CN106278367B - Microwave heating prepares the device and method of coal-based carbon foam under normal pressure - Google Patents
Microwave heating prepares the device and method of coal-based carbon foam under normal pressure Download PDFInfo
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- CN106278367B CN106278367B CN201610634092.8A CN201610634092A CN106278367B CN 106278367 B CN106278367 B CN 106278367B CN 201610634092 A CN201610634092 A CN 201610634092A CN 106278367 B CN106278367 B CN 106278367B
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Abstract
The device and method that microwave heating prepares coal-based carbon foam under normal pressure, the device mainly includes：Microwave protection case is placed in holder in microwave chemical defence case, quartz molds, the intelligent temperature control instrument and microwave power adjuster for being placed in the microwave generator below holder and being placed in outside microwave chemical defence case.The preparation method is that the method that microwave heating prepares coal-based carbon foam under normal pressure, key step include：Preparation, the microwave heating of coal-based carbon foam precursor prepare the first raw body of coal-based carbon foam and carry out charing process to raw body at the beginning of coal-based carbon foam, and coal-based carbon foam is made.The beneficial effects of the invention are as follows：The time for preparing coal-based carbon foam is greatly shortened, energy consumption is reduced, solves the problems, such as that occurring macroscopic cracking when preparing coal-based carbon foam by heat transfer even cracks, while the invention has simple and practicable, easy to spread feature.
Description
Technical field
The invention belongs to prepare coal-based carbon foam technology field, coal base is prepared more particularly to microwave heating under a kind of normal pressure
The device and method of carbon foams.
Background technology
Carbon foams are a kind of brand-new materials having both structure and functional characteristic, it is a kind of with three-dimensional cross-linked hole, hole wall
And the lightweight Carbon Materials of different holes crosslink part composition.The pore structure of carbon foams include bulk density, the porosity, real density,
Hole pattern, average pore diameter, the density in hole (the hole number that i.e. unit volume carbon foams have)), pore-size distribution etc..Pass through change
Raw material type and property and preparation parameter, may be implemented the cutting of carbon foams pore structure, and then carbon foams performance may be implemented
Regulation and control.Therefore, carbon foams have as thermal management materials, absorbing material, electromagnetic shielding material, catalyst carrier, adsorption material
The property of material；Since carbon foams have biocompatibility, also there is the potential quality of application in life science；Carbon foams can also be with
Other metals or nonmetallic compound preparation structure material；Due to the characteristics of carbon foams are light, dimensionally stable, easy processing, Ke Yiyong
The mold and space microscope base etc. of fibrous woven and composite material preparation.In short, the preparation of carbon foams, application, modification etc. are ground
Study carefully is to receive significant attention at home.And the preparation of carbon foams is the most important link in carbon foams research and application.
Up to the present, the preparation method of carbon foams includes following several：
(1) foaming agent foam method
Foaming agent foam method is to prepare the common method of resin base carbon foams.This method is using resin as raw material, with foaming agent
Mixing is heated using outside reactor under high pressure, and heat conducts heat by the outer wall of reactor to material, when temperature liter
To resin softening point temperatures above, then decompression step by step, makes foaming agent decompose or volatilize, leaves vacancy and form bubble in resin
Foam finally carbonizes, graphitization (high-temperature process) obtains carbon foams.If presoma resin is thermoplastic resin, also needed before charing
Through peroxidating, solidification process.And in practical applications, sometimes for the intensity for improving resin base carbon foams, even with thermosetting
Property resin be presoma, oxidation processes are also carried out before charing.
This method needs to add foaming agent, additionally needs and carries out pre-oxidation treatment to presoma, therefore cost is also higher.
