CN102491308A - Method for synthesis of carbon nanostructure material by using organic material - Google Patents
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Abstract
The invention discloses a method for synthesis of a carbon nanostructure material by using an organic material. According to the method, a solid organic waste material is subjected to thermal cracking to obtain one or more gaseous carbon-containing monomers of the organic waste material; combustion-supporting gas is added to carry out complete mixing combustion to generate mixed gas containing carbon dioxide, carbon monoxide and hydrogen; after a high temperature filtration treatment is performed, the treated mixed gas is introduced into a tube type furnace to be converted into the carbon nanostructure material, and the high heat value combustible gas generated during the reaction process is collected as a by-product. With the technical scheme, the thermal cracking treatment is adopted to decompose the solid organic waste with the organic polymer form into the solid organic waste with the organic monomer form, such that the carbon source in the organic monomer is synthesized into the carbon nanostructure material under the effect of the catalyst; the preparation method is simple, the synthetic steps and the process are easy to control, the raw materials adopted by synthesis are sufficient, and the cost is low; concurrently the by-product generated during the synthesis process is the combustible gas with the high heat value, and the combustible gas can be recovered as the supplement for energy consumption during the reaction process.
Description
Technical field
The present invention relates to the preparation method of carbon nano-structured material; Relate in particular to and utilize life and solid organic castoffs such as industrial plastics waste, rubber tyre waste and biomass waste; Under the effect of high temperature and catalyzer, with the method for organism synthesis of carbon nanostructures material.
Background technology
Carbon nanotube, homoatomics such as carbon black and Graphene abnormity nano structural material has excellent heat conduction, and conduction and mechanical property can be widely used in nanosecond science and technology, electronics, optics and fields such as Materials science and technology.Carbon nano-structured material compound method commonly used comprises arc-over, laser ablation, high pressure carbon monoxide, flame is synthetic and chemical vapour deposition etc.Present compound method need consume the hydrocarbon polymer and the highly flammable chemical of a large amount of costlinesses, such as hydrogen (H2).Therefore, along with carbon nano-structured material extensive popularized its application, preparation just needs to consider continuable raw material supply and safety and controllable preparation method more.The method of a kind of polyolefine compound/carbon nano pipe that burns of one Chinese patent application number 200410011337.9 introductions; 200610016733.X the method for the synthesizing nanometer carbon pipe by cracking polymer of introducing; Though 200810019267.X introduce a kind ofly have lower-cost advantage through preparing the method that alpha zirconium phosphate catalyst carbonizing polymer prepares carbon nanotube; Above preparation method only is confined to use the petroleum base polymkeric substance; And can't accurately control reaction conditions because of it, cause it can't optionally synthesize quality controllable carbon nanomaterial.In addition, in these preparing method's courses of processing,, be unfavorable for large-scale industrial production, also do not meet environmental requirement owing to, in building-up process, can produce a large amount of uncontrollable soots not with fuel and air thorough mixing.A kind of method of utilizing biomass residue to prepare the high-ratio surface micro-pore carbon material that number of patent application 200910099470.7 is introduced; 201110023855.2 a kind of method of utilizing biodegradable plastic to prepare carbon nanotube of introducing; Though using biomass or bio-based polymers to prepare carbon nano-structured material as carbon source, these can reduce requirement to reaction conditions; Simplified process equipment; But its conversion process is based on the solid-state solid-state thaumatropy that arrives, and has limited its application to other carbon back waste, need carry out large-scale process modification and just can meet industrial production requirement.
Along with the progress of fast development of Chinese economy with society, the people also constantly consume increasing resource when improving constantly standard of living, produce increasing life and industrial waste simultaneously.What among this, account for significant proportion is carbonaceous organic waste, such as waste plastic, and waste rubber tire, and biomass waste.Wherein have only a fraction of organic waste to realize utilizing again, and its major part all is to handle through the mode of landfill and burning through reclaiming.With the minimizing day by day in soil capable of using, handling organic waste through landfill at last can't be as a kind of solution of Sustainable development.Adopt the burning disposal solid organic castoff, take up an area of huge problem though can solve refuse, simple is to have ignored such fact fully with its burning: these carbonaceous organic wastes are ten minutes fine starting material in fact.Such as the waste plastic as petroleum product, its energy of containing is that the energy with gasoline (perhaps coal) is suitable.Considering from the angle of practicing thrift earth resources, go out high value-added product through utilizing these solid organic castoffs as raw material production, is crucial.
