CN1587034A - Process for preparing nano porous graphite - Google Patents
Process for preparing nano porous graphite Download PDFInfo
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- CN1587034A CN1587034A CN 200410052871 CN200410052871A CN1587034A CN 1587034 A CN1587034 A CN 1587034A CN 200410052871 CN200410052871 CN 200410052871 CN 200410052871 A CN200410052871 A CN 200410052871A CN 1587034 A CN1587034 A CN 1587034A
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Abstract
The preparation of nanometer porous graphite includes thermochemical process to prepare graphite intercalation compound, microwave process to swell the graphite intercalation compound and mechanical process to extrude expanded graphite. The porous graphite m prepared through the said process contains nanometer level pores, has effectively improved liquid or gas matter absorbing capacity, strengthened heat exchanging and transferring capacity, etc. and thus wide applicated in ecological building, environment protection, purification and other fields.
Description
Technical field
The invention belongs to technical field of nano material, be specifically related to a kind of preparation method with porous graphite of nano level hole.
Background technology
A main branch is expanded graphite and deriving technology thereof in the graphite material.So-called expanded graphite is by thermochemical method or electrochemical method, and the flaky graphite starting material are carried out intercalation processing, carries out expanded then under hot environment and the graphite material porosity and looseness with high porosity that obtains.Expanded graphite can obtain many-sided application through after the appropriate postprocessing, comprises cleaning oil pollution material, sound-proof material, heat preserving and insulating material and medical material etc.
But adopt the void ratio of expanded graphite of existing expanded graphite technology preparation thicker, generally all more than micron order.Cross every performance that thick hole has seriously retrained expanded graphite, comprise adsorptive power, heat transfer exchange capability of heat and sound insulation capabilities etc.In recent years, the nano material technology development is very fast.The mano-porous material technology is a very important focus of field of nanometer material technology.Utilize the method for various physics and chemistry that traditional porous material is improved, its aperture is further narrowed down to nanometer range, the preparation mano-porous material, not only can improve every performance of mano-porous material, can also produce some novel effect and performances, these all have significant values to range of application and its application potential of excavation of expanding porous material.
Summary of the invention
Purpose of the present invention is proposing a kind of preparation method with porous graphite of nanoaperture.
The preparation method of the Nano-size Porous Graphite that the present invention proposes comprises the preparation, expanded and compress three steps, specific as follows of graphite intercalation compound:
(1) preparation of graphite intercalation compound:
Adopt thermochemical method to prepare graphite intercalation compound.At first the flaky graphite starting material are cleaned oven dry; Then crystalline flake graphite is mixed with intercalator, oxygenant, three's weight proportion is a crystalline flake graphite: intercalator: oxygenant=1: 3-10: 0.1-1; Under 25-60 ℃ water bath with thermostatic control condition stirring heating 20-60 minute; Refilter with water washed mixture to pH value and be 0-3; At last with this mixture oven dry.
In this step, it is sulfuric acid more than 98% that intercalator can adopt concentration, and oxygenant can adopt potassium permanganate.Crystalline flake graphite can adopt fineness greater than 80 orders, carbon content greater than 90% crystalline flake graphite.
Stir RPM (per minute rotates all numbers) and get 200-400.Bake out temperature is got 60～80 ℃, drying time 6～12 hours.
(2) graphite intercalation compound is expanded:
Adopt microwave method expanded graphite intercalation thing.At first take by weighing a certain amount of graphite intercalation compound, put into terrine, then terrine is put into microwave oven and carried out expanded.Generally, the desirable 200～2000ml of terrine volume.Expanded power is taken in 100～800W scope, and the expanded time got 10～30 seconds.
(3) extruding of expanded graphite:
Adopt mechanical means compression-expansion graphite.Specifically expanded graphite can be put into pipe (pipe or square tube), with the extremely certain compression ratio of expanded graphite in the piston extruded tube.Generally getting compression ratio is 0.1～0.5 of graphite expansion ratio.The section area of piston is identical with shape with the interior section area of shape and pipe.
The thermochemistry intercalation, microwave bulking and the pressing method that adopt the present invention to propose prepare the porous graphite material and contain nano level hole; can effectively improve the performance such as adsorptive power, heat exchange heat-transfer capability of porous graphite liquid towards or gaseous substance; and some unique nano effects can appear, can have purposes widely at aspects such as ecotecture, environment protection and purifying treatment.