(2) pressurization charring
This method is also known as high pressure nitriding gas method, refers to being placed in high pressure using pitch, coal or thermoplastic polymer as presoma and setting
In standby, reach certain pressure (i.e. blow pressure) to high-tension apparatus inside inflated with nitrogen, heated using outside reactor, heat passes through
The outer wall of reactor conducts heat to material, reaches set temperature (i.e. blowing temperature), at this temperature, constant temperature certain time
After (i.e. foamed time), pressure release foaming, obtaining your carbon foams, just (document having claims green foam to raw body, refers to that presoma is completed
Foaming, and cure, form the whole semicoke of porous structure).Then charing and graphitization processing are carried out again.This method is adjustable
Parameter has blow pressure, blowing temperature, foamed time, pressure release rate and forerunner's volume property, therefore designability is stronger, is mesh
The preceding main method for preparing carbon foams, preparation flow are as shown in Figure 1.
Generate two kinds of new methods again based on this method：
1) spontaneous foam method
So-called spontaneous platen press refers to using thermoplastic material (pitch, coal or thermoplastic polymer etc.), after being heated in presoma
Molecular side chain breaks to form gaseous state small molecule and original small-molecule substance volatilizes parent together, reaches by these gases
One blow pressure, the constant temperature certain time under blowing temperature, pressure release nucleation foaming obtains carbon foams just raw body, using charing,
Obtain carbon foams.It is required to carry out graphitization processing according to application scenario.
2) space law is limited
This method is the invention that Wang Chengyang teaches seminar.The isostatic pressed that raw material generates in mold by volume expansion has
Conducive to forming the hole of uniform pore diameter.The specific method is as follows：It is sealed after mesophase pitch powder is put people's mold, then mold is added
Heat arrives asphalt softening point temperatures above, cools down after keeping the temperature a period of time, obtains carbon foams raw body, then will be carbonized and be graphitized
Processing is to get to intermediate phase pitch-based carbon foams.It, can be by adjusting mold in the case that gross space is certain in holding mold
Interior feeding quantity adjusts pressure, realizes Carbon foam pore size control；It also can be in the case where feeding quantity be certain by adjusting foaming
The size in mold freedom space adjusts pressure in the process, realizes the pore size control of Carbon foam.
In recent years, coal-based carbon foam is considered most application potential since feed coal is cheap, derives from a wealth of sources, by
Extensive concern.The U.S. prepares coal-based carbon foam using medium degree of metamorphism bituminous coal as raw material, using pressurization charring, is formed many special
Profit, and in touchstone company industry.It is consistent through analyzing requirement of these patents to coal, that is, requires the necessary low ash of coal low
The free wxpansion ordinal number of sulphur and coal is 3-5 (i.e. caking property is good).And there is China's coal high grey high-sulfur, bad adhesion and mixed coal to occupy
More, such coal is not suitable for preparing coal-based carbon foam.Applicant is directed to this present situation, the liquor zinci chloridi or benzene for being 1.35 with proportion
Combination solution with carbon tetrachloride is flotation fluid, and the vitrinite in the medium degree of metamorphism bituminous coal of separation and concentration obtains vitrinite's richness
Collect object, carbon foams, the granted China's invention of this method are prepared using pressure charring (also known as high pressure nitriding gas method) using it as raw material
Patent (prepares the method that coal base is graphitized carbon foams, Patent No. ZL 2,012 1 is 0364942.9) using pretreatment bituminous coal.Root
When preparing large scale (a diameter of 120mm, a length of 300 cylinder) carbon foams according to patented method, external heat, heat are used when preparation
It is conducted to material core by the wall of high-tension apparatus.It was found that：It is relatively uniform to prepare the nascent body opening born of the same parents of carbon foams, but prepares carbon foams
Just there are macroscopic crackings, or even cracking for raw body for the carbon foams that the time of first raw body is up to 10 hours, and obtains.
