CN111017926A - Method and device for preparing magnetic carbon nanotube/porous carbon material by using green environment-friendly biomass - Google Patents
Method and device for preparing magnetic carbon nanotube/porous carbon material by using green environment-friendly biomass Download PDFInfo
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- CN111017926A CN111017926A CN201911245269.5A CN201911245269A CN111017926A CN 111017926 A CN111017926 A CN 111017926A CN 201911245269 A CN201911245269 A CN 201911245269A CN 111017926 A CN111017926 A CN 111017926A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
- B01J21/185—Carbon nanotubes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/16—Preparation
- C01B32/162—Preparation characterised by catalysts
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/39—Apparatus for the preparation thereof
Abstract
The invention discloses a method and a device for preparing a magnetic carbon nano tube/porous carbon material by using green and environment-friendly biomass. And (3) feeding the dried raw material into a paddle type carbonization furnace for carbon thermal reduction, wherein a pyrolysis solid product is the magnetic carbon nano tube/porous carbon material. And meanwhile, the generated volatile combustible gas is filtered by a calcium oxide filter to be acid gas, then is combusted by a combustor, exchanges heat with a molten salt boiler, and the waste gas and the molten salt after heat exchange are respectively used as heat sources of a dryer and a carbonization furnace. The device recovers heat generated by combustion of pyrolysis gas as a heat source for drying and pyrolyzing the raw materials, the whole system does not need external heat supply, and utilizes molten salt for heat supply, so that the accurate temperature control of the carbonization furnace is realized, and meanwhile, the quality of the magnetic carbon material is improved by adopting the biomass in-situ loaded metal salt.
Description
Technical Field
The invention relates to the field of biomass pyrolysis, and relates to a method and a device for preparing a magnetic carbon nano tube/porous carbon material from green and environment-friendly biomass.
Background
The excessive exploitation and use of the traditional fossil energy aggravates the environmental pollution and the exhaustion of resources, and the development and utilization of renewable energy are important problems which need to be solved urgently in the human society. Biomass energy has the characteristics of abundant reserves, easy acquisition, renewability, low pollution and the like, and is considered as an important renewable energy source.
Biomass generally refers to natural plants or plant-based materials. According to statistics, the production of biomass in the world can reach more than 1000 hundred million tons every year. China, as a big agricultural country, also produces a large amount of biomass every year, and the rest is simply buried or burned except for satisfying the eating and use of people. The treatment method not only causes resource waste, but also causes certain environmental pollution. Therefore, in order to increase the utilization value of biomass, gas, biodiesel, carbon materials, and the like can be produced using biomass. Not only realizes the improvement of the economic value of the biomass, but also relieves the problems of environmental pollution and energy.
The biomass carbon material is generally prepared by treating the biomass carbon material at a high temperature in an oxygen-free environment to retain carbon elements in the biomass, thereby obtaining the biomass carbon material. The biomass has the characteristics of high carbon content, rich pore structure and the like, so that the method for preparing the carbon material by using the biomass has obvious advantages. The carbon material prepared by the biomass has high yield, large specific surface area, heteroatom doping and the like. Meanwhile, the prepared carbon material can be used as a carrier of a catalyst, a material for energy storage and conversion, an adsorbent and the like. The utilization value of the biomass raw material can be improved, and a new idea is provided for the development of sustainable energy.
Disclosure of Invention
Aiming at the prior art, the method and the device for preparing the magnetic carbon nano tube/porous carbon by using the green and environment-friendly biomass are provided, and the high-quality composite carbon material can be processed and prepared by using the biomass raw material and combining metal salts of Fe and Ni.
A method for preparing a magnetic carbon nano tube/porous carbon material by using green environment-friendly biomass comprises the following steps: feeding the biomass raw material into a double-helix stirrer, and stirring and mixing a metal salt solution of iron and nickel with the biomass raw material through a solution pump and a nozzle; drying the mixed raw materials until the water content is 5-10%; the dried raw materials enter a paddle type carbonization furnace for carbothermic reduction, the pyrolysis temperature is controlled to be 600 +/-10 ℃, solid products generated in the pyrolysis are discharged through the carbonization furnace so as to obtain a magnetic carbon nano tube/porous carbon material, and combustible gas generated in the pyrolysis enters a combustor for combustion after acid gas generated by mixing with a metal salt solution is removed through a calcium oxide filter;
the high-temperature flue gas after combustion exchanges heat through a molten salt boiler, the heated molten salt is used as a heat source of the paddle type carbonization furnace, and the waste gas after heat exchange is used as a heat source of the drum dryer.