Summary of the invention
The purpose of this invention is to provide a kind of limitation that existing carbon nano-structured material uses the carbon back starting material in synthetic that overcomes, the method for utilizing organism synthesis of carbon nanostructures material of the more perfect solution route that organic waste is turned waste into wealth can be provided simultaneously.
The present invention adopts following technical scheme, and the concrete steps of carbon nano-structured material preparation are following:
At first, the solid organic castoff fragmentation is placed in the heating tube, is feeding rare gas element in the temperature more than 300 ℃, under starvation, carry out thermo-cracking, produce the mixture of gaseous hydrocarbon;
Secondly, in mixture, behind the adding combustion-supporting gas thorough mixing, at high temperature burn, produce the mixed gas of carbonated, carbon monoxide and hydrogen 20-50%;
Again secondly, the gained mixed gas is imported a strainer, obtain being used for the reactant gases of synthesize nano carbon material after the filtration;
At last; Output terminal at strainer is provided with tube furnace, and tube furnace is provided with two-layer above alloyed metal nethike embrane as catalyzer, is heated to more than 400 ℃; Above-mentioned reactant gases is through alloyed metal nethike embrane array in the tube furnace, the carbon nano-structured material of promptly synthetic black.
The carbon nano-structured material of described acquisition is scraped from the alloyed metal nethike embrane and to be got when being cooled to below 200 ℃, obtains the flaky two-dimentional Graphene carbon nano-structured material of pulverous tubulose one dimension carbon nano-structured material or powder.
Described solid organic castoff is Vilaterm, Vestolen PP 7052, PS, polyethyleneterephthalate, polyethyleneterephthalate, SE, POLYACTIC ACID, polyester, urethane, polycarbonate, polymeric amide, acrylonitrile-styrene-butadienecopolymer, polymethylmethacrylate, ethylene-vinyl acetate copolymer, tree elastomer, styrene-butadiene rubber(SBR), bagasse, corn, distiller's dried grain and solvend thereof.
Described rare gas element is argon gas or carbonic acid gas.
The mixture staple of described gaseous hydrocarbon is methane, ethane, ethene, acetylene, benzene and hydrogen.
Described combustion-supporting gas is one or more the mixed gas in oxygen, nitrogen, argon gas, carbonic acid gas, the water vapour, the perhaps mixed gas of one or more in hydrogen, nitrogen, argon gas, carbonic acid gas, the water vapour.
The material of described alloyed metal nethike embrane is ferrous alloy or copper base alloy, and it comprises iron, nickel, cobalt, manganese, copper.
Described solid organic castoff fragment is that bulk or the big solid organic castoff of sheet caking ability are cut into strip, and the solid organic castoff that caking ability is big is ground into particle.
It is described that in mixture, to add the combustion-supporting gas thorough mixing be to betide in the venturi tube.
Described mixed gas imports a strainer, and the high heating value inflammable gas of the remainder that is filtered is a sub product.
The present invention adopts above technical scheme, utilizes the anaerobic thermo-cracking that solid organic castoff is decomposed into the form of organic monomer from the form of organic polymer, and then the carbon source in the organic monomer is synthesized carbon nano-structured material under the alloyed metal catalyst action; The method for preparing carbon nano-structured material is simple; Synthetic step and process are controlled easily, the time of a building-up process about 1 minute, its to the transformation efficiency of solid-state carbon source more than 10%; And the synthetic raw material that is adopted is sufficient; With low cost, the sub product that produces in building-up process simultaneously is the inflammable gas with high heating value, can it be reclaimed replenishing as energy consumption in the reaction process.The present invention not only provides the novel method of low-cost preparation nano structural material, but also the new way of handling solid organic castoff is provided.