In conclusion there are common ground for the method for carbon foams made above：The main equipment for preparing carbon foams is high pressure
Equipment；In the external heating of high-tension apparatus, heat by the metallic walls of high-tension apparatus to the raw material prepared used in carbon foams into
Row heat transfer.Due to for prepare carbon foams coal or vitrinite's enriched substance thermal coefficient it is very low, when closing on high-tension apparatus
After the material of metallic walls reaches blowing temperature, the temperature of material core is far from reaching blowing temperature, from appts wall to material core
There are larger temperature differences in portion.After the material of nearby device wall forms semicoke, the thermal coefficient of semicoke is high, can just significantly improve
The temperature of material adjacent with semicoke is generated from high-tension apparatus wall to material core foaming process layer by layer.Two will be brought in this way to ask
Topic, first, causing the time for preparing carbon foams longer because the thermal coefficient of presoma is low, energy consumption is high；In addition, due to sending out layer by layer
Bubble, leads to inside carbon foams that there are multilayer interfaces, and internal residual thermal stress is larger, and carbon foams is caused to generate macroscopic cracking, very
To cracking.Especially latter problem becomes bottleneck prepared by large scale coal-based carbon foam.
Invention content
The object of the present invention is to provide it is a kind of coal-based carbon foam can be greatly shortened at the beginning of raw body preparation time, reduce energy
Consumption；And solves coal-based carbon foam there are macroscopic cracking and microwave heating prepares coal-based carbon foam under the normal pressure of problem of Cracking
Device.
Another object of the present invention is to prepare coal-based carbon bubble to realize that the above method provides microwave heating under a kind of normal pressure
The method of foam.
The technology of the present invention is as follows：
To achieve the goals above, the technical solution adopted in the present invention is：
Microwave heating prepares the device of coal-based carbon foam under a kind of normal pressure of the present invention, it is characterised in that：It is anti-including microwave
Protecting box, the holder being arranged in microwave protection case and the quartz molds being placed on holder, set on the outside of the quartz molds
There is insulating layer, the gas vent being connected to quartz molds is equipped on insulating layer, row is equipped at the top of the microwave protection case
Tracheae and temperature thermocouple mounting hole are provided with microwave introduction channel in the lower part of the holder, and microwave generator is placed in microwave
The lower part of introduction channel is equipped with temperature thermocouple, the thermometric end position of the temperature thermocouple on the top of the microwave protection case
In quartz molds in presoma, the temperature thermocouple signal output end is connected with the signal input part of intelligent temperature control instrument,
The signal output end of the intelligent temperature control instrument is connected with microwave power adjuster, and microwave power adjuster is connected with microwave generator,
For the power according to temperature thermocouple measured value real-time monitoring microwave generator 13.
Further, the microwave protection case and holder are made using 304 stainless steel plate plates.
Further, the insulating layer selects alumina silicate fiber felt as insulating layer.
The method that microwave heating prepares coal-based carbon foam under a kind of normal pressure of the present invention, this method include：Prepare coal-based carbon
Foam precursor prepares the first raw body of coal-based carbon foams and carries out charing process to raw body at the beginning of coal-based carbon foams, and feature exists
In：Including following operating procedure：
(1) presoma of coal-based carbon foam is prepared：
Dry ash free basis volatilization is divided into 20.00%~45.00% bituminous coal and is crushed to 60~200 mesh, as preparing coal
Base carbon foams powdery precursor, it is spare；
Or the coal-based carbon foam powdery precursor that will have been prepared, the vitrinite's enriched substance obtained using concentration and separation will
It is used as and prepares coal-based carbon foam powdery precursor, spare；
Or coal-based carbon foam powdery precursor is added in metal die, coal original washing powder shape presoma is carried out with forcing press
It is forced into 5~20MPa, coal-based carbon foam type shape presoma is made, it is spare；
(2) heating prepares coal-based carbon foams just raw body：
The coal-based carbon foam powdery precursor or carbon foams type shape presoma are added in quartz molds, silicon is utilized
Sour aluminum fiber mat wraps up quartz molds, then quartz molds are placed on holder, and the thermometric end of temperature thermocouple is inserted into quartzy mould
In powdery precursor or type shape carbon foams presoma in tool, then intelligent temperature control instrument is arranged at 400 DEG C~500 DEG C, microwave
The temperature signal that power governor is measured according to intelligent temperature control instrument automatically adjusts the power of microwave generator, with 5 DEG C/min~50
DEG C/min is warming up to 400 DEG C~500 DEG C, constant temperature 30~60 minutes after constant temperature, closes microwave power supply, cooled to room temperature
Afterwards, coal-based carbon foams just raw body is just obtained.
