience and stress relaxation rate.It is moreover, existing
Flexible graphite material i.e. allow to avoid above-mentioned deficiency and to carrying out further it on the basis of flexible graphite material
Improvement, process is complicated, adds cost.
The content of the invention
It is an object of the invention to provide a kind of heat safe graphite material and preparation method thereof, to solve above-mentioned background skill
The problem of being proposed in art.
To achieve the above object, the present invention provides following technical solution.
A kind of preparation method of heat safe graphite material, comprises the following steps.
1）By graphite according to solid-to-liquid ratio 1g:4-6mL ratios add in the glycollic acid solution of 2-3mol/L, are heated to 80 DEG C, perseverance
Mixture A is made in warm 80-90min.
2）Ethyl orthosilicate and aminopropyl trimethoxysilane are added in mixture A, heat 65-75 DEG C of reaction 0.8-
1.2h after the completion of reaction, filters, washs to neutrality, mixture B is obtained after being dried in vacuo 10-12h at 60 DEG C.
3）Made mixture B is placed in hydrazine hydrate alcoholic solution, hydro-thermal reaction, 70-80 DEG C of temperature are carried out after stirring and evenly mixing
Lower reaction 1.5-1.8h after the completion of reaction, is filtered, washed to neutrality, puffing after vacuum drying 10-12h at 60 DEG C to obtain stone
Ink material.
As further embodiment of the present invention：Step 1）In, by graphite according to solid-to-liquid ratio 1g:5mL ratios add in 2-3mol/
The glycollic acid solution of L.
As further embodiment of the present invention：Step 1）In, the concentration of glycollic acid solution is 2.5mol/L.
As further embodiment of the present invention：The mass ratio of ethyl orthosilicate, aminopropyl trimethoxysilane and graphite is
2-3:1:3-5。
As further embodiment of the present invention：The mass ratio of hydrazine hydrate alcoholic solution and graphite is 5-7:1.
As further embodiment of the present invention：Step 2）In, heat 70 DEG C of reaction 1h.
As further embodiment of the present invention：Step 3）In, hydro-thermal reaction is to react 1.6h at a temperature of 75 DEG C.
As further embodiment of the present invention：Step 3）In, the mass ratio of hydrazine hydrate and alcohol is 1 in hydrazine hydrate alcoholic solution:
0.8-1.5。
As further embodiment of the present invention：Graphite uses crystalline flake graphite.
Another object of the present invention provides the graphite material according to made from the above method.
Compared with prior art, the beneficial effects of the invention are as follows.
The present invention is the stone for handling graphite by glycolic, ethyl orthosilicate, aminopropyl trimethoxysilane, hydrazine hydrate
Ink material, thermal weight loss is lower, has high high temperature resistance, and service life is just grown, and improves tensile strength, and can increase swollen
Change volume, the low graphite material of high temperature resistant, high intensity, thermal weight loss is directly made in graphite by benzene invention after various reagents are handled,
Many reprocessing processes are saved, reduce cost.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical solution in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, those of ordinary skill in the art's all other embodiments obtained without making creative work, all
Belong to the scope of protection of the invention.
Embodiment 1.
In the embodiment of the present invention, a kind of preparation method of heat safe graphite material comprises the following steps.
1）By crystalline flake graphite according to solid-to-liquid ratio 1g:4mL ratios add in the glycollic acid solution of 2mol/L, are heated to 80 DEG C, perseverance
Mixture A is made in warm 80min.
2）Ethyl orthosilicate and aminopropyl trimethoxysilane are added in mixture A, heat 65 DEG C of reaction 0.8h, instead
It after the completion of answering, filters, washs to neutrality, mixture B is obtained after being dried in vacuo 10h at 60 DEG C；Ethyl orthosilicate, aminopropyl three
The mass ratio of methoxy silane and crystalline flake graphite is 2:1:3.
3）Made mixture B is placed in hydrazine hydrate alcoholic solution, carries out hydro-thermal reaction after stirring and evenly mixing, it is anti-at a temperature of 70 DEG C
1.5h is answered, after the completion of reaction, filters, washs to neutrality, it is puffing after vacuum drying 10h at 60 DEG C to obtain graphite material；Hydration
The mass ratio of hydrazine alcoholic solution and crystalline flake graphite is 5:1.The mass ratio of hydrazine hydrate and alcohol is 1 in hydrazine hydrate alcoholic solution:0.8.
Embodiment 2.
In the embodiment of the present invention, a kind of preparation method of heat safe graphite material comprises the following steps.
1）By crystalline flake graphite according to solid-to-liquid ratio 1g:6mL ratios add in the glycollic acid solution of 3mol/L, are heated to 80 DEG C, perseverance
Mixture A is made in warm 90min.
2）Ethyl orthosilicate and aminopropyl trimethoxysilane are added in mixture A, heat 75 DEG C of reaction 1.2h, instead
It after the completion of answering, filters, washs to neutrality, mixture B is obtained after being dried in vacuo 12h at 60 DEG C；Ethyl orthosilicate, aminopropyl three
The mass ratio of methoxy silane and crystalline flake graphite is 3:1:5.
