CN102530916A - Preparation method of coal-based carbon foam - Google Patents
Preparation method of coal-based carbon foam Download PDFInfo
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- CN102530916A CN102530916A CN2011104556323A CN201110455632A CN102530916A CN 102530916 A CN102530916 A CN 102530916A CN 2011104556323 A CN2011104556323 A CN 2011104556323A CN 201110455632 A CN201110455632 A CN 201110455632A CN 102530916 A CN102530916 A CN 102530916A
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Abstract
The invention relates to a normal-pressure preparation method of a coal-based carbon foam material, which belongs to the technical field of preparation of the coal-based carbon foam. The method comprises the following processes of: (1) performing crushing and screening treatment on coal; (2) adding coal particles into a normal-pressure container, exerting mechanical extrusion force on a coal bed, heating in an inert atmosphere to foaming temperature for foaming, and then naturally cooling down to room temperature to get a coal-based nascent carbon foam material; (3) carbonizing the coal-based foam material under the protection of the inert atmosphere at the temperature of 800-1500 DEG C to get the coal-based carbon foam material; and (4) placing the coal-based carbon foam material obtained after carbonization into a graphitizing furnace to perform graphitizing treatment to get a graphite foam material. The normal-pressure preparation method of the coal-based carbon foam material, disclosed by the invention, has the characteristics that a high-pressure kettle and other pressure expansion equipment are not required, a foaming agent is not required for foaming, oxidation stabilization treatment does not need to be performed on the nascent carbon foam before the carbonization, the preparation of the coal-based carbon foam under normal pressure can be realized by adopting a mechanical compressing method, and preparation equipment is simple. According to the normal-pressure preparation method of the coal-based carbon foam material, disclosed by the invention, the structure and the performances of the carbon foam can be conveniently regulated.
Description
Technical field
This preparation method who relates to the coal-based carbon foam of a kind of high-strength thermal insulation belongs to coal-based carbon foam preparing technical field.
Background technology
Coal-based carbon foam (also claiming Carbon foam) or graphite foam be a kind ofly have that density is little, high temperature resistant, anti-thermal shock, corrosion-resistant, the porous carbon materials that is prone to premium propertiess such as processing, heat-conductivity conducting (the heat-conductivity conducting performance is adjustable) and thermal expansivity be little; Be widely used in thermal management materials, thermally protective materials, biomaterial, stealth material, matrix material frock, advanced composite material skeleton, heavy-duty battery electrode materials, support of the catalyst, and many technical fields such as lightweight armor material.
In the method for coal-based carbon foam preparation, the method for employing has: pitch is isolated in (1) from coal rare, and rare with pitch is feedstock production carbon foam.This method hydrogenation needs hydrogen supply dissolvent, high pressure and catalyzer etc., makes technology and equipment become complicated like this, and cost increases; (2) the carbon foam is prepared in the control heating in the mould of non-oxidizing atmosphere.This method advantage is to improve the external gas pressure in the coal cracking process through coal self volatilization gas, and shortcoming is to need high-intensity mould.
Summary of the invention
The objective of the invention is in the coal-based carbon foam preparation process, to the defective that prior art exists, providing a kind of can directly be raw material with the coal, and environmental stress is a preparation carbon foam under the condition of normal pressure (1 standard atmospheric pressure).This procedure is simple, and can control its structure and performance.
The present invention realizes through following proposal.The present invention is for being the coal-based carbon foamy preparation method under the normal pressure (1 standard atmospheric pressure) at environmental stress.A kind of coal-based carbon foamy preparation method of the present invention is characterized in that having following process and step:
A. adopt non-pressure vessel, the coal grain is added in the container, on coal bed, apply briquetting, make coal bed receive 100 ~ 10 for every square metre
5The pressure of N.Elder generation is heated to 300 ~ 450 ℃, constant temperature 0.5 ~ 10h with the heat-up rate of 0.5 ~ 20 ℃/min under protection of inert gas; Heat-up rate with 0.1 ~ 10 ℃/min is heated to 350 ~ 800 ℃ again, and constant temperature 0 ~ 10h accomplishes nascent carbon foamy preparation.
B. the carbon foam that step a is made places carbide furnace; Heat-up rate with 1 ~ 20 ℃/min under protection of inert gas is warming up to 350 ~ 800 ℃; Heat-up rate with 0.1 ~ 10 ℃/min is warming up to 800 ~ 1500 ℃ again, and constant temperature 0.1 ~ 20h under this temperature obtains the carbonization foam.
C. the carbonized carbonaceous foam that step b is made is put into graphitizing furnace and is carried out graphitization processing, obtains the greying foam materials.
Above-mentioned coal grain is a kind of or its mixture in brown coal, bituminous coal and the hard coal that contains certain volatile matter, and above-mentioned rare gas element is nitrogen, argon gas or carbonic acid gas etc.