(3) charing process is carried out to raw body at the beginning of coal-based carbon foams：
By coal-based carbon foam that step (2) obtains, just raw body is put into retort, under the protection of inert gas, with 1 DEG C/
Min~5 DEG C/min is warming up to 950 DEG C~1050 DEG C, keeps constant temperature 30 minutes~60 minutes, and cooled to room temperature obtains coal
Base carbon foams, the bulk density and compression strength of the coal-based carbon foam are respectively in 0.10g/cm3~1.00g/cm3With 10MPa~
Between 40MPa.
The invention also includes graphitization processings：The graphitization processing is the coal-based carbon bubble for obtaining above-mentioned steps (3)
Foam is put into graphitizing furnace, under the protection of inert nitrogen gas, with 5 DEG C/min~10 DEG C/min be warming up to 2500 DEG C~
3000 DEG C, keep constant temperature 30 minutes~180 minutes, cooled to room temperature, or control rate of temperature fall by the near room temperature of furnace temperature, i.e.,
Graphitization coal-based carbon foam is made.
It is an advantage of the invention that：The present invention provides heat system by heat transfer efficiently against as described in background for raw material
There are long preparation period, of high cost and carbon foams macroscopic cracking even problem of Cracking when raw body first for coal-based carbon foam.It is main
It shows as：
(1) time for preparing the first raw body of coal-based carbon foam is greatly shortened, energy consumption is reduced.
(2) can prepare structural integrity does not have the coal-based carbon foam of macroscopic cracking.
(3) it for preparing coal-based carbon foam by heat transfer offer heat relatively, prepares coal-based carbon using microwave heating and steeps
Foam can more effectively be adjusted the porosity of coal-based carbon foam.
Above-mentioned good effect why is generated, the mechanism of action of this method is based primarily upon, it is embodied in：
One, ionic conduction and dipole rotation are the cardinal principles of microwave heating, therefore heat medium is with polarity
Absorb the premise of microwave.Coal is a kind of macromolecular mixture of complexity, and there is high polymer feature, aromatic proton periphery to exist a large amount of
Polarity aliphatic chain and functional group, therefore coal has the chemical basis for absorbing microwave.
Secondly, microwave heating technique it is different from traditional heating mode, it is high by heated material internal dipole molecule
Frequency moves back and forth, and generates " interior frictional heat " and heating object material temperature degree is made to increase, be not necessary to any heat transfer process, can make material
Inside and outside heats while heating up simultaneously, and heating speed is fast and uniform.Therefore, using microwave heating to prepare coal-based carbon foam can be with
Reach energy-efficient purpose, simultaneously because temperature uniformly and presoma inside and outside foams simultaneously, and then avoid the occurrence of foamed phenomenon layer by layer,
Whole carbon foams are avoided macroscopic cracking or cracking occur.Cylinder coal-based carbon for preparing a diameter of 120mm, a length of 300mm steeps
Foam prepares method (the Patent No. ZL 2,012 1 0364942.9) preparation that coal base is graphitized carbon foams using pretreatment bituminous coal
The time of the first raw body of coal-based carbon foam is up to 10~12 hours, and using the method for this patent, it is nascent to prepare coal-based carbon foam
The time of body only needs 1~3 hour.
Thirdly, influence coal-based carbon foam pore structure factor include forerunner's volume property, blowing temperature, foamed time, heating
Rate.For preparing coal-based carbon foam by heat exchange pattern relatively, microwave heating, which prepares coal-based carbon foam, more to widen
In the range of adjust heating rate, therefore can the significantly more efficient bulk density for adjusting carbon foams.Utilize pretreatment bituminous coal system
The method (Patent No. ZL 2,012 1 0364942.9) of standby coal base graphitization carbon foams prepares carbon foams, obtains carbon foams
Volume density can be in 0.3g/cm3~0.8g/cm3It is adjusted in range, and according to the method for this patent, the bulk density of carbon foams can
With in 0.1g/cm3~1.0g/cm3It is adjusted in range.
