CN102108216A - Method for preparing conductive carbon black and hydrogen by plasma technology - Google Patents
Method for preparing conductive carbon black and hydrogen by plasma technology Download PDFInfo
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Abstract
The invention discloses a low-cost, high-dispersibility and high-conductivity carbon black and hydrogen preparation method, which is characterized in that: a gas or gasifiable carbon-containing raw material is selected, hydrogen is used as a carrier gas, a gas hydrocarbon compound is added into the carrier gas, a secondary gas hydrocarbon compound is added into a plasma wake flame, and a high-voltage, low-current and long-gap-discharge mode is adopted; the gases in plasma generators have high space velocity and short reaction dwell time; the reactants are filled in a thermal-insulation fluid bed reactor, and the dwell time of carbon black in the thermal-insulation fluid bed reactor is several seconds to several minutes; after the separation of the carbon black from the gas, part of the gas circularly enters the first plasma generator and the first fluid bed reactor, and the rest gas enters a second plasma generator and a second fluid bed reactor; and if to obtain purer hydrogen, a third plasma generator and a third fluid bed reactor can be used to obtain low-cost, high-dispersibility, high-graphitization and high-conductivity conductive carbon black and pure hydrogen.
Description
Technical field
The present invention relates to the preparation method of the graphitized carbon black and the purified hydrogen of a kind of low cost, polymolecularity and high conduction performance, be specifically related to a kind of method that adopts lower temperature plasma technology and fluidized-bed reactor to prepare graphitized carbon black and purified hydrogen.Graphitized carbon black preparation product of rubber and plastic, coating, printing ink, battery, electron device, etc. the aspect application is all arranged, and hydrogen is a kind of novel clean energy.
Background technology
Nanometer be one meter part per billion, when the yardstick of material enters nano level, just have many special performances, as surface effects, volume effect, quantum effect etc.Carbon black is a few nano material that realizes volume production very early, has that price is low, colourity is high, characteristics such as nontoxicity and chemical stability are good.The carbon black consumption in the whole world 80% is on automotive industry, and even to this day, China's automobile market also is in sales volume and raises up the stage, and market is unsaturation still.And the automobile product of rubber and plastic is to the sustainable growth that is bound to of sooty demand.According to the rising tendency in present Chinese automobile market, Chinese automobile was sold 9,380,000 in 2008, increased by 15% at least in 2009.Show that according to current research report the coming years, the whole world carbon black market requirement increased fast with average annual 5% speed at least.
High-graphitized, high dispersive, particularly be the nano-sized carbon that form such as nanotube exists and have excellent conducting performance, behind the filled conductive carbon blacks such as plastics, rubber and coating, antistatic or conductivity has very big lifting, cheap, stable performance simultaneously, thereby being used for fields such as antistatic, the antistatic coating of antistatic, electronic equipments wrapping material of product of rubber and plastic and printing ink, engineering plastics are antistatic, drying battery, cable shield, consumption is being stablized rising always.
Preparation sooty method is a lot, and traditional method can be divided into channel process and furnace treated black.Though these traditional production methods carbon black that all energy is in enormous quantities, low cost is prepared, be used for fields such as reinforcing rubber, plastics are anti-aging, tire is wear-resistant, but also exist some weakness: not only energy consumption is big, and pollute big, sooty unit consumption height, emission amount of carbon dioxide are greatly, pollution is big, the sooty conductivity is low, Deng, run in the opposite direction with the low-carbon economy of the world today.Certainly, use acetylene, use the furnace treated black technology also can produce the carbon black of high conduction, but produce calcium carbide, produce the process that acetylene itself is exactly a high pollution, high energy consumption then as raw material.Therefore, the scientific research personnel is seeking a kind of more effective and more economical preparation method always for many years.
The research work that utilizes heat plasma technology to prepare graphitized carbon black at present is mainly several companies of the U.S., Russia, France and Norway.The CB﹠amp of Norway; H technology is to be equipped with graphitized carbon black with the thermal plasma legal system, once has the report annual production to reach 2000 tons, but the finally not success of this project.The heat plasma technology greatly developed of the Timcal company of the IMP laboratory of Fa Guo Ecole desMines de Paris and Centre National de la Recherche Scientifique and Switzerland for many years, but also not success.
