CN112126471A - Environment-friendly binary carbonate circulating reaction system - Google Patents
Environment-friendly binary carbonate circulating reaction system Download PDFInfo
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- CN112126471A CN112126471A CN202011095973.XA CN202011095973A CN112126471A CN 112126471 A CN112126471 A CN 112126471A CN 202011095973 A CN202011095973 A CN 202011095973A CN 112126471 A CN112126471 A CN 112126471A
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- C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
- C10J3/00—Production of combustible gases containing carbon monoxide from solid carbonaceous fuels
- C10J3/57—Gasification using molten salts or metals
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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- C01B32/30—Active carbon
- C01B32/312—Preparation
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- C10J3/72—Other features
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
- C10J2300/00—Details of gasification processes
- C10J2300/09—Details of the feed, e.g. feeding of spent catalyst, inert gas or halogens
- C10J2300/0913—Carbonaceous raw material
- C10J2300/0916—Biomass
- C10J2300/092—Wood, cellulose
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
- C10J2300/00—Details of gasification processes
- C10J2300/09—Details of the feed, e.g. feeding of spent catalyst, inert gas or halogens
- C10J2300/0953—Gasifying agents
- C10J2300/0973—Water
- C10J2300/0976—Water as steam
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- C10J2300/00—Details of gasification processes
- C10J2300/09—Details of the feed, e.g. feeding of spent catalyst, inert gas or halogens
- C10J2300/0983—Additives
- C10J2300/0986—Catalysts
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- C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
- C10J2300/00—Details of gasification processes
- C10J2300/12—Heating the gasifier
- C10J2300/1246—Heating the gasifier by external or indirect heating
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
- C10J2300/00—Details of gasification processes
- C10J2300/16—Integration of gasification processes with another plant or parts within the plant
- C10J2300/1625—Integration of gasification processes with another plant or parts within the plant with solids treatment
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
- C10J2300/00—Details of gasification processes
- C10J2300/18—Details of the gasification process, e.g. loops, autothermal operation
- C10J2300/1807—Recycle loops, e.g. gas, solids, heating medium, water
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
- C10J2300/00—Details of gasification processes
- C10J2300/18—Details of the gasification process, e.g. loops, autothermal operation
- C10J2300/1861—Heat exchange between at least two process streams
- C10J2300/1884—Heat exchange between at least two process streams with one stream being synthesis gas
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The application discloses binary carbonate circulation reaction system of environmental protection, including reaction system, sprinkler system, delivery pump, filter and membrane separator, reaction system includes reation kettle. The reaction kettle is filled with fused salt, the upper part of the reaction kettle is provided with a biomass feed inlet, a fused salt inlet, a gasifying agent inlet and a pyrolysis gas outlet, the upper part of the side wall of the reaction kettle is provided with an overflow port, and the liquid level of the fused salt in the reaction kettle is slightly higher than the overflow port; the overflow port of the reaction kettle is connected with a spraying system through an overflow pipe, activated carbon generated by reaction in the reaction kettle can overflow into the spraying system along with the molten salt, the spraying system sprays clean water to perform washing treatment, the filtration is performed, wet activated carbon filter residue is dried to obtain an activated carbon product, and the filtrate is desalted by a membrane separator, and the obtained strong salt solution is reused in the reaction kettle. The method realizes the recycling of the water vapor and the molten salt in the reaction system, strengthens the reaction, simplifies the process, and has the advantages of environmental protection, energy conservation and no consumption.
Description
Technical Field
The application belongs to the field of biomass gasification cracking, and particularly relates to an environment-friendly binary carbonate circulating reaction system.
Background
In the process of preparing the activated carbon by gasifying the biomass, the activated carbon is uniformly distributed in the molten salt, and the common mechanical separation method is to scrape out the crude activated carbon product on the surface of the salt cake after the molten salt is cooled into the salt cake, so that the separation of the activated carbon and the main body of the molten salt is realized, and the process is complicated. And the activated carbon acid-washing solution can not be reused, the fused salt can not be directly recycled in the system, and the energy consumption is large. Therefore, an environment-friendly binary carbonate circulating reaction system is urgently needed.
Disclosure of Invention
In view of the above problems, an object of the present application is to provide an environment-friendly binary carbonate cyclic reaction system, which realizes that water vapor generated in the reaction system and separated binary carbonate can be recycled, pneumatic stirring is simultaneously performed, activated carbon can be prepared by activating below the liquid level of molten salt, activated carbon overflows by using the temperature change of the molten salt, and the environment-friendly binary carbonate cyclic reaction system has the advantages of environmental protection and no consumption.