Description of drawings
Combine accompanying drawing that the present invention is done further detailed description at present:
Fig. 1 is the sem photograph of the embodiment of the invention 1 synthetic carbon nano-structured material;
Fig. 2 is the sem photograph of the embodiment of the invention 2 synthetic carbon nano-structured materials;
Fig. 3 is the transmission electron microscope picture of the embodiment of the invention 2 synthetic carbon nano-structured materials;
Fig. 4 is the transmission electron microscope picture of the embodiment of the invention 3 synthetic carbon nano-structured materials.
Embodiment
The concrete steps of carbon nano-structured material preparation of the present invention are following:
At first, the solid organic castoff fragmentation is placed in the heating tube, is feeding rare gas element in the temperature more than 300 ℃; Described rare gas element is argon gas or carbonic acid gas, under starvation, carries out thermo-cracking, produces the mixture of gaseous hydrocarbon; The mixture staple of described gaseous hydrocarbon is a methane, ethane, ethene; Acetylene, benzene and hydrogen.Described solid organic castoff is Vilaterm, Vestolen PP 7052, PS, polyethyleneterephthalate, polyethyleneterephthalate, SE, POLYACTIC ACID, polyester, urethane, polycarbonate, polymeric amide, acrylonitrile-styrene-butadienecopolymer, polymethylmethacrylate, ethylene-vinyl acetate copolymer, tree elastomer, styrene-butadiene rubber(SBR), bagasse, corn, distiller's dried grain and solvend thereof.The solid organic castoff fragment is that bulk or the big solid organic castoff of sheet caking ability are cut into strip, and the solid organic castoff that caking ability is big is ground into particle.
Secondly, in mixture, behind the adding combustion-supporting gas thorough mixing, at high temperature burn, produce the mixed gas of carbonated, carbon monoxide and hydrogen 20-50%; In mixture, adding the combustion-supporting gas thorough mixing can betide in the venturi tube.Combustion-supporting gas is one or more the mixed gas in oxygen, nitrogen, argon gas, carbonic acid gas, the water vapour, the perhaps mixed gas of one or more in hydrogen, nitrogen, argon gas, carbonic acid gas, the water vapour.
Again secondly, the gained mixed gas is imported a strainer, obtain being used for the reactant gases of synthesize nano carbon material after the filtration, and the high heating value inflammable gas of the remainder that is filtered, can be used as sub product.
At last, at the output terminal of strainer tube furnace is set, tube furnace is provided with two-layer above alloyed metal nethike embrane as catalyzer, and the material of alloyed metal nethike embrane is ferrous alloy or copper base alloy, and it comprises iron, nickel, cobalt, manganese, copper.It is preheated to more than 400 ℃, and above-mentioned reactant gases is through alloyed metal nethike embrane array in the tube furnace, the carbon nano-structured material of promptly synthetic black.
The carbon nano-structured material of described acquisition is scraped from the alloyed metal nethike embrane and to be got when being cooled to below 200 ℃, obtains the flaky two-dimentional Graphene carbon nano-structured material of pulverous tubulose one dimension carbon nano-structured material or powder.
Embodiment 1
Temperature is set to 300 ℃ in the high-temperature cracking furnace, and silica tube is placed in the stove, and the argon gas (perhaps carbonic acid gas) that in pipe, feeds 5 liters of PMs is as rare gas element.The waste plastic bottle cap that the Vestolen PP 7052 of 1 gram is made is cut into 20 * 60 millimeters strip, it is positioned in the silica tube, under the environment of starvation with its thermo-cracking.
The solid high density poly propylene is decomposed into the mixture of the gaseous hydrocarbon of high heating value fully through Pintsch process, and its staple is methane, ethane, ethene, propane, propylene and acetylene.With one or more the mixed gas in this mixture and oxygen, nitrogen, argon gas, carbonic acid gas, the water vapour after the venturi tube of the end of this silica tube is carried out thorough mixing; At high temperature ignite automatically; Produce 12% carbonic acid gas, 20% carbon monoxide and 8% hydrogen.