The prepared magnetic carbon nanotube/porous carbon material is an internal porous carbon, an external carbon nanotube composite structure, and a metal salt solution is used as an activating agent to promote the generation of a catalyst porous structure, and in the carbothermic reduction process, the generation of hydrocarbon volatile components is promoted, the hydrocarbon volatile components are subjected to vapor deposition on the surface of a metal active site to generate the carbon nanotube, and nano metal particles are embedded and uniformly dispersed in the carbon-based material.
The paddle type carbonization furnace is heated by using the molten salt boiler, the molten salt which provides a heat source for the carbonization furnace is heated by using the molten salt boiler, the inlet temperature of the molten salt is about 650 ℃, the outlet temperature of the molten salt is about 550 ℃, the accurate temperature control of the carbonization furnace is realized, the pyrolysis temperature of the raw material in the paddle type carbonization furnace is kept unchanged, and the molten salt is heated and flows back to the liquid storage tank through the molten salt pump to realize repeated heat exchange.
Waste gas generated after heat exchange of the high-temperature flue gas after combustion in the molten salt boiler is used as a heat source to supply heat to the drum dryer, and the temperature is 200-300 ℃.
The device for preparing the magnetic carbon nano tube/porous carbon material by using the biomass comprises a metal salt solution storage tank, a solution pump, a double-helix stirring machine, a drum dryer, a carbonization furnace, a calcium oxide filter, a burner, a fan, a molten salt boiler, a molten salt storage tank and a molten salt pump;
the double-helix stirrer comprises a raw material inlet, a nozzle and a material outlet; the drum dryer comprises a material inlet, a material outlet, a gas inlet and a waste gas outlet; the paddle type carbonization furnace comprises a material inlet, a molten salt outlet and a gas outlet; the calcium oxide dryer comprises a gas inlet, a gas outlet, a calcium oxide inlet and a calcium oxide outlet; the molten salt boiler comprises a gas outlet, a molten salt inlet and a molten salt outlet;
the outlet of the metal salt liquid storage tank is connected with a solution pump, the solution pump is connected with a nozzle of a double-helix stirring machine, the discharge port of the double-helix stirring machine is connected with the feed inlet of a drum dryer, the discharge port of the drum dryer is connected with the feed inlet of a paddle type carbonization furnace, the gas outlet of the carbonization furnace is connected with the inlet of a calcium chloride filter, the gas outlet of the filter is connected to a molten salt boiler through a burner, and the waste gas outlet of the molten salt boiler is connected with the gas inlet of the drum dryer;
the fused salt liquid storage pot links to each other with fused salt boiler's fused salt entry, and fused salt boiler's export links to each other with the fused salt entry of paddle formula carbide furnace, and carbide furnace's fused salt export links to each other with the fused salt pump, and the fused salt pump links to each other with the fused salt liquid storage pot.
Compared with the prior art, the invention has the following remarkable advantages: (1) the biomass is used for carrying metal salt in situ, and the metal salt solution is used as an activating agent, so that the generation of a porous structure of the catalyst is promoted on one hand. On the other hand, during the carbothermic reduction process, the generation of hydrocarbon volatile components is promoted, carbon nano-tubes are generated on the surface of the metal active sites through vapor deposition, and nano-metal particles are embedded and uniformly dispersed in the carbon-based material, so that the carbon material is an external carbon nano-tube/internal porous carbon composite carbon material; (2) a fused salt boiler is adopted to supply heat to the paddle type carbonization furnace, the pyrolysis temperature of the carbonization furnace is controlled to be 600 +/-10 ℃, and the recycling of fused salt is realized; (3) the heat generated by the combustion of combustible gas generated by reaction is utilized to realize the heat supply of the whole system, the whole system device realizes the gradient utilization of energy, external energy supply is basically not needed, and the system has high operation safety and low cost.
Drawings
FIG. 1 is a structural diagram of an apparatus for preparing magnetic carbon nanotubes/porous carbon materials from green and environment-friendly biomass according to the present invention.
In the figure: 1-a metal salt liquid storage tank, 2-a solution pump, 3-a double-screw mixer material inlet, 4-a nozzle, 5-a double-screw mixer, 6-a double-screw mixer material outlet, 7-a drum dryer material inlet, 8-a drum dryer, 9-a drum dryer gas inlet and 10-a drum dryer waste gas outlet. 11-material outlet of drum dryer, 12-material inlet of paddle type carbonization furnace, 13-paddle type carbonization furnace, 14-fused salt outlet of paddle type carbonization furnace, 15-fused salt inlet of paddle type carbonization furnace, 16-pyrolysis gas outlet, 17-gas inlet of calcium oxide dryer, 18-calcium oxide dryer, 19-gas outlet of calcium oxide dryer, 20-inlet of calcium oxide, 21-outlet of calcium oxide, 22-burner, 23-blower, 24-fused salt boiler, 25-fused salt inlet of boiler, 26-fused salt outlet of boiler, 27-waste gas outlet of fused salt boiler, 28-fused salt storage tank and 29-fused salt pump.
