CN1528861A - Method and apparatus for continuously preparing foam carbon material from coal - Google Patents
Method and apparatus for continuously preparing foam carbon material from coal Download PDFInfo
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- CN1528861A CN1528861A CNA031350054A CN03135005A CN1528861A CN 1528861 A CN1528861 A CN 1528861A CN A031350054 A CNA031350054 A CN A031350054A CN 03135005 A CN03135005 A CN 03135005A CN 1528861 A CN1528861 A CN 1528861A
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Abstract
The invention belongs to a cross technology field of coal chemistry, chemical reaction project, plasma science and charcoal material science. It refers to a method and device for using coal and water steam as materials to produce foam charcoal material continuously. The method sprays powder coal and high temperature steam into direct current arc plasma and produce foam charcoal material continuously, the mixing, foaming, synthesizing charring and graphitizing are all completed in one step. The device is made up of steam generating and supplying system, coal powder transmitting system, plasma generator, solid collector, gas cooling and purifying system, explosion protection device, system pressure adjusting system and draught fan. The invention can be operated conveniently; it can be controlled, and can be operated continuously with low cost.
Description
Technical field
The invention belongs to the technical field that Coal Chemical Industry, chemical reaction engineering, plasma science and carbon material science intersect.Relating to a kind of is core with the DC arc plasma technology, is method and the device that raw material prepares foam carbon material continuously by coal and water vapor.
Background technology
Foam carbon material has characteristics such as low density, high specific tenacity, good high temperature resistant and excellent acid-alkali-corrosive-resisting performance and surperficial oxide-free impurity, is a kind of light porous property material.It should be noted that the Carbon foam capacity of heat transmission is distributed more widely; Common Carbon foam is the same with other foam materials, and the capacity of heat transmission is lower, can be used as heat preserving and insulating material; And the higher Carbon foam of degree of graphitization has the capacity of heat transmission higher 4～6 times than metallic copper, and the thermal characteristics of Carbon foam uniqueness makes it be with a wide range of applications in high-tech sectors such as aerospace as structured material.The Carbon foam surface is polynuclear plane, the hole bubble has opening and remains silent two kinds, the higher Carbon foam of open porosity can be used as sorbent material or support of the catalyst and uses, and also can be used as good thermally conductive material and is used for the needs occasion of a large amount of heats of dissipation fast, as highly integrated computer chip etc.; The porous foam carbon material both can be processed into unit-electron emitting device crucial in many modern high technology products, as, with the field-transmitting cathode (United States Patent6054801) and the fuel cell electrode of porous foam carbon material preparation; Can be processed into again with carbon black filled foam, use (United States Patent4795763) as insulating material, therefore, the application prospect of foam carbon material is extremely extensive.
Along with science and technology development, the comprehensive utilization of coal is developed rapidly, and particularly chemistry, industrial chemicals and the high-performance carbon material of producing high added value by coal receives much attention.Utilize coal and derivative thereof successfully to make multiple carbon material through hot-work, as: coal-tar pitch based carbon fiber, intermediate phase charcoal microballon, active carbon from coal, coal charcoal processing molecular sieve etc.Rich coal resources in China is that the feedstock production carbon material has not only been expanded the range of application of coal beyond energy field with the coal, and can reduces the synthetic cost of carbon material greatly that its development prospect is wide.
Abroad, be that raw material prepares the fine Carbon foam and has been subjected to paying attention to widely with the coal, its method and principle are: high volatile volatile bituminous coal is heated to 350～550 ℃ will produce a large amount of volatile gaseses, raw material itself is the viscous fluid shape, gas discharges in viscous fluid and produces foam, the pressure release of control reaction system will make raw material expand becomes foam, and typing can generate foam materials after temperature is higher than after 500 ℃, and the foam of viscosity solidifies.The Stiller of U.S. West Virginia Univ. in 1997 etc. are raw material (United StatesPatent5888469) with bituminous coal, adopt the intermittent reaction device, and making density through operations such as deliming, hydrogenation, coking foaming and greyings is 0.2～0.4g/cm
3, the aperture is foam carbon material comparatively uniformly.The Stiller of U.S. West Virginia Univ. in 1998 etc. also is raw material (United States Patent6241957) with bituminous coal, utilize relevant technology to make light-weight, have the unique resistance to compression and the foam carbon material of conductivity, and its purposes at aspects such as aerospace field, environmental protection field, unicircuit is described.