After combustion reactions finishes, this products of combustion is imported a strainer, products of combustion is filtered, and then obtain to be used for the reactant gases of synthesize nano carbon material.
Placing another at the output terminal of strainer preheats to 900 ℃ silica tube; With unit surface is that 50 section 304 stainless steel nethike embrane of 4 square centimeters is positioned in this silica tube, just available catalyst surface area is increased to 480 square centimeters thus, and described catalyzer is a ferrous alloy; It is characterized in that ferro element is the staple of catalyzer; Other alloying constituent comprises nickel, cobalt, manganese etc.It is preheated to 900 ℃.The reactant gases water conservancy diversion through this catalyst array, has been increased the total mass of synthesis of carbon nanostructures material thus.In a batch process, in 25 seconds time, utilize the waste plastic bottle cap of 1 gram can synthesize 80 milligrams tubulose one dimension carbon nano-structured material.Described life and industrial solid plastic are Vilaterm, Vestolen PP 7052, PS, polyethyleneterephthalate; Polyethyleneterephthalate, SE, POLYACTIC ACID, polyester; Urethane, polycarbonate, polymeric amide; Acrylonitrile-styrene-butadienecopolymer, polymethylmethacrylate, ethylene/vinyl acetate copolymer.After reaction finishes, continue to feed argon gas reaction unit is cooled to below 200 ℃, can this catalyst array be taken out.The synthetic black product that obtains covers catalyst surface equably, can obtain pulverous tubulose one dimension carbon nano-structured material through scraping to get.
As shown in Figure 1, the sem photograph of present embodiment product, as can be seen from the figure, the product of present embodiment mainly is made up of fibrous carbon nanotube, and its diameter mainly is distributed between 20 to 100 nanometers, in 2 to 6 microns of length distribution.
Embodiment 2
Temperature is set to 600 ℃ in the high-temperature cracking furnace, and silica tube is placed in the stove, and the argon gas (perhaps carbonic acid gas) that in pipe, feeds 3 liters of PMs is as rare gas element.The bagasse fibre of 4 grams is pulverized to size is lower than 500 microns particle and it is positioned in the silica tube, under the environment of starvation with its thermo-cracking.
The solid bagasse fibre is decomposed into the mixture of the gaseous hydrocarbon of high heating value fully through Pintsch process, and its staple is carbon monoxide, methane, ethene, ethane and acetylene.The mixed gas of one or more in venturi tube place feeding hydrogen, nitrogen, argon gas, carbonic acid gas, water vapour fully dilutes these hot pyrolysis gas; And then with strainer of its importing; The gas that is imported is filtered, and then obtain to be used for the reactant gases of synthesize nano carbon material.
Placing another at the output terminal of strainer and preheat to 900 ℃ silica tube, in the synthetic operation of carbon nano-structured material, is that 50 section 304 stainless steel nethike embrane of 4 square centimeters is positioned in the same silica tube with unit surface; Just available catalyst surface area is increased to 480 square centimeters thus; Described catalyzer is a ferrous alloy, it is characterized in that ferro element is the staple of catalyzer, and other alloying constituent comprises nickel; Cobalt, manganese etc.It is preheated to 900 ℃.The reactant gases water conservancy diversion through this catalyst array, has been increased the total mass of synthesis of carbon nanostructures material thus.In a batch process, in 100 seconds time, utilize the bagasse fibre (or other biomass solid waste) of 4 grams can synthesize 350 milligrams one dimension tubulose carbon nano-structured material.Said biomass solid waste is a bagasse, corn distiller's dried grain and solvend.After reaction finishes, continue to feed argon gas reaction unit is cooled to below 200 ℃, can this catalyst array be taken out.The synthetic black product that obtains covers catalyst surface equably, can obtain pulverous tubulose one dimension carbon nano-structured material through scraping to get.
Fig. 2 has provided the sem photograph of present embodiment product, and as can be seen from the figure, the product of present embodiment mainly is made up of fibrous carbon nanotube, and its diameter mainly is distributed between 50 to 100 nanometers, between in 50 to 100 microns of the length distribution.Fig. 3 has provided the transmission electron microscope picture of present embodiment product, and as can be seen from the figure, the product of present embodiment mainly is made up of fibrous carbon nanotube.