3）Made mixture B is placed in hydrazine hydrate alcoholic solution, carries out hydro-thermal reaction after stirring and evenly mixing, it is anti-at a temperature of 80 DEG C
1.8h is answered, after the completion of reaction, filters, washs to neutrality, it is puffing after vacuum drying 12h at 60 DEG C to obtain graphite material；Hydration
The mass ratio of hydrazine alcoholic solution and crystalline flake graphite is 7:1.The mass ratio of hydrazine hydrate and alcohol is 1 in hydrazine hydrate alcoholic solution:1.5.
Embodiment 3.
In the embodiment of the present invention, a kind of preparation method of heat safe graphite material comprises the following steps.
1）By crystalline flake graphite according to solid-to-liquid ratio 1g:5mL ratios add in the glycollic acid solution of 2.5mol/L, are heated to 80 DEG C,
Mixture A is made in constant temperature 80min.
2）Ethyl orthosilicate and aminopropyl trimethoxysilane are added in mixture A, heat 70 DEG C of reaction 1h, reaction
After finishing, filter, wash to neutrality, mixture B is obtained after being dried in vacuo 10h at 60 DEG C；Ethyl orthosilicate, aminopropyl front three
The mass ratio of oxysilane and crystalline flake graphite is 2:1:3.
3）Made mixture B is placed in hydrazine hydrate alcoholic solution, carries out hydro-thermal reaction after stirring and evenly mixing, it is anti-at a temperature of 75 DEG C
1.6h is answered, after the completion of reaction, filters, washs to neutrality, it is puffing after vacuum drying 10h at 60 DEG C to obtain graphite material；Hydration
The mass ratio of hydrazine alcoholic solution and crystalline flake graphite is 5:1.The mass ratio of hydrazine hydrate and alcohol is 1 in hydrazine hydrate alcoholic solution:0.8.
Embodiment 4.
In the embodiment of the present invention, a kind of preparation method of heat safe graphite material comprises the following steps.
1）By crystalline flake graphite according to solid-to-liquid ratio 1g:5mL ratios add in the glycollic acid solution of 2.5mol/L, are heated to 80 DEG C,
Mixture A is made in constant temperature 90min.
2）Ethyl orthosilicate and aminopropyl trimethoxysilane are added in mixture A, heat 70 DEG C of reaction 1h, reaction
After finishing, filter, wash to neutrality, mixture B is obtained after being dried in vacuo 12h at 60 DEG C；Ethyl orthosilicate, aminopropyl front three
The mass ratio of oxysilane and crystalline flake graphite is 3:1:5.
3）Made mixture B is placed in hydrazine hydrate alcoholic solution, carries out hydro-thermal reaction after stirring and evenly mixing, it is anti-at a temperature of 75 DEG C
1.6h is answered, after the completion of reaction, filters, washs to neutrality, it is puffing after vacuum drying 12h at 60 DEG C to obtain graphite material；Hydration
The mass ratio of hydrazine alcoholic solution and crystalline flake graphite is 7:1.The mass ratio of hydrazine hydrate and alcohol is 1 in hydrazine hydrate alcoholic solution:1.5.
Embodiment 5.
In the embodiment of the present invention, a kind of preparation method of heat safe graphite material comprises the following steps.
1）By crystalline flake graphite according to solid-to-liquid ratio 1g:5mL ratios add in the glycollic acid solution of 2.5mol/L, are heated to 80 DEG C,
Mixture A is made in constant temperature 85min.
2）Ethyl orthosilicate and aminopropyl trimethoxysilane are added in mixture A, heat 70 DEG C of reaction 1h, reaction
After finishing, filter, wash to neutrality, mixture B is obtained after being dried in vacuo 11h at 60 DEG C；Ethyl orthosilicate, aminopropyl front three
The mass ratio of oxysilane and crystalline flake graphite is 2.5:1:4.
3）Made mixture B is placed in hydrazine hydrate alcoholic solution, carries out hydro-thermal reaction after stirring and evenly mixing, it is anti-at a temperature of 75 DEG C
1.6h is answered, after the completion of reaction, filters, washs to neutrality, it is puffing after vacuum drying 11h at 60 DEG C to obtain graphite material；Hydration
The mass ratio of hydrazine alcoholic solution and crystalline flake graphite is 6:1.The mass ratio of hydrazine hydrate and alcohol is 1 in hydrazine hydrate alcoholic solution:1.2.
Graphite material made from embodiment 1-5 is tested into thermal weight loss by JBT/9141-7 1999, by JBT/9141-2
1999 tested for tensile strength survey allowance for expansion by GB 10698-89, and the data obtained is shown in Table 1.