Of the present inventionly be a little: need not use pressure expansion equipment such as autoclave, not need whipping agent, also need before carbonization, not carry out oxidation-stabilized processing nascent carbon foam; And equipment is simple.The present invention can regulate carbon foamy structure and performance easily.
Description of drawings
Accompanying drawing 1 is a heating curve in the coal-based nascent carbon foam preparation process among the embodiment two.
Accompanying drawing 2 is a heating curve in the coal-based nascent carbon foam carbonization process among the embodiment two.
Accompanying drawing 3 is to obtain coal-based carbon foamy electron scanning micrograph among the embodiment two.
Embodiment
Embodiment 1
Taking by weighing the coal grain that 40g crosses 80 mesh sieves is raw material.Put into as figure with shown in foaming vessel, vibrating compacting makes the surfacing of coal grain.Put briquetting and lever at the coal bed upper surface, briquetting and lever make every square metre of coal bed receive the pressure of 1000N, make lever pass container cover intermediary hole then, the covered container lid.With container place retort furnace under protection of nitrogen gas with the heat-up rate to 500 of 1 ℃/min ℃, under this temperature, be incubated 2h, obtain nascent carbon foam.The nascent carbon foam that obtains is placed carbide furnace, and the heat-up rate with 1 ℃/min under protection of nitrogen gas is warming up to 1100 ℃, under this temperature, is incubated 2h, obtains the carbonization foam.The carbonization foam is placed graphitizing furnace, and the heat-up rate with 2 ℃/min under the protection of high-purity argon gas is warming up to 2800 ℃, under this temperature, is incubated 2h, obtains graphite foam.
Embodiment 2
Taking by weighing the coal grain that 40g crosses 100 mesh sieves is raw material.Put into as figure with shown in foaming vessel, vibrating compacting makes the surfacing of coal grain.Put briquetting and lever at the coal bed upper surface, briquetting and lever make every square metre of coal bed receive the pressure of 1000N, make lever pass container cover intermediary hole then, the covered container lid.With container place retort furnace under protection of nitrogen gas with the heat-up rate to 380 of 5 ℃/min ℃, under this temperature, be incubated 2h.Heat-up rate with 1 ℃/min is warmed up to 480 ℃, under this temperature, is incubated 2h, obtains nascent carbon foam.The nascent carbon foam that obtains is placed carbide furnace, and the heat-up rate with 5 ℃/min under protection of nitrogen gas is warming up to 480 ℃, and the heat-up rate with 1 ℃/min is warming up to 1100 ℃ then, under this temperature, is incubated 2h, obtains the carbonization foam.Its ESEM picture is as shown in Figure 4.The carbonization foam is placed graphitizing furnace, and the heat-up rate with 2 ℃/min under the protection of high-purity argon gas is warming up to 2800 ℃, under this temperature, is incubated 2h, obtains graphite foam.
Embodiment 3
Taking by weighing the coal grain that 40g crosses 100 mesh sieves is raw material.Put into as figure with shown in foaming vessel, vibrating compacting makes the surfacing of coal grain.Put briquetting and lever at the coal bed upper surface, briquetting and lever make every square metre of coal bed receive the pressure of 500N, make lever pass container cover intermediary hole then, the covered container lid.With container place retort furnace under protection of nitrogen gas with the heat-up rate to 380 of 5 ℃/min ℃, under this temperature, be incubated 2h.Heat-up rate with 0.5 ℃/min is warmed up to 450 ℃, under this temperature, is incubated 6h, obtains nascent carbon foam.The nascent carbon foam that obtains is placed carbide furnace, and the heat-up rate with 5 ℃/min under protection of nitrogen gas is warming up to 450 ℃, and the heat-up rate with 1 ℃/min is warming up to 1100 ℃ then, under this temperature, is incubated 2h, obtains the carbonization foam.The carbonization foam is placed graphitizing furnace, and the heat-up rate with 2 ℃/min under the protection of high-purity argon gas is warming up to 2800 ℃, under this temperature, is incubated 2h, obtains graphite foam.
Embodiment 4
Taking by weighing the coal grain that 40g crosses 120 mesh sieves is raw material.Put into as figure with shown in foaming vessel, vibrating compacting makes the surfacing of coal grain.Put briquetting and lever at the coal bed upper surface, briquetting and lever make every square metre of coal bed receive the pressure of 500N, make lever pass container cover intermediary hole then, the covered container lid.With container place retort furnace under protection of nitrogen gas with the heat-up rate to 400 of 3 ℃/min ℃, under this temperature, be incubated 2h.Heat-up rate with 0.5 ℃/min is warmed up to 480 ℃, under this temperature, is incubated 2h, obtains nascent carbon foam.The nascent carbon foam that obtains is placed carbide furnace, and the heat-up rate with 5 ℃/min under protection of nitrogen gas is warming up to 450 ℃, and the heat-up rate with 1 ℃/min is warming up to 1100 ℃ then, under this temperature, is incubated 2h, obtains the carbonization foam.The carbonization foam is placed graphitizing furnace, and the heat-up rate with 2 ℃/min under the protection of high-purity argon gas is warming up to 2800 ℃, under this temperature, is incubated 2h, obtains graphite foam.