Foam carbon material normally prepares with indirect discontinuous formula technological method.Foam materials mostly is main component (United States Patent:4795763 and 5397809) with the polymkeric substance, need the raw materials such as whipping agent, catalyzer and tensio-active agent of being correlated with in the preparation process, therefore, the preparation cost of foam materials is higher, and process is complicated.U.S. Oak Ridge laboratory Klett in 1997 etc. have invented with the method (United Stated Patent6033506) of mesophase pitch as the feedstock production Carbon foam, the aperture average out to 100 μ m of the foam carbon material that makes, have higher specific tenacity and heat conductivility, ultimate compression strength based on the Carbon foam of polymkeric substance is lower, and be difficult to greying, therefore, limited its use range, still needed its performance is improved.
Research about the Carbon foam preparation all sporadically appears in external document, up to now, does not see the domestic bibliographical information that has.Many to the research for preparing about Carbon foam abroad at present is raw material with bituminous coal or pitch, adopts the batch autoclave reaction unit.When being the feedstock production Carbon foam with bituminous coal, the bituminous coal that requires to select for use will have higher volatile content, and at first will carry out the extracting pre-treatment, removes toluene or quinoline insolubles and inorganics impurity, isolates coal-tar pitch.Be to utilize high pressure reaction assembly (under 1～5MPa) the condition, to be heated to 300～350 ℃ with the temperature rise rate of 50～100 ℃/min, and to be incubated 10～30min vacuumizing (0.001MPa) or high pressure nitrogen; Then at high pressure nitrogen (under 1～10MPa) the condition, temperature rise rate with 2 ℃/min is heated to more than 500 ℃ again, under this temperature, be incubated 1～5h and make foam curing, and under the inert atmosphere of 1000 ℃ and 2600～3200 ℃, carry out charing and greying respectively, to prepare high performance foam carbon material.This kind method prepares the Carbon foam claimed apparatus and at high temperature has tightness energy preferably, and is so that can both use under vacuum and condition of high voltage, therefore higher to the reaction unit performance requriements.On preparation technology, need strictly controlled temperature system (comprising temperature rise rate and temperature) and pressure regime, so that the volatilization when raw material reaches suitable viscosity of the volatile matter of raw material produces foamy structure, to generate even aperture distribution (being generally 200～1000 μ m), the higher Carbon foam of open porosity.
As can be seen, the method technical process of existing preparation Carbon foam is long, many and the complicated operation of the parameter of control, condition changes greatly in the preparation process, and because the limitation of metal reaction device resistance to elevated temperatures, charing just can be finished on different devices and heating installation with graphited process need, therefore can't realize serialization production, the size of product also is subjected to the limitation of reaction unit, the cost height of product, and the production cycle is long.
Summary of the invention
The objective of the invention is to overcome the shortcoming of the expensive and complex technical process of raw material in the prior art, having proposed a kind of is raw material with fine coal and pyritous water vapor directly, utilize the DC arc plasma technology to realize the method and the device of the serialization preparation of one step of foam carbon material, can reduce production costs, and, high-temperature electric arc plasma body by rotation both can be so that the reaction between the active particle that coal dust and water vapor produce have become fully and is quick, again can one the step finish the preparation process of technologies such as the charing that comprises Carbon foam and greying, technology is simple; In addition, by adding electromagnetic field, both can the constraint arc plasma body, improve the life-span of electrode and active particle, again can electric current in the coil be regulated reactant such as coal and the action time of the highly active arc plasma that excites by changing, improve utilization ratio of raw materials, make whole technology become controlled.
Technical solution of the present invention is: a kind ofly preparing the method for foam carbon material continuously by coal, is raw material with coal and water vapor directly, utilizes the DC arc plasma technology to prepare foam carbon material continuously, and concrete steps and technology are:
(1) pressure with gas in the steam generator is set at 1.4～1.8 normal atmosphere, adds the water among the hot water steam generator, after water vapor reaches the pressure of setting, open induced draft fan, regulate pressure regulating system, making system pressure is negative 20 millimeter water column, connects recirculated cooling water.