Summary of the invention
The purpose of this invention is to provide a kind of that be easy to realize, low-cost, polymolecularity and the graphitized carbon black of high conduction performance and the preparation method of purified hydrogen, the nano carbon black that can prepare different-shape, as spherical, bar-shaped and tubulose, resulting nano-powder good dispersity.
For achieving the above object, the technical solution used in the present invention is: select with gaseous state (as Sweet natural gas, refinery gas, coal-seam gas, coke-oven gas, oil liquefied gas, Deng) or gasifiable carbon raw material (as coal tar, ethylene bottom oil, heavy oil, biomass, waste oil is produced in life, Deng) be carbon source, in the highfield and temperature field in low-temperature plasma, use hydrogen to be carrier gas through the tail gas preheating, add gaseous hydrocarbon in the carrier gas, the hydrocarbon polymer that adds secondary in the plasma tail flame, carry out scission reaction, adopt high-voltage, the pattern of low current and big gap discharge, voltage is at 360～20kV, electric current is at 0.1～200A, the temperature of low-temperature plasma is between 1000～2600 ℃, discharging gap is several millimeters to tens of centimetres, uses the needle point discharge, the needle plate discharge, the needle ring discharge, a kind of or its combination of dull and stereotyped discharge or slip arc-over; The mol ratio of carbon source and hydrogen is between 1: 0.5～1: 5, and gas adopts high-speed, reaction time between 0.01～0.3 second in the plasma generator; Reactant enters the fluidized-bed reactor of an insulation, the carbon black residence time therein at several seconds between several minutes; After carbon black was separated from the gas, the portion gas circulation entered first plasma generator and first class bed bioreactor, and remaining gas enters second plasma generator and second fluidized-bed reactor; Obtain more purified hydrogen as need, can use C grade gas ions producer and fluidized-bed reactor.Obtain the graphitized carbon black of low cost, polymolecularity, high-graphitized and high conduction performance, and purified hydrogen.
In technique scheme, utilize " low-temperature plasma " as type of heating, to compare with the routine heating, this technology has its special advantage.Conventional oven process black carbon technology is finished by the thermo-cracking mode, is the partial combustion heating by reactant; And there is not combustion processes in the plasma technique, there is not emission of carbon-dioxide, after particularly using " lower temperature plasma technology ", temperature of reaction is significantly less than thermal plasma, very energy-conservation, overcome the shortcoming that electrode and refractory materials often damage in the heat plasma technology, therefore can non-stop run; Also overcome the very difficult shortcoming of using hydrogen as carrier gas in the heat plasma technology, can produce purified clean energy----hydrogen.
Because the utilization of technique scheme, the present invention compared with prior art has following advantage:
Suitable temperature field and highfield that low-temperature plasma generator produces, replace furnace treated black with the high temperature of oil fuel (or fuel gas) and air mixed burning generation, cracking stock oil (or Sweet natural gas, acetylene gas, Deng) produce carbon black, technological process has following advantage:
1. do not have combustion processes, the yield height of material carbon reaches the purpose of low-carbon (LC); 2. in the production process, do not produce and discharge harmful exhaust, cleaner production helps environment protection; 3. go into operation, close and regulate and load conveniently, can play the effect of regulating the peak valley electricity; 4. can combine with traditional carbon black production device, consume the cheap electric energy that waste-heat power generation produces in the conventional apparatus; 5. raw material sources are wide, can use coal tar, heavy oil, ethylene bottom oil, biomass, life to produce waste oil or Sweet natural gas, oil liquefied gas etc.; 6. compare with heat plasma technology, energy consumption is low, device can the long-time continuous operation.7. the operation of this project can play pioneer's model in the whole nation and even international carbon black industry, instructs the technological revolution of the sector----energy-saving and emission-reduction and low-carbon (LC).8. product is widely used in anlistatig rubber and plastics, anlistatig coating and printing ink and battery weighting material, electron trade; High-purity hydrogen can be done the new forms of energy of cleaning.Therefore this project can drive the development of numerous industrial circles.