Description of drawings
Fig. 1 is the pore size distribution curve of the Nano-size Porous Graphite of embodiment 1.
Fig. 2 is the pore size distribution curve of the Nano-size Porous Graphite of embodiment 2.
Fig. 3 is the pore size distribution curve of the Nano-size Porous Graphite of embodiment 3.
Embodiment
Embodiment 1
Get fineness and be 80 orders, carbon content and be 90% crystalline flake graphite 3 grams, concentration and be 98% sulfuric acid 30 grams and potassium permanganate 2 grams, put into beaker, stir, mix with glass stick.Then this beaker is put into water bath with thermostatic control, the temperature of water-bath is set at 45 ℃.Adopt bar magnet that mixture is continued to stir, stir RPM and be decided to be 300.Carry out water wash procedures behind the intercalation.Mixture is filtered with 200 purpose stainless (steel) wires, will filter the beaker that residuum is put into 500ml then, enter the clear water of 400ml, fully stir, and then filter with 200 purpose stainless (steel) wires with glass stick.Twice of repeated washing.The pH value of measuring last stirring liquid is 0.2.Last filtering residuum is put into glass culture dish, put into baking oven then and dry.Oven temperature is 60 ℃, and the drying course time length is 10 hours.Get the good graphite intercalation compound of oven dry 0.5 gram, put into the terrine that volume is 500ml, then terrine is put into microwave oven.With the power setting of microwave oven on 200W.Start microwave oven, the microwave time of origin is 30 seconds.Measure the quality and the volume of expanded graphite.Then expanded graphite is put into compressed pipe and push, getting press ratio is 0.2 of rate of expansion.Adopt mercury penetration method to measure the pore structure of last porous graphite.Accompanying drawing 1 is put into distribution curve for its aperture.
Embodiment 2
Get fineness and be 50 orders, carbon content and be 95% crystalline flake graphite 3 grams, concentration and be 98% sulfuric acid 30 grams and potassium permanganate 2 grams, put into beaker, stir, mix with glass stick.Then this beaker is put into water bath with thermostatic control, the temperature of water-bath is set at 50 ℃.Adopt bar magnet that mixture is continued to stir, stir RPM and be decided to be 300.Carry out water wash procedures behind the intercalation.Mixture is filtered with 200 purpose stainless (steel) wires, will filter the beaker that residuum is put into 500ml then, enter the clear water of 400ml, fully stir, and then filter with 200 purpose stainless (steel) wires with glass stick.Repeated washing 4 times.The pH value of measuring last stirring liquid is 3.0.Last filtering residuum is put into glass culture dish, put into baking oven then and dry.Oven temperature is 60 ℃, and the drying course time length is 10 hours.Get the good graphite intercalation compound of oven dry 0.5 gram, put into the terrine that volume is 500ml, then terrine is put into microwave oven.With the power setting of microwave oven on 200W.Start microwave oven, the microwave time of origin is 30 seconds.Measure the quality and the volume of expanded graphite.Then expanded graphite is put into compressed pipe and push, getting press ratio is 0.2 of rate of expansion.Adopt mercury penetration method to measure the pore structure of last porous graphite.Accompanying drawing 2 is put into distribution curve for its aperture.
Embodiment 3
Get fineness and be 80 orders, carbon content and be 90% crystalline flake graphite 3 grams, concentration and be 98% sulfuric acid 30 grams and potassium permanganate 2 grams, put into beaker, stir, mix with glass stick.Then this beaker is put into water bath with thermostatic control, the temperature of water-bath is set at 60 ℃.Adopt bar magnet that mixture is continued to stir, stir RPM and be decided to be 300.Carry out water wash procedures behind the intercalation.Mixture is filtered with 200 purpose stainless (steel) wires, will filter the beaker that residuum is put into 500ml then, enter the clear water of 400ml, fully stir, and then filter with 200 purpose stainless (steel) wires with glass stick.Repeated washing 6 times.The pH value of measuring last stirring liquid is 6.0.Last filtering residuum is put into glass culture dish, put into baking oven then and dry.Oven temperature is 60 ℃, and the drying course time length is 10 hours.Get the good graphite intercalation compound of oven dry 0.5 gram, put into the terrine that volume is 500ml, then terrine is put into microwave oven.With the power setting of microwave oven on 200W.Start microwave oven, the microwave time of origin is 30 seconds.Measure the quality and the volume of expanded graphite.Then expanded graphite is put into compressed pipe and push, getting press ratio is 0.2 of rate of expansion.Adopt mercury penetration method to measure the pore structure of last porous graphite.Accompanying drawing 3 is put into distribution curve for its aperture.