Detailed Description
The invention is further explained below with reference to the drawings.
As shown in fig. 1, the apparatus for preparing magnetic carbon nanotube/porous carbon material from green environmental protection biomass comprises: a metal salt solution storage tank 1, a solution pump 2, a double-helix stirring machine 5, a drum-type dryer 8, a blade type carbonization furnace 13, a calcium oxide dryer 18, a combustor 22, a fan 23, a molten salt boiler 24, a molten salt storage tank 28 and a molten salt pump 29;
the export of metal salt liquid storage pot 1 links to each other with solution pump 2, solution pump 2 links to each other with double helix mixer 5's nozzle, the pan feeding mouth 7 of drum dryer 8 is connected to double helix mixer 5's discharge gate 6, the pan feeding mouth 12 of paddle formula carbide furnace 13 is connected to drum dryer's discharge gate 11, the gas outlet 16 of carbide furnace links to each other with the entry 17 of calcium chloride filter 18, the gas outlet 19 of filter is connected to fused salt boiler 24 through combustor 22, fused salt boiler's exhaust outlet 27 links to each other with drum dryer 8's gas inlet 9.
The molten salt storage tank 28 is connected with a molten salt inlet 25 of the molten salt boiler 24, an outlet 26 of the molten salt boiler is connected with a molten salt inlet 15 of the paddle-type carbonization furnace 13, a molten salt outlet 14 of the carbonization furnace is connected with a molten salt pump 29, and the molten salt pump is connected with the molten salt storage tank 28.
The method for preparing the magnetic carbon nano tube/porous carbon material by using the green environment-friendly biomass comprises the following specific steps: sending the wood chips of the biomass raw material into a double-helix stirrer 5, and fully stirring and mixing the chloride solution of iron and nickel metal with the biomass raw material through a solution pump 2 and a nozzle 4; the mixed raw materials are sent into a roller type dryer 8 to be dried at about 200 ℃ until the water content is 5-10%; the dried raw material enters a paddle type carbonization furnace 13 for carbothermic reduction, the pyrolysis temperature is controlled to be 600 +/-10 ℃, the pyrolysis time is 2 hours, a solid product generated in the pyrolysis is discharged through the carbonization furnace to obtain a magnetic carbon nano tube/porous carbon material, and combustible gas generated in the pyrolysis enters a combustor 22 for combustion after hydrogen chloride gas generated by mixing with a metal salt solution is removed through a calcium oxide filter 18.
Wherein, the burning high temperature flue gas exchanges heat through the fused salt boiler 24, so that the fused salt temperature reaches 650 ℃, the heated fused salt is used as the heat source of the paddle type carbonization furnace 13, and the waste gas after heat exchange is used as the heat source of the roller type dryer 8.
A method for preparing a magnetic carbon nano tube/porous carbon material from green environment-friendly biomass comprises the steps of firstly stirring and mixing a biomass raw material with a metal salt solution through a double-helix stirrer, drying after in-situ loading of Fe and Ni elements, then carrying out carbothermic reduction on the dried raw material in a carbonization furnace, wherein the generated carbon material is an internal porous carbon and external carbon nano tube composite structure, and nano metal particles are embedded and uniformly dispersed in the carbon-based material. Meanwhile, the invention recovers the energy generated by the combustion of the pyrolysis gas as a heat source for drying and pyrolyzing the raw materials, and the whole system does not need external heat supply.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and these improvements and modifications should be construed as being within the scope of the present invention.
Claims (5)
1. A method for preparing a magnetic carbon nano tube/porous carbon material by using green environment-friendly biomass is characterized by comprising the following steps: the method comprises the following steps: feeding the biomass raw material into a double-helix stirrer, and stirring and mixing a metal salt solution of iron and nickel with the biomass raw material through a solution pump and a nozzle; drying the mixed raw materials until the water content is 5-10%; the dried raw materials enter a paddle type carbonization furnace for carbothermic reduction, the pyrolysis temperature is controlled to be 600 +/-10 ℃, solid products generated in the pyrolysis are discharged through the carbonization furnace so as to obtain a magnetic carbon nano tube/porous carbon material, and combustible gas generated in the pyrolysis enters a combustor for combustion after acid gas generated by mixing with a metal salt solution is removed through a calcium oxide filter;
the high-temperature flue gas after combustion exchanges heat through a molten salt boiler, the heated molten salt is used as a heat source of the paddle type carbonization furnace, and the waste gas after heat exchange is used as a heat source of the drum dryer.