Description of drawings
Fig. 1 is the reaction process synoptic diagram in the embodiment of the invention one and the example two, is specially " the preparation carbon black of one section conversion and the schema of hydrogen ";
Wherein, 1: plasma generator; 2: cracking reactor; 3: cooling duct; 4-6: cyclonic separator; 7: ash bucket; 8: the cloth bag funnel; 9: hydrogen gas compressor: 10: flare stack; 11: the water resistance firearm; 12: side direction charging: 13: hydrogen; 14-15: interchanger; 16: methane.
Accompanying drawing 2 is the SEM picture of the graphitized carbon black of preparation in the embodiment of the invention two;
Accompanying drawing 3 is the TEM picture of the graphitized carbon black of preparation in the embodiment of the invention two;
Accompanying drawing 4 is the HRTEM picture of the carbon nanotube of preparation in the embodiment of the invention three.
Embodiment
Below in conjunction with drawings and Examples the present invention is further described:
Embodiment one: a kind of is the method for raw material production graphitized carbon black with methane, uses hydrogen as carrier gas, adds methane in the carrier gas, and the voltage of discharge is at 360V, and electric current is at 20A, and discharging gap is 2～3 millimeters, uses the needle point discharge mode; The mol ratio of carbon source and hydrogen was at 1: 5, and the residence time of gas in plasma generator entered the fluidized-bed reactor of an insulation then at 0.01 second; Adopt one-level plasma generator and fluidized-bed reactor.Its reaction process is referring to shown in the accompanying drawing 1.By using the hyperthermia radiation instrumentation fixed, under above-mentioned operating mode, probably at 1200～1600 degree, the per pass conversion of methane is about 30% to the temperature in the reactor in the test.The SEM of the product of preparation and TEM are respectively shown in accompanying drawing 2 and accompanying drawing 3.
Embodiment two: a kind of propane is the method for raw material production graphitized carbon black, uses hydrogen as carrier gas, adds propane in the carrier gas, carries out scission reaction, and voltage is at 560～580V, and electric current is at 25～30A, and discharging gap is 3～5 millimeters, uses needle ring formula discharge mode; The mol ratio of carbon source and hydrogen was at 1: 5, and the residence time of gas in plasma generator entered the fluidized-bed reactor of an insulation then at 0.01 second; Adopt one-level plasma generator and fluidized-bed reactor.Its reaction process is referring to shown in the accompanying drawing 1.Finding has a lot of carbon nanotubes in the product graphitized carbon black, and its HRTEM as shown in Figure 4.The per pass conversion of propane is about 50%.
Embodiment three: a kind of is the method for raw material production graphitized carbon black and purified hydrogen with methane, uses hydrogen as carrier gas, adds methane in the carrier gas, the voltage of first plasma generator is at 5kV, electric current is at 10A, and discharging gap is 1.5 centimetres, uses needle ring formula discharge mode; The mol ratio of carbon source and hydrogen was at 1: 5, and the residence time of gas in plasma generator entered the fluidized-bed reactor of an insulation then at 0.02 second; Adopt the combination of three grades of plasma generators and fluidized-bed reactor, the voltage of second plasma generator is at 5kV, and electric current is at 8A; The voltage of C grade gas ions producer is at 5kV, and electric current is at 5A.The purity of final hydrogen is about 96%, and all the other are unconverted methane.