Bulk density and compression strength based on coal-based carbon foam made of above-mentioned mechanism can respectively 0.10~
1.00g/cm3With 12MPa~40MPa range interior clippings.
Description of the drawings
Fig. 1 is the process flow chart that former pressure charring prepares carbon foams.
Fig. 2 is the structural schematic diagram for the device that microwave heating prepares coal-based carbon foam under normal pressure of the present invention.
Fig. 3 is the stereoscan photograph for the pore structure that coal-based carbon foam is prepared using normal pressure microwave heating.
In figure：1- microwave protection casees, 2- insulating layers, 3- quartz molds, 4- presomas, 5- microwave introduction channels, 6- holders,
7- exhaust pipes, 8- temperature thermocouples, 9- temperature thermocouple mounting holes, 10- exhaust pipes, 11- intelligent temperature control instruments, 12- microwave powers
Adjuster, 13- microwave emitters.
Specific implementation mode
The specific implementation mode of the present invention is illustrated below in conjunction with attached drawing 2.
As shown in Fig. 2, microwave heating prepares the device of coal-based carbon foam under a kind of normal pressure of the invention, and feature exists
In：Including microwave protection case 1, the holder 6 being arranged in microwave protection case 1 and the quartz molds 3 being placed on holder 6, described
The outsides of quartz molds 3 be equipped with insulating layer 2, the gas vent 10 that is connected to quartz molds 3 is equipped on insulating layer 2, described
Microwave protection case 1 top be equipped with exhaust pipe 7 and temperature thermocouple mounting hole 9, the temperature thermocouple mounting hole 9 with row
Stomata 10 is correspondingly arranged, and for facilitating installation temperature thermocouple, microwave introduction channel 5 is provided in the lower part of the holder 6, micro-
Wave producer 13 is placed in the lower part of microwave introduction channel 5, and temperature thermocouple 8 is equipped on the top of the microwave protection case 1, should
The thermometric end of temperature thermocouple 8 is located in the presoma in quartz molds 3,8 signal output end of temperature thermocouple and intelligence
The signal input part of energy temperature controller 11 is connected, and the signal output end of the intelligent temperature control instrument 11 is connected with microwave power adjuster 12,
Microwave power adjuster 12 is connected with microwave generator 13, for according to temperature thermocouple measured value real-time monitoring microwave generator
13 power.
The material of microwave protection case and holder of the present invention is 304 stainless steel plates, and microwave protection case provides sky for material foaming
Between, while preventing microwave from leaking, microwave protection upper box part panel sets two holes, and one is used to place temperature thermocouple, another
Hole is for being vented.
The microwave generation portion part of the present invention is microwave generator, and microwave is generated after energization, is heated to material.
Temperature thermocouple uses E types thermoelectricity occasionally K-type thermocouple, the temperature for measuring coal-based carbon foam precursor.
Quartz molds for filling foaming presoma, the shapes and sizes of quartz molds according to the shapes of prepared carbon foams and
Depending on size, it is internal diameter 125mm, high 400mm that cup-shaped quartz molds, size are used in the present invention.