The environment-friendly binary carbonate circulating reaction system is characterized by comprising a reaction system, a spraying system, a delivery pump, a filter and a membrane separator, wherein the reaction system comprises a reaction kettle; the reactor is filled with molten salt, the upper part of the reactor is provided with a biomass feed inlet, a molten salt inlet, a gasifying agent inlet and a pyrolysis gas outlet, the upper part of the side wall of the reactor is provided with an overflow port, and the liquid level of the molten salt in the reactor is slightly higher than the overflow port on the upper part of the side wall of the reactor; an overflow port of the reaction kettle is connected with a spraying system through an overflow pipe, a liquid outlet of the spraying system is connected with a filter through a pipeline through a delivery pump, a filtrate outlet of the filter is connected with a membrane separator through a pipeline, and control valves are arranged on the corresponding pipelines;
the biomass and the gasifying agent are subjected to catalytic reaction in the molten salt in the reaction kettle to generate active carbon and pyrolysis gas, the active carbon can float to the surface of the molten salt and is conveyed to a spraying system through a pipeline along with a small amount of molten salt through an overflow port; the spraying system sprays clean water to wash the entered activated carbon-molten salt mixture, steam generated in the washing process is reused in the reaction kettle for catalytic reaction, mixed liquid of a salt solution and activated carbon is formed at the same time, the mixed liquid is conveyed to the filter by the conveying pump to be filtered, wet activated carbon filter residue is dried to obtain an activated carbon product, filtrate is conveyed to the membrane separator to be desalted to obtain fresh water and a concentrated salt solution, the fresh water can be reused in the spraying system, and the concentrated salt solution can be reused in the reaction kettle for catalytic reaction.
The environment-friendly binary carbonate circulating reaction system is characterized in that the spraying system comprises a spraying chamber, a spraying head and a clear water liquid inlet pipe, wherein the spraying head and the clear water liquid inlet pipe are arranged inside the upper end of the spraying chamber;
the fresh water side outlet of the membrane separator is connected with the side part of the fresh water inlet pipe through a pipeline so as to spray fresh water obtained by desalination treatment of the membrane separator into the spray chamber through the spray header; the concentrated water side outlet of the membrane separator is connected with the side part of the molten salt inlet of the reaction kettle through a pipeline, so that the concentrated salt solution obtained by desalting treatment of the membrane separator can be reused in the reaction kettle for catalytic reaction.
The environment-friendly binary carbonate circulating reaction system is characterized in that a steam outlet is also formed in the top of the spray chamber, and when clean water is sprayed in the spray chamber to cool the molten salt, part of water is vaporized at high temperature when meeting the molten salt to form water vapor; and water vapor discharged from a vapor outlet at the top of the spray chamber is used as a gasifying agent and reused in the reaction kettle through a pipeline.
The environment-friendly binary carbonate circulating reaction system is characterized by further comprising a rotary kiln, wet activated carbon filtered by a filter is sent to the rotary kiln, pyrolysis gas formed in the reaction kettle is discharged from a pyrolysis gas outlet in the upper portion of the reaction kettle, is ignited in a heating sleeve and is converted into flue gas, the flue gas is sent to the rotary kiln to serve as a heat source for heating the rotary kiln, moisture in the wet activated carbon is heated and vaporized to form water vapor, and the water vapor can be used as a gasifying agent to be reused in the reaction kettle.
The environment-friendly binary carbonate circulating reaction system is characterized by further comprising a sleeve assembly, wherein the sleeve assembly comprises a sleeve and a turntable vertically and fixedly mounted on the outer side of the lower end of the sleeve, the sleeve is rotatably arranged at the top of the reaction kettle, and the turntable is arranged in the reaction kettle; the rotary table is provided with a notch, so that when biomass is fed through a biomass feed port in the upper part of the reaction kettle, the biomass can enter molten salt through the notch in the rotary table; when the biomass and the gasifying agent are subjected to catalytic reaction in the molten salt in the reaction kettle, the rotary table is slightly immersed below the surface of the molten salt, and the rotary table is driven to rotate together by the rotation of the sleeve to prevent the biomass in the molten salt from floating up to the surface.