Claims (6)
1. coal-based carbon foamy preparation method is characterized in that having following process:
Adopt non-pressure vessel, the coal grain is added in the container, on coal bed, apply briquetting, make coal bed receive 100 ~ 10 for every square metre
5The pressure of N.
2. first heat-up rate with 0.5 ~ 20 ℃/min is heated to 300 ~ 450 ℃, constant temperature 0.5 ~ 10h under protection of inert gas; Heat-up rate with 0.1 ~ 10 ℃/min is heated to 350 ~ 800 ℃ again, and constant temperature 0 ~ 10h accomplishes nascent carbon foamy preparation.
3. the carbon foam that step a is made places carbide furnace; Heat-up rate with 1 ~ 20 ℃/min under protection of inert gas is warming up to 350 ~ 800 ℃; Heat-up rate with 0.1 ~ 10 ℃/min is warming up to 800 ~ 1500 ℃ again, and constant temperature 0.1 ~ 20h under this temperature obtains the carbonization foam.
4. the carbonized carbonaceous foam that step b is made is put into graphitizing furnace and is carried out graphitization processing, obtains the greying foam materials.
5. by the described a kind of coal-based carbon foamy preparation method of claim, it is characterized in that said coal grain is a kind of or its mixture in brown coal, bituminous coal and the hard coal, contains 5% ~ 50% volatile matter, its softening temperature is at 300 ~ 450 ℃.
6. by a kind of coal-based carbon foamy preparation method described in the claim 1, it is characterized in that described rare gas element can be nitrogen, argon gas or carbonic acid gas etc.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104229773A (en) * | 2014-09-15 | 2014-12-24 | 荣成炭谷有限公司 | Preparation method of foamy carbon material |
| CN106278367A (en) * | 2016-08-04 | 2017-01-04 | 辽宁科技大学 | Under normal pressure, the device and method of coal-based carbon foam prepared by microwave heating |
| CN111547703A (en) * | 2020-05-22 | 2020-08-18 | 太原理工大学 | Method for preparing coal-based foam carbon based on normal-pressure self-foaming |
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| CN2679134Y (en) * | 2003-09-29 | 2005-02-16 | 大连理工大学 | Appts. for continuous prepn. of foamed charcoal material from coal |
| US20060222854A1 (en) * | 2005-03-31 | 2006-10-05 | Matviya Thomas M | High density carbon foam |
| CN1872677A (en) * | 2005-06-03 | 2006-12-06 | 中国矿业大学（北京校区） | High heat conducting foam material of graphite, and fabricating method |
| CN101693533A (en) * | 2009-10-23 | 2010-04-14 | 大连理工大学 | Method for preparing nanometer carbon fiber/foam coal through taking coal liquefaction residues as raw materials |
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2011
- 2011-12-31 CN CN2011104556323A patent/CN102530916A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2679134Y (en) * | 2003-09-29 | 2005-02-16 | 大连理工大学 | Appts. for continuous prepn. of foamed charcoal material from coal |
| US20060222854A1 (en) * | 2005-03-31 | 2006-10-05 | Matviya Thomas M | High density carbon foam |
| CN1872677A (en) * | 2005-06-03 | 2006-12-06 | 中国矿业大学（北京校区） | High heat conducting foam material of graphite, and fabricating method |
| CN101693533A (en) * | 2009-10-23 | 2010-04-14 | 大连理工大学 | Method for preparing nanometer carbon fiber/foam coal through taking coal liquefaction residues as raw materials |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104229773A (en) * | 2014-09-15 | 2014-12-24 | 荣成炭谷有限公司 | Preparation method of foamy carbon material |
| CN106278367A (en) * | 2016-08-04 | 2017-01-04 | 辽宁科技大学 | Under normal pressure, the device and method of coal-based carbon foam prepared by microwave heating |
| CN106278367B (en) * | 2016-08-04 | 2018-11-13 | 辽宁科技大学 | Microwave heating prepares the device and method of coal-based carbon foam under normal pressure |
| CN111547703A (en) * | 2020-05-22 | 2020-08-18 | 太原理工大学 | Method for preparing coal-based foam carbon based on normal-pressure self-foaming |
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Application publication date: 20120704 |