2. The method for preparing magnetic carbon nanotube/porous carbon material from biomass according to claim 1, wherein: the prepared magnetic carbon nanotube/porous carbon material is an internal porous carbon, an external carbon nanotube composite structure, and a metal salt solution is used as an activating agent to promote the generation of a catalyst porous structure, and in the carbothermic reduction process, the generation of hydrocarbon volatile components is promoted, the hydrocarbon volatile components are subjected to vapor deposition on the surface of a metal active site to generate the carbon nanotube, and nano metal particles are embedded and uniformly dispersed in the carbon-based material.
3. The method for preparing magnetic carbon nanotube/porous carbon material from biomass according to claim 1, wherein: the paddle type carbonization furnace is heated by using the molten salt boiler, the molten salt which provides a heat source for the carbonization furnace is heated by using the molten salt boiler, the inlet temperature of the molten salt is about 650 ℃, the outlet temperature of the molten salt is about 550 ℃, the accurate temperature control of the carbonization furnace is realized, the pyrolysis temperature of the raw material in the paddle type carbonization furnace is kept unchanged, and the molten salt is heated and flows back to the liquid storage tank through the molten salt pump to realize repeated heat exchange.
4. The method for preparing magnetic carbon nanotube/porous carbon material from biomass according to claim 1, wherein: waste gas generated after heat exchange of the high-temperature flue gas after combustion in the molten salt boiler is used as a heat source to supply heat to the drum dryer, and the temperature is 200-300 ℃.
5. The device for preparing the magnetic carbon nano tube/porous carbon material by using the biomass is characterized in that: comprises a metal salt solution storage tank (1), a solution pump (2), a double-helix stirring machine (5), a drum dryer (8), a carbonization furnace (13), a calcium oxide filter (18), a burner (22), a fan (23), a molten salt boiler (24), a molten salt storage tank (28) and a molten salt pump (29);
the double-helix stirrer (5) comprises a raw material inlet (3), a nozzle (4) and a material outlet (6); the drum dryer (8) comprises a material inlet (7), a material outlet (11), a gas inlet (9) and a waste gas outlet (10); the paddle type carbonization furnace (13) comprises a material inlet (12), a molten salt inlet (15), a molten salt outlet (14) and a gas outlet (16); the calcium oxide dryer (18) comprises a gas inlet (17), a gas outlet (19), a calcium oxide inlet (20) and a calcium oxide outlet (21); the molten salt boiler (24) comprises a gas outlet (27), a molten salt inlet (25) and a molten salt outlet (26);
the outlet of the metal salt liquid storage tank (1) is connected with a solution pump (2), the solution pump (2) is connected with a nozzle of a double-helix stirring machine (5), a discharge hole (6) of the double-helix stirring machine (5) is connected with a feed hole (7) of a drum-type dryer (8), a discharge hole (11) of the drum-type dryer is connected with a feed hole (12) of a paddle-type carbonization furnace (13), a gas outlet (16) of the carbonization furnace is connected with an inlet (17) of a calcium chloride filter (18), a gas outlet (19) of the filter is connected to a molten salt boiler (24) through a combustor (22), and a waste gas outlet (27) of the molten salt boiler is connected with a gas inlet (9) of the drum-type dryer (8);
the molten salt storage tank (28) is connected with a molten salt inlet (25) of the molten salt boiler (24), an outlet (26) of the molten salt boiler is connected with a molten salt inlet (15) of the paddle type carbonization furnace (13), a molten salt outlet (14) of the carbonization furnace is connected with a molten salt pump (29), and the molten salt pump (29) is connected with the molten salt storage tank (28).
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Cited By (3)
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| CN111628181A (en) * | 2020-05-25 | 2020-09-04 | 常熟氢能源研究院有限公司 | Process for preparing gas diffusion layer for fuel cell by using wood as raw material |
| CN113148983A (en) * | 2021-04-14 | 2021-07-23 | 淮阴工学院 | Method for preparing carbon nano tube/porous carbon material and hydrogen-rich synthetic gas by biomass pyrolysis |
| CN114754579A (en) * | 2022-03-31 | 2022-07-15 | 中南大学 | Method and device for preparing carbon material by pyrolyzing biomass through molten salt heated by solar energy |
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| CN111628181B (en) * | 2020-05-25 | 2021-07-23 | 常熟氢能源研究院有限公司 | Process for preparing gas diffusion layer for fuel cell by using wood as raw material |
| CN113148983A (en) * | 2021-04-14 | 2021-07-23 | 淮阴工学院 | Method for preparing carbon nano tube/porous carbon material and hydrogen-rich synthetic gas by biomass pyrolysis |
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Application publication date: 20200417 |