Embodiment 3
Temperature is set to 600 ℃ in the high-temperature cracking furnace, and silica tube is placed in the stove, and the argon gas (perhaps carbonic acid gas) that in pipe, feeds 3 liters of PMs is as rare gas element.The bagasse fibre of 4 grams is pulverized to size is lower than 500 microns particle and it is positioned in the silica tube, under the environment of starvation with its thermo-cracking.
The solid bagasse fibre is decomposed into the mixture of the gaseous hydrocarbon of high heating value fully through Pintsch process, and its staple is carbon monoxide, methane, ethene, ethane and acetylene.The mixed gas of one or more in venturi tube place feeding hydrogen, nitrogen, argon gas, carbonic acid gas, water vapour fully dilutes these hot pyrolysis gas; And then with strainer of its importing; The gas that is imported is filtered, and then obtain to be used for the reactant gases of synthesize nano carbon material.
Placing another at the output terminal of strainer preheats to 1050 ℃ silica tube; In the synthetic operation of carbon nano-structured material; With unit surface is that 50 sections fine copper membrane array of 4 square centimeters are positioned in the same silica tube; Just available catalyst surface area is increased to 200 square centimeters thus, it is preheated to 1050 ℃.The reactant gases water conservancy diversion through this catalyst array, has been increased the total amount of synthesis of carbon nanostructures material thus.In a batch process, in 100 seconds time, utilize the bagasse fibre (or other biomass solid waste) of 4 grams can Synthetic 2 00 square centimeter two-dimentional Graphene carbon nano-structured material.Said biomass solid waste is a bagasse, corn distiller's dried grain and solvend.After reaction finishes, continue to feed argon gas reaction unit is cooled to below 200 ℃, can this catalyst array be taken out.The synthetic transparent products that obtains covers catalyst surface equably, can it be peeled off from catalyst surface through UW.
Fig. 4 has provided the transmission electron microscope picture of present embodiment product, and as can be seen from the figure, the product of present embodiment mainly is made up of lamellated carbon graphite alkene, and its area is between 1 to 10 square micron.
Embodiment 4
Temperature is set to 950 ℃ in the high-temperature cracking furnace, and silica tube is placed in the stove, and the argon gas (perhaps carbonic acid gas) that in pipe, feeds 5 liters of PMs is as rare gas element.The waste tire of automobile of 1 gram is cut into 20 * 80 millimeters strip, it is positioned in the silica tube, under the environment of starvation with its thermo-cracking.
Waste tire of automobile is decomposed into the mixture of the gaseous hydrocarbon of high heating value fully through Pintsch process, and its staple is methane, ethene, acetylene and benzene.With one or more the mixed gas in this mixture and oxygen, nitrogen, argon gas, carbonic acid gas, the water vapour after the venturi tube of the end of this silica tube is carried out thorough mixing; At high temperature ignite automatically; Produce 9% carbonic acid gas, 13% carbon monoxide and 3% hydrogen.
After combustion reactions finishes, this products of combustion is imported a strainer, products of combustion is filtered, and then obtain to be used for the reactant gases of synthesize nano carbon material.
Placing another at the output terminal of strainer and preheat to 400 ℃ silica tube, in this operation, is that 50 section 304 stainless steel nethike embrane of 4 square centimeters is positioned in the same silica tube with unit surface; Just available catalyst surface area is increased to 480 square centimeters thus; Described catalyzer is a ferrous alloy, it is characterized in that ferro element is the staple of catalyzer, and other alloying constituent comprises nickel; Cobalt, manganese etc.It is preheated to 850 ℃.The reactant gases water conservancy diversion through this catalyst array, has been increased the total mass of synthesis of carbon nanostructures material thus.In a batch process, in 25 seconds time, utilize the waste tire of automobile of 1 gram can synthesize 40 milligrams one dimension tubulose carbon nano-structured material.Said industrial solid solid waste comprises tree elastomer, styrene-butadiene rubber(SBR).After reaction finishes, continue to feed argon gas reaction unit is cooled to below 200 ℃, can this catalyst array be taken out.The synthetic black product that obtains covers catalyst surface equably, can obtain pulverous tubulose one dimension carbon nano-structured material through scraping to get.