(2) connect the plasma body working gas, this working gas is a pressurized air, and compressed-air actuated flow is 1.2～3.5 cubic metres/hour; Connect the electric current of solenoid, electric current is 180～310 amperes; Connect power supply and cause electric arc in the plasma generator, the electric current of electric arc is 200～300 amperes, and this moment, the voltage of electric arc was 320～240 volts; Connect the high-temperature water vapor in the steam transmission system, the flow of water vapor is 1.5～3.0 kilograms/hour; Start coal powder conveying system, the operational throughput of coal dust is 1.5～3.6 kilograms/hour; Like this, pressurized air is directly gone into Pulverized coal injecting in the air arc-plasma of rotation.
(3) in plasma generator, mixture such as coal dust and the water vapour generation Carbon foam that under the exciting of high reactivity arc plasma of rotation, reacts, the foam carbon material that generates drops in the solid collector, the small amount of solid product is enriched on the wall of plasma generator, and gas enters gas cooling and purification system and discharges by induced draft fan along the horizontal gas passage of solid collector top.Plasma body work gas is pressurized air, and above the plasma generator lid, pressurized air is that an arm from coal dust line of pipes end enters the coal dust line of pipes, and then, pressurized air is carried coal dust secretly and entered plasma generator.The operational throughput of coal dust is to change by the rotating speed of controlling direct-current motor in the coal powder conveying system, be to change the voltage that is added on the electric motor specifically by the access resistance that changes rheochord in the circuit, thereby change the rotating speed of coal dust conveying lever, change the operational throughput of coal dust at last.Gas in the total system draws by taking out of induced draft fan, guarantee that the pressure in the plasma generator is little negative pressure, and the gas that produces is along the down going channel of reaction, respectively through the horizontal gas passage of solid collector top and gas sweetening and cooling system and through the induced draft fan discharge, intrasystem pressure can be as required satisfies different requirement of experiment by the adjusting of the pressure regulating system of induced draft fan front.
Implement a kind ofly to prepare the device of the method for foam carbon material continuously by coal, it is made up of cooling and purification system, explosion-proof equipment, system pressure regulation system and the induced draft fan of water vapor generation and plenum system, coal powder conveying system, plasma generator, solid collector, gas.Their connection is by being in proper order from top to bottom and from left to right: the cooling of water vapor generation and plenum system, coal powder conveying system, plasma generator, solid collector, gas and purification system, explosion-proof equipment, pressure regulating system and induced draft fan, the water vapor generation systems is connected with plasma generator with the coal dust line of pipes by the water supply vapour line respectively with coal powder conveying system.Plasma generator places the front of solid collector and gas sweetening and cooling system, after the coal dust that the water vapor of input and pressurized air are carried secretly enters plasma generator, be subjected to exciting of high reactivity plasma body and react during through the arc region of rotation, reacted solid and gas move downward along the down going channel of plasma generator below, subsequently, solid drops in the solid collector, and gas enters gas cooling and purification system and discharges by induced draft fan along the horizontal gas passage of solid collector top.
The present invention has utilized plasma technique, be raw material directly with high volatile volatile bituminous coal and pyritous water vapor, reduced production cost, high-temperature electric arc plasma body by rotation both can impel the reaction between the active particle that coal dust and water vapor produce to become fully and fast, again can one the step finish the preparation process of technologies such as the charing that comprises Carbon foam, greying, technology is simple; In addition, by adding electromagnetic field, both can the constraint arc plasma body, improve the life-span of electrode and active particle, again can electric current in the coil be regulated reactant such as coal and the action time of the highly active arc plasma that excites by changing, improve utilization ratio of raw materials, make whole technology become controlled.The remain silent foam aperture narrow distribution of Carbon foam of gained is about average out to 10 μ m; The micro content of open-cell foam charcoal is abundant, and pore size distribution is narrow, mainly is the micropore of 0.5～1.0nm, and macropore is distributed more widely, between 0.05～20 μ m.The crystalline size of gained Carbon foam is between 28～34nm, distance between average synusia is between 0.3361～0.3363nm, explanation is higher with the Carbon foam degree of graphitization that this kind method makes, have unique heat conductivility, will have wide practical use in high-tech sectors such as aerospace as structured material.