The environment-friendly binary carbonate circulating reaction system is characterized by further comprising a coil assembly, wherein the coil assembly comprises a hollow connecting rod sleeved on the inner side of the sleeve and a mosquito-repellent incense coil arranged at the lower end of the hollow connecting rod, the upper end of the hollow connecting rod penetrates out of the sleeve, and a plurality of air outlet holes are formed in the mosquito-repellent incense coil; wherein the hollow connecting rod is connected with the sleeve in a rotating and sealing way;
when biomass and gasifying agent are subjected to catalytic reaction in molten salt in the reaction kettle, the mosquito-repellent incense coil is immersed in the molten salt, the hollow connecting rod rotates to drive the mosquito-repellent incense coil to rotate together, and meanwhile, the gasifying agent is introduced into the upper end opening of the hollow connecting rod and is discharged through a plurality of air outlet holes in the mosquito-repellent incense coil and is uniformly distributed in the molten salt to be in contact reaction with the biomass.
The environment-friendly binary carbonate circulating reaction system is characterized in that a heating jacket is arranged outside the reaction kettle in a matching manner, the heating jacket is an electric heating jacket or an interlayer sleeve, the electric heating jacket heats the reaction kettle by electrifying, the interlayer sleeve heats the reaction kettle by introducing high-temperature flue gas, and the interlayer sleeve is provided with a flue gas inlet and a flue gas outlet; wherein, the heating jacket comprises a side wall heating jacket arranged on the outer side of the side part of the reaction kettle and a bottom heating jacket arranged on the outer side of the bottom part of the reaction kettle.
The environment-friendly binary carbonate circulating reaction system is characterized in that the catalytic reaction of biomass and a gasifying agent is carried out in molten salt in a reaction kettle, and the method comprises the following steps:
1) starting a side wall heating jacket on the outer side of the side part of the reaction kettle and a bottom heating jacket on the outer side of the bottom of the reaction kettle for heating, heating the reaction kettle to 700-1000 ℃, adding biomass into molten salt in the reaction kettle through a gap on a rotary table, slightly immersing the rotary table of a sleeve assembly below the surface of the molten salt, rotating the sleeve assembly to fully contact the biomass with the molten salt, immersing a mosquito-repellent incense coil of the coil assembly in the molten salt, introducing a gasifying agent, discharging the gasifying agent through a plurality of air outlet holes in the mosquito-repellent incense coil, and pneumatically stirring to fully contact and react the gasifying agent with the biomass in the molten salt;
2) after biomass is gasified and cracked, the sleeve pipe assembly and the coil pipe assembly are lifted to be above the liquid level of the molten salt, the bottom heating jacket on the outer side of the bottom of the reaction kettle is closed, the molten salt is slowly cooled to 400-plus-500 ℃, the density of the molten salt on the bottom is changed, the active carbon generated by the reaction slowly floats to the surface of the molten salt, and the active carbon is conveyed into a spraying system through an overflow port and a pipeline along with a small amount of molten salt;
3) the spraying system sprays clean water to wash the entering activated carbon-molten salt mixture, part of the clean water is gasified at high temperature when meeting molten salt, is preheated and then circulates to the reaction kettle to be used as a gasifying agent for reutilization, the sprayed mixture is filtered by a filter to obtain wet activated carbon, and then is subjected to heat exchange with pyrolysis gas in the rotary kiln to obtain dry activated carbon, and steam generated in the heat exchange process is preheated and then circulates to the reaction kettle to be used as the gasifying agent for reutilization; and (3) after spraying, enabling the mixture to pass through a filter to obtain a saline solution, and then performing desalination treatment through a membrane separator to obtain fresh water and a strong brine solution, wherein the fresh water can be reused in a spraying system, and the strong brine solution can be reused in a reaction kettle to perform catalytic reaction.
The environment-friendly binary carbonate circulating reaction system is characterized in that the molten salt is a binary eutectic of sodium carbonate and potassium carbonate, and the mass ratio of the sodium carbonate to the potassium carbonate is 60:40-40:60, preferably 55.5: 44.5; the reaction temperature is 700-1000 ℃, and the gasifying agent is steam; the biomass is coconut shells, walnut shells, chestnut shells, bamboo powder or cellulose monomers, and the cellulose monomers are glucose or cellobiose.
The environment-friendly binary carbonate circulating reaction system is characterized in that the reaction system can be applied to hydrogen production by molten salt catalytic decoking, biomass gasification, activated carbon production by biomass gasification or super capacitors production by biomass gasification.
Compared with the prior art, the beneficial effect that this application was got is:
1) the application provides a binary carbonate circulation reaction system of environmental protection, has simplified mechanical separation technology, low cost, reaction is rapid, safety ring protects, has realized that the steam that produces in the reaction system and the binary carbonate who separates can recycle, and gasification agent motion produces stirring effect simultaneously, and can make active carbon in the activation below the fused salt liquid level, utilizes the fused salt alternating temperature to overflow the active carbon, has the advantage that the environmental protection is not consumed.