The material of insulating layer is the thermal insulation material of saturating microwave, preferably alumina silicate fiber felt, before coal-based carbon foam
Drive body heat preservation leads to the external temperature of coal-based carbon foam precursor due to heat dissipation after preventing coal-based carbon foam precursor from heating
It reduces, an aperture is set on the top of insulating layer, for being vented and being inserted into temperature thermocouple；
The method that microwave heating prepares coal-based carbon foam under a kind of normal pressure of the present invention, this method include：Prepare coal-based carbon
Foam precursor prepares the first raw body of coal-based carbon foams and carries out charing process to raw body at the beginning of coal-based carbon foams, and feature exists
In：Including following operating procedure：
(1) presoma of coal-based carbon foam is prepared：
Dry ash free basis volatilization is divided into 20.00%~45.00% bituminous coal and is crushed to 60~200 mesh, as preparing coal
Base carbon foams powdery precursor, it is spare；
Or the coal-based carbon foam powdery precursor that will have been prepared, the vitrinite's enriched substance obtained using concentration and separation will
It is used as and prepares coal-based carbon foam powdery precursor, spare；
Or coal-based carbon foam powdery precursor is added in metal die, it is pressurizeed to powdery precursor with forcing press
To 5~20MPa, the type shape presoma of coal-based carbon foam is made, it is spare；The consistency of presoma is adjusted by pressurization to be adjusted
The bulk density of coal-based carbon foam is made；
(2) heating prepares coal-based carbon foams just raw body：
The coal-based carbon foam powdery precursor or coal-based carbon foam type shape presoma are added in quartz molds 3,
Quartz molds are wrapped up using alumina silicate fiber felt, are put on the frame 6 as insulating layer 2, then by quartz molds 3, by thermometric thermoelectricity
Type shape drives in body 4 before even thermometric end is inserted into the coal-based carbon foam powdery precursor in quartz molds or coal-based carbon foam, then
Intelligent temperature control instrument is arranged at 400 DEG C~500 DEG C, opens intelligent temperature control instrument 11, microwave power adjuster is according to intelligent temperature control instrument
The temperature signal measured automatically adjusts the power of microwave emitter, and 400 DEG C~500 are warming up to 5 DEG C/min~50 DEG C/min
DEG C, constant temperature 30~60 minutes after constant temperature, closes microwave power supply, after cooled to room temperature, just obtains coal-based carbon foams
First raw body.
(3) charing process is carried out to raw body at the beginning of coal-based carbon foams：
By coal-based carbon foam that step (2) obtains, just raw body is put into retort, under the protection of inert gas, with 1 DEG C/
Min~5 DEG C/min is warming up to 950 DEG C~1050 DEG C, keeps constant temperature 30 minutes~60 minutes, and cooled to room temperature obtains coal
Base carbon foams, the bulk density and compression strength of the coal-based carbon foam are respectively in 0.10g/cm3~1.00g/cm3And 10MPa
Between~40MPa.
In order to improve some physical properties of coal-based carbon foam, the invention also includes graphitization processings：The graphitization
Processing is that the coal-based carbon foam for obtaining above-mentioned steps (3) is put into graphitization, under the protection of inert nitrogen gas, with 5
DEG C/min~10 DEG C/min is warming up to 2500 DEG C~3000 DEG C, and keep constant temperature 30 minutes~180 minutes, cooled to room temperature,
Or the near room temperature of furnace temperature is obtained graphitization coal-based carbon foam by control rate of temperature fall.By graphitization processing, coal-based carbon foam
It is converted into graphitization coal-based carbon foam, corresponding thermal conductivity is increased to 60~70W/mK by 1~2W/mK.
Embodiment 1：
(1) presoma of coal-based carbon foam is prepared：
Dry ash free basis volatilization is divided into 20.45% bituminous coal and is crushed to 60~200 mesh, as preparing coal-based carbon foam powder
Shape presoma, it is spare；
Or the coal-based carbon foam powdery precursor that will have been prepared, the vitrinite's enriched substance obtained using concentration and separation will
It is used as and prepares coal-based carbon foam powdery precursor, spare；
Or coal-based carbon foam powdery precursor is added in metal die, it is pressurizeed to powdery precursor with forcing press
To 5~20MPa, the type shape presoma of coal-based carbon foam is made, it is spare；
The coking coal that dry ash free basis volatilization is divided into 20.45% is crushed to 60~200 mesh, and the coal after 1500 grams are crushed fills
Enter in metal die, 10MPa is forced into using forcing press, obtains coal-based carbon foam type shape presoma；
(2) heating prepares coal-based carbon foam just raw body：
The type shape presoma for the coal-based carbon foam that step (1) obtains is moved on in quartz molds, alumina silicate fiber felt is utilized
After wrapping up insulating layer for quartz molds, then the quartz molds with insulating layer are put on the holder in microwave protection case, the row of opening
Intelligent temperature control instrument is arranged in the valve of tracheae, is added to 487 DEG C with the rate of 25 DEG C/min, constant temperature 30 minutes after constant temperature, closes
Microwave is closed, room temperature is naturally cooling to, obtains carbon foams just raw body；
(3) charing process is carried out to raw body at the beginning of coal-based carbon foams：
The first raw body of coal-based carbon foam that step (2) obtains is transferred in retort, is added with the heating rate of 2.5 DEG C/min
Heat is to 1000 DEG C, and constant temperature 45 minutes, constant temperature terminates to automatically shut power off, cooled to room temperature, obtains coal-based carbon foam；
(4) graphitization processing is carried out to coal-based carbon foam
The coal-based carbon foam that step (3) obtains is transferred in graphitizing furnace, is then warming up to the rate of 7.5 DEG C/min
2800 DEG C, constant temperature 120 minutes, stop heating, cooled to room temperature, obtain graphitization coal-based carbon foam, bulk density and
Compression strength is respectively 0.95g/cm3And 39.5MPa, thermal conductivity 68mK.Normal pressure microwave heating prepares coal-based carbon foam
The stereoscan photograph of pore structure is shown in Fig. 3.