Plasma generator comprises: steam entry 1, coal powder entrance 2, compressed air inlet 3, hollow cylindrical anode 7, one and the isolated lid of this anode electricity, a cathod elements is housed in the lid center, graphite rod in the cathod elements is as negative electrode 6, cathode bar has axial adjustability, electric arc forms between cathode bar and round shape anode, bottom at the anode barrel, just the round-meshed graphite barrier film of a central zone piece 4 is placed in the below of electric arc, like this, can be so that the coal particle behind the process partial reaction of arc region be because be subjected to stopping and the reactor that rebounds back every module, thereby the action time of the high reactivity plasma body that improves coal dust and excite, reach the purpose that improves raw material availability; The cathode bar of plasma generating system promotes by the stepless speed regulation stepper-motor, and the negative electrode of supplement consumed is with stablizing of pilot arc; A d-c solenoid 5 that magnetic field is adjustable is housed in the outside of hollow cylindrical anode 7, the electric arc of formation was rotated, improve the life-span of electrode and plasma body, electric arc can be limited in the middle part of solenoid again, make plasma body be evenly distributed on the cross section of reactor and improve reaction efficiency.
The barrel of hollow cylindrical anode 7 and descending each joint reaction channel are all formed by three layers, and innermost layer is a graphite bushing, and its internal diameter all is 150 millimeters, highly all is 300 millimeters; Outwards one deck is an insulation bushing; Outermost layer is a water-cooling jacket.Negative electrode 6 graphite rods place the center of anode 7 barrels, and its diameter is 30 millimeters.A d-c solenoid 5 that magnetic field is adjustable is housed in the outside of hollow cylindrical anode 7.The top of gas sweetening and cooling system, just the end at pipeline is sealed by elasticity rubber.
Directly over the rubber of the terminal elasticity rubber sealing of pipeline vertical, a blade is housed, constitute explosion-proof equipment, when the pressure of system increased to certain degree, upwards expansible rubber will be scratched by blade and discharge intrasystem high pressure, thereby plays explosion-proof purpose.
The lid of device is a water-cooling jacket, and the lid that the intake pipeline of water vapor vertically passes device enters plasma generator; The coal dust line of pipes radially passes the water-cooling jacket on the lid and becomes 50 degree angles to enter producer with lid along circular lid.Above the plasma generator lid, pressurized air is that an arm from coal dust line of pipes end enters the coal dust line of pipes, and then, pressurized air is carried coal dust secretly and entered plasma generator.
The invention has the beneficial effects as follows:
Realized directly preparing foam carbon material by coal and water vapor successive.Be raw material directly, reduced the cost of raw material with fine coal and water vapor.Highly active arc plasma with rotation not only provides high temperature of reaction as means, and the high reactivity particle has played crucial activation to reaction in the plasma body, and a step is finished the various preparation process that comprise charing.Coal dust adopts the mode of airflow blow to guarantee that reactant system mixes, and has improved utilization ratio of raw materials.The adjustable electric magnetic field that adds not only is limited in electric arc the middle part of solenoid and is evenly distributed on the cross section of reactor, improved the efficient of reaction, prolonged the life-span of high reactivity particle in electrode and the plasma body, and, can regulate the intensity of reaction by the electric current that changes in the solenoid.Apparatus structure of the present invention is reasonable, and is easy and simple to handle, controlled, but serialization and operation cheaply.Do not need special vacuum or pyroreaction device, can prepare near the serialization that realizes Carbon foam under the atmospheric condition.
Description of drawings
Below in conjunction with drawings and Examples the utility model is further specified.
Fig. 1 is that to utilize arc discharge method be that raw material prepares the foam carbon material schematic representation of apparatus continuously by fine coal and water vapor directly in the present invention.
Fig. 2 is the plasma generator structural representation
Among the figure, 1. steam entry, 2. coal powder entrance, 3. compressed air inlet, 4. graphite barrier film piece, 5. solenoid, the 6. negative electrode of electric arc, the 7. anode of electric arc.
Fig. 3 is the photo of taking with scanning electronic microscope that utilizes the closed foam carbon material of institute of the present invention synthetic.
Fig. 4 is the photo that utilizes the closed foam carbon material of institute's synthetic part of the present invention that scanning electronic microscope is taken.