Claims (4)
1, a kind of preparation method of Nano-size Porous Graphite is characterized in that concrete steps are as follows:
(1) adopt thermochemical method to prepare graphite intercalation compound: at first the flaky graphite starting material to be cleaned oven dry; Then crystalline flake graphite is mixed with intercalator, oxygenant, three's weight proportion is a crystalline flake graphite: intercalator: oxygenant=1: 3-10: 0.1-1; Under 25-60 ℃ water bath with thermostatic control condition stirring heating 20-60 minute; Refilter with water washed mixture to pH value and be 0-3; At last with this mixture oven dry;
(2) adopt microwave method expanded graphite intercalation thing: at first take by weighing a certain amount of graphite intercalation compound, put into terrine, then terrine is put into microwave oven and carried out expandedly, expanded power is 100～800W, and the expanded time is 10～30 seconds;
(3) compression-expansion graphite: expanded graphite is put into pipe,, get the 0.1-0.5 that compression ratio is the graphite expansion ratio with graphite in the piston extruded tube.
2, preparation method according to claim 1 is characterized in that said intercalator is the sulfuric acid more than 98%, and oxygenant is a potassium permanganate.
3, preparation method according to claim 1, the fineness that it is characterized in that said crystalline flake graphite greater than 80, carbon content is greater than 90%.
4, preparation method according to claim 1 is characterized in that said bake out temperature is 60-80 ℃, and drying time is 6-12 hour.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100528714A CN100336720C (en) | 2004-07-15 | 2004-07-15 | Process for preparing nano porous graphite |
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| CNB2004100528714A CN100336720C (en) | 2004-07-15 | 2004-07-15 | Process for preparing nano porous graphite |
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| CN1587034A true CN1587034A (en) | 2005-03-02 |
| CN100336720C CN100336720C (en) | 2007-09-12 |
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| CNB2004100528714A Expired - Fee Related CN100336720C (en) | 2004-07-15 | 2004-07-15 | Process for preparing nano porous graphite |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891186A (en) * | 2010-06-11 | 2010-11-24 | 北京工业大学 | Method for preparing expanded graphite by adopting microwave puffing method |
| CN101077988B (en) * | 2007-06-29 | 2011-07-27 | 燕山大学 | Method for preparing nano expanded graphite lubricating oil additive |
| CN103395777A (en) * | 2013-08-07 | 2013-11-20 | 大同市普朔科技有限责任公司 | Preparation method of nano-graphite carbon powder |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102963886A (en) * | 2012-11-28 | 2013-03-13 | 同济大学 | Preparation method of porous graphene oxide |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1043031C (en) * | 1996-07-12 | 1999-04-21 | 清华大学 | Microwave bulking desulfurating method for expansible graphite |
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2004
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101077988B (en) * | 2007-06-29 | 2011-07-27 | 燕山大学 | Method for preparing nano expanded graphite lubricating oil additive |
| CN101891186A (en) * | 2010-06-11 | 2010-11-24 | 北京工业大学 | Method for preparing expanded graphite by adopting microwave puffing method |
| CN101891186B (en) * | 2010-06-11 | 2012-01-18 | 北京工业大学 | Method for preparing expanded graphite by adopting microwave puffing method |
| CN103395777A (en) * | 2013-08-07 | 2013-11-20 | 大同市普朔科技有限责任公司 | Preparation method of nano-graphite carbon powder |
| CN103395777B (en) * | 2013-08-07 | 2014-07-30 | 大同市普朔科技有限责任公司 | Preparation method of nano-graphite carbon powder |
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| CN100336720C (en) | 2007-09-12 |
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Granted publication date: 20070912 Termination date: 20100715 |