The operating procedure of other embodiment is same as Example 1, and design parameter variation see the table below 1.
1 embodiment list of table
Note：B-represents bituminous coal；V-represents vitrinite's enriched substance；- 200 mesh of 60 mesh-refer to 60 mesh sieve minus mesh and
The combination grain material of the oversize of 200 mesh sieve；Blowing temperature：Choose coal used or the maximum Ji Shi streams of vitrinite's enriched substance
It is dynamic to spend corresponding temperature；
Embodiment 1-4, the type for embodying coal changes and the change of blowing temperature, to carbon foams bulk density and compression strength
Influence；Embodiment 5-8 embodies the change of the change and blowing temperature of vitrinite's enrichment species, to carbon foams bulk density and
The influence of compression strength；When embodiment 9-13 is embodied using vitrinite's enriched substance as presoma, the variation of mechanical mass pressurization is to charcoal
The influence of foam volume density and compression strength；When embodiment 14-18 is embodied using vitrinite's enriched substance as presoma, microwave heating
Heating rate change, the influence to carbon foams bulk density and compression strength；Embodiment 19-22 embodiments are enriched with vitrinite
When object is presoma, after microwave heating to blowing temperature, the variation of constant temperature time (i.e. foamed time), to carbon foams bulk density
With the influence of compression strength.
The present disclosure additionally applies for：After the adjusting of blowing temperature, it is also applied for thermoplastic materials such as pitch and resins
Carbon foams are prepared for presoma.
Claims (5)
1. microwave heating prepares the device of coal-based carbon foam under a kind of normal pressure, it is characterised in that：Including microwave protection case, setting exists
Holder in microwave protection case and the quartz molds being placed on holder, insulating layer is equipped in the outside of the quartz molds,
Insulating layer is equipped with the gas vent being connected to quartz molds, and exhaust pipe and thermometric heat are equipped at the top of the microwave protection case
Galvanic couple mounting hole is provided with microwave introduction channel in the lower part of the holder, and microwave generator is placed under microwave introduction channel
Portion is equipped with temperature thermocouple on the top of the microwave protection case, and the thermometric end of the temperature thermocouple is located in quartz molds
Presoma in, the temperature thermocouple signal output end is connected with the signal input part of intelligent temperature control instrument, the intelligent temperature control
The signal output end of instrument is connected with microwave power adjuster, and microwave power adjuster is connected with microwave generator, for according to survey
Warm the power of galvanic couple measured value real-time monitoring microwave generator.
2. microwave heating prepares the device of coal-based carbon foam under normal pressure according to claim 1, it is characterised in that：Described
Microwave protection case and holder are made using 304 stainless steel plates.
3. microwave heating prepares the device of coal-based carbon foam under normal pressure according to claim 1, it is characterised in that：Described
Insulating layer selects alumina silicate fiber felt as insulating layer.