Table 1.
| Allowance for expansion（ml/g） | Tensile strength（MPa） | 670 DEG C/4h loss on ignitions（%） | |
| Embodiment 1 | 200 | 5.15 | 10.3 |
| Embodiment 2 | 200 | 5.18 | 9.8 |
| Embodiment 3 | 210 | 5.30 | 5.4 |
| Embodiment 4 | 210 | 5.32 | 5.0 |
| Embodiment 5 | 210 | 5.35 | 4.6 |
As seen from the above table, by graphite by graphite material made from above-mentioned processing, allowance for expansion, which is stablized, to be improved, and is increased anti-
Tensile strength reduces loss on ignition.Embodiment 3-5 is more excellent, and embodiment 5 is optimal.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned exemplary embodiment, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Profit requirement rather than above description limit, it is intended that all by what is fallen within the meaning and scope of the equivalent requirements of the claims
Variation is included within the present invention.
Moreover, it will be appreciated that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
Using specification as an entirety, the technical solutions in each embodiment can also be properly combined, forms those skilled in the art
It is appreciated that other embodiment.
Claims (10)
1. a kind of preparation method of heat safe graphite material, which is characterized in that comprise the following steps：
1）By graphite according to solid-to-liquid ratio 1g:4-6mL ratios add in the glycollic acid solution of 2-3mol/L, are heated to 80 DEG C, constant temperature 80-
Mixture A is made in 90min；
2）Ethyl orthosilicate and aminopropyl trimethoxysilane are added in mixture A, heat 65-75 DEG C of reaction 0.8-
1.2h after the completion of reaction, filters, washs to neutrality, mixture B is obtained after being dried in vacuo 10-12h at 60 DEG C；
3）Made mixture B is placed in hydrazine hydrate alcoholic solution, carries out hydro-thermal reaction after stirring and evenly mixing, it is anti-at a temperature of 70-80 DEG C
1.5-1.8h is answered, after the completion of reaction, filters, washs to neutrality, it is puffing after vacuum drying 10-12h at 60 DEG C to obtain graphite material
Material.
2. the preparation method of heat safe graphite material according to claim 1, which is characterized in that step 1）In, by stone
Ink is according to solid-to-liquid ratio 1g:5mL ratios add in the glycollic acid solution of 2-3mol/L.
3. the preparation method of heat safe graphite material according to claim 1, which is characterized in that step 1）In, ethyl alcohol
The concentration of acid solution is 2.5mol/L.
4. the preparation method of heat safe graphite material according to claim 1, which is characterized in that ethyl orthosilicate, ammonia
The mass ratio of propyl trimethoxy silicane and graphite is 2-3:1:3-5.
5. the preparation method of heat safe graphite material according to claim 1, which is characterized in that hydrazine hydrate alcoholic solution with
The mass ratio of graphite is 5-7:1.
6. the preparation method of heat safe graphite material according to claim 1, which is characterized in that step 2）In, heating
70 DEG C of reaction 1h.
7. the preparation method of heat safe graphite material according to claim 1, which is characterized in that step 3）In, hydro-thermal
Reaction is to react 1.6h at a temperature of 75 DEG C.
8. the preparation method of heat safe graphite material according to claim 1, which is characterized in that step 3）In, hydration
The mass ratio of hydrazine hydrate and alcohol is 1 in hydrazine alcoholic solution:0.8-1.5.
9. the preparation method of heat safe graphite material according to claim 1, which is characterized in that graphite uses scale stone
Ink.
10. graphite material made from the method as described in claim 1-9 is any.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100740633B1 (en) * | 2005-12-22 | 2007-07-18 | 재단법인 포항산업과학연구원 | Method for preparing graphite coated with silica |
| CN102642830A (en) * | 2012-04-25 | 2012-08-22 | 南京大学 | Method for preparing graphene modified by silane coupling agent |
| CN106115671A (en) * | 2016-06-23 | 2016-11-16 | 常州第六元素材料科技股份有限公司 | A kind of preparation method of alkylation modification Graphene |
-
2017
- 2017-09-29 CN CN201710907808.1A patent/CN108083273A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100740633B1 (en) * | 2005-12-22 | 2007-07-18 | 재단법인 포항산업과학연구원 | Method for preparing graphite coated with silica |
| CN102642830A (en) * | 2012-04-25 | 2012-08-22 | 南京大学 | Method for preparing graphene modified by silane coupling agent |
| CN106115671A (en) * | 2016-06-23 | 2016-11-16 | 常州第六元素材料科技股份有限公司 | A kind of preparation method of alkylation modification Graphene |
Non-Patent Citations (4)
| Title |
|---|
| TSUNG-CHIH WU ET AL: ""Synthesis, characterization, and properties of silane-functionalized expandable graphite composites"", 《JOURNAL OF COMPOSITE MATERIALS》 * |
| 普罗德曼: "《聚合物基体复合材料中的界面》", 30 September 1980, 中国建筑工业出版社 * |
| 胡小龙: ""超声法制备高岭土-水合肼插层复合物"", 《化工管理》 * |
| 高端娟等: ""氧化硅溶胶对石墨表面的亲水改性"", 《上海大学学报（自然科学版）》 * |
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Application publication date: 20180529 |