Claims (10)
1. low cost, the graphitized carbon black of polymolecularity and high conduction performance and the preparation method of hydrogen, it is characterized in that: select with gaseous state (as Sweet natural gas, refinery gas, coal-seam gas, coke-oven gas, oil liquefied gas, Deng) or gasifiable carbon raw material (as coal tar, ethylene bottom oil, heavy oil, biomass, waste oil is produced in life, Deng) be carbon source, use hydrogen to be carrier gas through the tail gas preheating, add gaseous hydrocarbon in the carrier gas, the hydrocarbon polymer that adds secondary in the plasma tail flame, in the highfield and temperature field in low-temperature plasma, carry out scission reaction, obtain carbon black and hydrogen.Adopt the pattern of high-voltage, low current and big gap discharge, voltage is at 360～20kV, electric current is at 0.1～200A, the temperature of low-temperature plasma is between 1000～2600 ℃, discharging gap is several millimeters to tens of centimetres, uses a kind of or its combination of needle point discharge, needle plate discharge, needle ring discharge, dull and stereotyped discharge or slip arc-over; The mol ratio of carbon source and hydrogen is between 1: 0.5～1: 5, and gas adopts high-speed, reaction time between 0.01～0.3 second in the plasma generator; Reactant enters the fluidized-bed reactor of an insulation, the carbon black residence time therein at several seconds between several minutes; After carbon black was separated from the gas, the portion gas circulation entered first plasma generator and first class bed bioreactor, and remaining gas enters second plasma generator and second fluidized-bed reactor; Obtain more purified hydrogen as need, can use C grade gas ions producer and the 3rd fluidized-bed reactor, obtain the graphitized carbon black of low cost, polymolecularity, high-graphitized and high conduction performance, and purified hydrogen.
2. the preparation method of a kind of graphitized carbon black according to claim 1 and purified hydrogen is characterized in that: adopt lower temperature plasma technology, the temperature of low-temperature plasma is between 1000～2600 ℃.Can reach purpose of energy saving, electrode materials and refractory materials are not fragile.
3. the preparation method of a kind of graphitized carbon black according to claim 1 and purified hydrogen, it is characterized in that: employing hydrogen is carrier gas, wherein add gaseous hydrocarbon, the mol ratio of carbon source and hydrogen is between 1: 0.5～1: 5, add the hydrocarbon polymer of secondary in the plasma tail flame, carry out scission reaction.Can produce purified clean energy: hydrogen; Simultaneously, can also reduce the generation of carbon distribution.
4. the preparation method of a kind of graphitized carbon black according to claim 1 and 2 and purified hydrogen is characterized in that: adopt high-voltage and low current.Can reach thermo-cracking and highfield cracking simultaneously, save energy; Reach discharge stability simultaneously, be difficult for current interruption; Can also reduce electrode damage.
5. according to the preparation method of claim 1 or 4 described a kind of graphitized carbon blacks and purified hydrogen, it is characterized in that: gas adopts high-speed in the plasma generator, and reaction time is between 0.01～0.3 second, to reduce carbon distribution.
6. the preparation method of a kind of graphitized carbon black according to claim 1 and purified hydrogen is characterized in that: adopt fluidized-bed reactor, the residence time of gas in this reactor is longer, and mean residence time can reach the several seconds, can increase transformation efficiency; The carbon black residence time therein several seconds between several minutes, carbon black has full-blown structure, conducts electricity very well.
7. according to the preparation method of claim 1 or 4 described a kind of graphitized carbon blacks and purified hydrogen, it is characterized in that: discharging gap is several millimeters to tens of centimetres, the current interruption that causes to reduce carbon distribution.
8. the preparation method of a kind of graphitized carbon black according to claim 1 and purified hydrogen, it is characterized in that: the method that adopts multiple plasma generator and fluidized-bed reactor to be in series, the hydrogen carrier gas circulation of inter-stage hydrocarbon-containiproducts reaches reactant utilization ratio height, can obtain purified hydrogen.
9. according to the preparation method of claim 1 or 4 described a kind of graphitized carbon blacks and purified hydrogen, it is characterized in that: adopt a kind of or its combination of needle point discharge, needle plate discharge, needle ring discharge, dull and stereotyped discharge or slip arc-over, to improve discharging efficiency, increase reaction-ure conversion-age, to reduce export license or electrode carbon distribution.
10. the preparation method of a kind of graphitized carbon black according to claim 1 and purified hydrogen, it is characterized in that: adopt the carrier gas of discharge tail gas preheating hydrogen, not only reclaim heat, all right stable plasma, increase the transformation efficiency of reactant, obtain more purified hydrogen.
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