4. a kind of method that microwave heating prepares coal-based carbon foam under normal pressure, this method include：Prepare the forerunner of coal-based carbon foam
Body prepares the first raw body of coal-based carbon foams and carries out charing process to raw body at the beginning of coal-based carbon foams, it is characterised in that：Including with
Lower operating procedure：
（1）Prepare the presoma of coal-based carbon foam：
The bituminous coal that dry ash free basis volatilization is divided into 20.00%~45.00% is crushed to 60~200 mesh, is steeped as coal-based carbon is prepared
Foam powdery precursor, it is spare；
Or the coal-based carbon foam powdery precursor that will have been prepared, the vitrinite's enriched substance obtained using concentration and separation are made
It is spare to prepare the shape presoma of coal-based carbon foam powder；
Or coal-based carbon foam powdery precursor is added in metal die, with forcing press to coal-based carbon foam powdery precursor into
Row is forced into 5~20 MPa, and coal-based carbon foam type shape presoma is made, spare；
（2）Heating prepares coal-based carbon foams just raw body：
The coal-based carbon foam powdery precursor or coal-based carbon foam type shape presoma are added in quartz molds, silicon is utilized
Sour aluminum fiber mat wraps up quartz molds, then quartz molds are placed on holder, and the thermometric end of temperature thermocouple is inserted into quartzy mould
In coal-based carbon foam powdery precursor or coal-based carbon foam type shape presoma in tool, then intelligent temperature control instrument is arranged 400
DEG C~500 DEG C, the temperature signal that microwave power adjuster is measured according to intelligent temperature control instrument automatically adjusts the work(of microwave generator
Rate is warming up to 400 DEG C~500 DEG C with 5 DEG C/min~50 DEG C/min, and constant temperature 30~60 minutes after constant temperature, closes
It closes microwave power supply, after cooled to room temperature, just obtains coal-based carbon foams just raw body；
（3）Charing process is carried out to raw body at the beginning of coal-based carbon foams：
By step（2）Just raw body is put into retort obtained carbon foams, under the protection of inert gas, with 1 DEG C/min~5
DEG C/min is warming up to 950 DEG C~1050 DEG C, keep constant temperature 30 minutes~60 minutes, cooled to room temperature obtains coal-based carbon bubble
Foam, the bulk density and compression strength of the coal-based carbon foam are respectively in 0.10g/cm3~1.00g/cm3With 10MPa~40MPa
Between.
5. the method that microwave heating prepares coal-based carbon foam under normal pressure according to claim 4, it is characterised in that：Further include
Graphitization processing：The graphitization processing is by step（3）Obtained coal-based carbon foam is put into graphitizing furnace, in indifferent gas
Under the protection of body nitrogen, 2500 DEG C~3000 DEG C are being warming up to 5 DEG C/min~10 DEG C/min, is keeping constant temperature 30 minutes~180
Minute, the near room temperature of furnace temperature is obtained graphitization coal-based carbon foam by cooled to room temperature, or control rate of temperature fall.
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| CN102344130A (en) * | 2010-08-05 | 2012-02-08 | 常州碳元科技发展有限公司 | High heat dispersion graphite material and manufacturing method thereof |
| CN102502575A (en) * | 2011-10-24 | 2012-06-20 | 上海理工大学 | Method for preparing carbon foam by using foaming agent |
| CN102530916A (en) * | 2011-12-31 | 2012-07-04 | 上海大学 | Preparation method of coal-based carbon foam |
| CN102849723A (en) * | 2012-09-27 | 2013-01-02 | 辽宁科技大学 | Preparation method of coal-based carbon foam from pre-treated bituminous coal |
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| CN102344130A (en) * | 2010-08-05 | 2012-02-08 | 常州碳元科技发展有限公司 | High heat dispersion graphite material and manufacturing method thereof |
| CN102502575A (en) * | 2011-10-24 | 2012-06-20 | 上海理工大学 | Method for preparing carbon foam by using foaming agent |
| CN102530916A (en) * | 2011-12-31 | 2012-07-04 | 上海大学 | Preparation method of coal-based carbon foam |
| CN102849723A (en) * | 2012-09-27 | 2013-01-02 | 辽宁科技大学 | Preparation method of coal-based carbon foam from pre-treated bituminous coal |
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