Fig. 5 is the photo of taking with scanning electronic microscope that utilizes the closed foam carbon material of institute of the present invention synthetic.
Fig. 6 is the photo of taking with scanning electronic microscope that utilizes institute of the present invention synthetic reticulated foams raw material of wood-charcoal material.
Embodiment
Adopting the lucky coal of platform is raw material, pulverizes the back coal particle size less than 2 millimeters.The pressure of gas in the vapour generator is set at 1.4～1.8 normal atmosphere, adds the water among the hot water steam generator, reach the pressure of setting after, open induced draft fan, regulate pressure regulating system, making system pressure is negative 20 millimeter water column, connects recirculated cooling water.
Connect plasma body working gas (pressurized air), compressed-air actuated flow is 1.2 cubic metres/hour; Connect the electric current of solenoid, electric current is 245 amperes; Connect power supply and cause the electric arc of plasma generator, the electric current of electric arc is 260 amperes, and this moment, the voltage of electric arc was 270 volts; Feed the high-temperature water vapor in the steam transmission system, the flow of water vapor is 2.4 kilograms/hour; Connect the coal dust in the coal powder conveying system, the operational throughput of coal dust is 3.0 kilograms/hour; Like this, pressurized air just injects directly into fine coal in the arc plasma jet of rotation; At last, coal dust in plasma generator and water vapour and their intermediate product generation Carbon foam that under the exciting of high reactivity particle of rotation, reacts, the a large amount of foam carbon materials that generate drop in the solid collector, small amount of foam raw material of wood-charcoal material is enriched on the wall of plasma generator, the foam carbon material typical situation such as Fig. 3～4 that utilize the present invention to prepare.
Other are with embodiment 1, and when the electric current of electric arc is 290 amperes, the voltage of electric arc is about 250 volts, and the operational throughput of coal dust is 2.1 kilograms/hour, and the photo of the exemplary electronic scanning electron microscope of gained foam carbon material is seen Fig. 5.
Other are with embodiment 1, and when the operational throughput of coal dust is 1.6 kilograms/hour, the photo of the exemplary electronic scanning electron microscope of gained foam carbon material is seen Fig. 6.
Claims (11)
1, a kind ofly preparing the method for foam carbon material continuously by coal, it is characterized in that, is raw material with coal and water vapor directly, utilizes the DC arc plasma technology to prepare foam carbon material continuously, and concrete steps and technology are:
(1) pressure with gas in the steam generator is set at 1.4～1.8 normal atmosphere, adds the water among the hot water steam generator, after water vapor reaches the pressure of setting, open induced draft fan, regulate pressure regulating system, making system pressure is negative 20 millimeter water column, connects recirculated cooling water;
(2) connect the plasma body working gas, this working gas is a pressurized air, and compressed-air actuated flow is 1.2～3.5 cubic metres/hour; Connect the electric current of solenoid, electric current is 180～310 amperes; Connect power supply and cause electric arc in the plasma generator, the electric current of electric arc is 200～300 amperes, and this moment, the voltage of electric arc was 320～240 volts; Connect the high-temperature water vapor in the steam transmission system, the flow of water vapor is 1.5～3.0 kilograms/hour; Start coal powder conveying system, the operational throughput of coal dust is 1.5～3.6 kilograms/hour; Subsequently, pressurized air is directly gone into Pulverized coal injecting in the air arc-plasma of rotation;
(3) in plasma generator, mixture such as coal dust and the water vapour generation Carbon foam that under the exciting of high reactivity arc plasma of rotation, reacts, the foam carbon material that generates drops in the solid collector, the small amount of solid product is enriched on the wall of plasma generator, and the horizontal gas passage that gas is provided with along solid collector top enters gas cooling and purification system and discharges by induced draft fan.
2, according to the described a kind of method for preparing foam carbon material by coal continuously of claim 1, it is characterized in that, the top of described plasma generator, pressurized air enters the coal dust line of pipes along an arm of coal dust line of pipes end, then, pressurized air is carried coal dust secretly and is entered plasma generator.
3., according to the described a kind of method for preparing foam carbon material by coal continuously of claim 1, it is characterized in that, the operational throughput of described coal dust is to change by the rotating speed of controlling direct-current motor in the coal powder conveying system, be to change the voltage that is added on the electric motor specifically by the access resistance that changes rheochord in the circuit, thereby change the rotating speed of coal dust conveying lever, reach the purpose of the operational throughput that changes coal dust.