Claims (11)
1. method of utilizing organism synthesis of carbon nanostructures material is characterized in that: the concrete steps of its carbon nano-structured material preparation are following:
At first, the solid organic castoff fragmentation is placed in the heating tube, is feeding rare gas element in the temperature more than 300 ℃, under starvation, carry out thermo-cracking, produce the mixture of gaseous hydrocarbon;
Secondly, in mixture, behind the adding combustion-supporting gas thorough mixing, at high temperature burn, produce the mixed gas of carbonated, carbon monoxide and hydrogen 20-50%;
Again secondly, the gained mixed gas is imported a strainer, obtain being used for the reactant gases of synthesize nano carbon material after the filtration;
At last; Output terminal at strainer is provided with tube furnace, and tube furnace is provided with two-layer above alloyed metal nethike embrane as catalyzer, is heated to more than 400 ℃; Above-mentioned reactant gases is through alloyed metal nethike embrane array in the tube furnace, the carbon nano-structured material of promptly synthetic black.
2. the method for utilizing organism synthesis of carbon nanostructures material according to claim 1; It is characterized in that: the carbon nano-structured material of described acquisition is when being cooled to below 200 ℃; Scrape from the alloyed metal nethike embrane and to get, obtain pulverous tubulose one dimension carbon nano-structured material.
3. the method for utilizing organism synthesis of carbon nanostructures material according to claim 1; It is characterized in that: the carbon nano-structured material of described acquisition is when being cooled to below 200 ℃; Scrape from the alloyed metal nethike embrane and to get, it is carbon nano-structured to obtain the flaky planar Graphene of powder.
4. the method for utilizing organism synthesis of carbon nanostructures material according to claim 1; It is characterized in that: described solid organic castoff is Vilaterm, Vestolen PP 7052, PS, polyethyleneterephthalate, polyethyleneterephthalate, SE, POLYACTIC ACID, polyester, urethane, polycarbonate, polymeric amide, acrylonitrile-styrene-butadienecopolymer, polymethylmethacrylate, ethylene-vinyl acetate copolymer, tree elastomer, styrene-butadiene rubber(SBR), bagasse, corn, distiller's dried grain and solvend thereof.
5. the method for utilizing organism synthesis of carbon nanostructures material according to claim 1 is characterized in that: described rare gas element is argon gas, nitrogen or carbonic acid gas.
6. the method for utilizing organism synthesis of carbon nanostructures material according to claim 1 is characterized in that: the mixture staple of described gaseous hydrocarbon is methane, ethane, ethene, acetylene, benzene and hydrogen.
7. the method for utilizing organism synthesis of carbon nanostructures material according to claim 1; It is characterized in that: described combustion-supporting gas is one or more the mixed gas in oxygen, nitrogen, argon gas, carbonic acid gas, the water vapour, the perhaps mixed gas of one or more in hydrogen, nitrogen, argon gas, carbonic acid gas, the water vapour.
8. the method for utilizing organism synthesis of carbon nanostructures material according to claim 1 is characterized in that: the material of described alloyed metal nethike embrane is ferrous alloy or copper-based material, and it comprises iron, nickel, cobalt, manganese, copper.
9. the method for utilizing organism synthesis of carbon nanostructures material according to claim 1; It is characterized in that: described solid organic castoff fragment is that bulk or the big solid organic castoff of sheet caking ability are cut into strip, and the solid organic castoff that caking ability is big is ground into particle.
10. the method for utilizing organism synthesis of carbon nanostructures material according to claim 1 is characterized in that: described in mixture, to add the combustion-supporting gas thorough mixing be to betide in the venturi tube.
11. the method for utilizing organism synthesis of carbon nanostructures material according to claim 1 is characterized in that: described mixed gas imports strainer, and the high heating value inflammable gas of the remainder that is filtered is a sub product.
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