4, according to the described a kind of method for preparing foam carbon material by coal continuously of claim 1, it is characterized in that, described gas draws by taking out of induced draft fan, guarantee that the pressure in the plasma generator is little negative pressure, and the gas that produces is along the down going channel of device, respectively through the horizontal gas passage of solid collector top and gas sweetening and cooling system and through the induced draft fan discharge, intrasystem pressure can be as required satisfies different requirement of experiment by the adjusting of the pressure regulating system of induced draft fan front.
5, implement the described a kind of device for preparing the method for foam carbon material by coal continuously of claim 1, it is characterized in that, it is taken place and plenum system by water vapor, coal powder conveying system, plasma generator, solid collector, the cooling of gas and purification system, explosion-proof equipment, system pressure regulation system and induced draft fan are formed, their connection is by being in proper order from top to bottom and from left to right: water vapor takes place and plenum system, coal powder conveying system, plasma generator, solid collector, the cooling of gas and purification system, explosion-proof equipment, pressure regulating system and induced draft fan, the water vapor generation systems is connected with plasma generator with the coal dust line of pipes by the water supply vapour line respectively with coal powder conveying system.
6, according to the described a kind of device for preparing foam carbon material by coal continuously of the described enforcement of claim 5 claim 1, it is characterized in that described plasma generator comprises: steam entry (1), coal powder entrance (2), compressed air inlet (3), hollow cylindrical anode (7), one and the isolated lid of this anode electricity, a cathod elements is housed in the lid center, graphite rod in the cathod elements is as negative electrode (6), cathode bar has axial adjustability, electric arc forms between cathode bar and round shape anode, the bottom of hollow cylindrical anode (7) barrel, just the round-meshed graphite barrier film of a central zone piece (4) is placed in the below of electric arc.
7, according to the described a kind of device for preparing foam carbon material by coal continuously of the described enforcement of claim 6 claim 1, it is characterized in that, described at hollow cylindrical anode (7) barrel and each descending joint reaction channel all form by three layers, innermost layer is a graphite bushing, its internal diameter all is 150 millimeters, highly all is 300 millimeters; Outwards one deck is an insulation bushing; Outermost layer is a water-cooling jacket; Negative electrode (6) graphite rod places the center of anode (7) cylinder, and its diameter is 30 millimeters.
8, a kind ofly prepare the device of foam carbon material continuously according to claim 6 and 7 described enforcement claims 1 are described, it is characterized in that a d-c solenoid (5) that magnetic field is adjustable is equipped with in described outside at hollow cylindrical anode (7) by coal.
9, a kind ofly prepare the device of the method for foam carbon material continuously according to the described enforcement of claim 5 claim 1 is described, it is characterized in that by coal, the top of described gas sweetening and cooling system, just the end at pipeline is sealed by elasticity rubber.
10, according to the described a kind of device for preparing the method for foam carbon material by coal continuously of the described enforcement of claim 5 claim 1, it is characterized in that described explosion-proof equipment is directly over the rubber of the terminal elasticity rubber sealing of pipeline vertical a blade to be housed.
11, according to the described a kind of device for preparing foam carbon material by coal continuously of the described enforcement of claim 5 claim 1, it is characterized in that, the lid of described device is a water-cooling jacket, and the lid that the intake pipeline of water vapor vertically passes reactor enters plasma generator; The coal dust line of pipes radially passes the water-cooling jacket on the lid and becomes 50 degree angles to enter producer with lid along circular lid.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101124410B (en) * | 2005-02-07 | 2013-07-24 | 爱德华兹有限公司 | Ejector pump |
| CN106582260A (en) * | 2016-11-02 | 2017-04-26 | 广西大学 | Apparatus for purifying hydrophobic organic waste gas and purifying method therefor |
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2003
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101124410B (en) * | 2005-02-07 | 2013-07-24 | 爱德华兹有限公司 | Ejector pump |
| CN106582260A (en) * | 2016-11-02 | 2017-04-26 | 广西大学 | Apparatus for purifying hydrophobic organic waste gas and purifying method therefor |
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