2) In the application, when the spraying system cools the molten salt, part of water is gasified at high temperature when meeting the molten salt and is circulated to the reaction system after being preheated; the wet activated carbon obtained by filtering is subjected to heat exchange with pyrolysis gas in a heat exchanger to obtain a finished product of dry activated carbon, and water vapor obtained in the heat exchange process is preheated and then circulated back to a reaction system, so that heat is recycled, and the energy consumption problem of the whole process is better solved.
3) In the application, a mixture of sodium carbonate and potassium carbonate (namely binary molten carbonate) with a mass ratio of 60:40-40:60 is used as a heat medium and a catalyst, and the mass ratio is preferably 55.5: 44.5 (the melting point is 710.3 ℃) is suitable for the reaction temperature of 700-1000 ℃, and has the advantages of extremely low corrosion to equipment, stable chemical property, small viscosity, large specific heat capacity, good catalytic activation effect and recyclability.
The utility model provides a binary carbonate circulation reaction system utilizes the fused salt as heat transfer medium and catalyst, and the steam that produces in the flow and the binary carbonate who separates can recycle, have the advantage that the environmental protection does not have the consumption, and can couple gasification agent one-step method biomass activated carbon, reduce tar and produce, utilize the fused salt alternating temperature to separate the product activated carbon simultaneously for this system provides technical support for the industrial production of activated carbon and hydrogen manufacturing decoking process.
Drawings
FIG. 1 is a schematic process flow diagram of a binary carbonate recycle reaction system of the present application;
FIG. 2 is a schematic diagram of the structure of an electrically heated binary carbonate recycle reaction system of the present application;
FIG. 3 is a schematic diagram of the configuration of a flue gas heated binary carbonate recycle reaction system of the present application;
FIG. 4 is a schematic diagram of a gas distributor;
in the figure: 1-reaction system, 1-1 side wall heating jacket, 1-2 bottom heating jacket, 1-3 ceramic lining, 1-4 reaction kettle, 1-5 hollow connecting rod, 1-6 sleeve, 1-7 turntable, 1-8 mosquito coil, 1-9 overflow pipe, 2-spraying system, 2-1 spray head, 2-2 spray chamber, 3-delivery pump, 4-filter, 5-membrane separator, 6-rotary kiln, 7-heating sleeve and 8-heat exchanger.
Detailed Description
The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the invention.
Example (b): compare FIGS. 1-4
An environment-friendly binary carbonate circulating reaction system comprises a reaction system, a spraying system, a delivery pump 3, a filter 4 and a membrane separator 5, wherein the reaction system comprises reaction kettles 1-4. The reaction kettle 1-4 is filled with molten salt, the upper part of the reaction kettle 1-4 is provided with a biomass feed inlet, a molten salt inlet, a gasifying agent inlet and a pyrolysis gas outlet, the upper part of the side wall of the reaction kettle 1-4 is provided with an overflow port, and the liquid level of the molten salt in the reaction kettle 1-4 is slightly higher than the overflow port on the upper part of the side wall; the overflow ports of the reaction kettles 1-4 are connected with a spraying system through overflow pipes 1-9, the liquid outlet of the spraying system is connected with a filter 4 through a pipeline through a delivery pump 3, the filtrate outlet of the filter 4 is connected with a membrane separator 5 through a pipeline, and control valves are arranged on the corresponding pipelines.
Referring to fig. 2 and 3, the spraying system comprises a spraying chamber 2-2, a spraying head 2-1 and a clear water inlet pipe, wherein the spraying head 2-1 and the clear water inlet pipe are arranged inside the upper end of the spraying chamber 2-2, the clear water inlet pipe penetrates into the spraying chamber 2-2 and is connected with the spraying head 2-1, so that clear water is sprayed into the spraying chamber 2-2 to cool molten salt, and a mixed solution of a salt solution and active carbon is formed in the spraying chamber 2-2; the fresh water outlet of the membrane separator 5 is connected with the side part of the fresh water inlet pipe by a pipeline, so that the fresh water obtained by the desalination treatment of the membrane separator 5 is sprayed into the spray chamber 2-2 through the spray header 2-1; the concentrated water side outlet of the membrane separator 5 is connected with the side part of the molten salt inlet of the reaction kettle 1-4 by a pipeline, so that the concentrated salt solution obtained by desalting treatment of the membrane separator 5 can be reused in the reaction kettle 1-4 for catalytic reaction; wherein, the concentrated salt solution obtained by the concentration of the membrane separator 5 mainly comprises a binary carbonate component and water, the binary carbonate component is introduced into the reaction kettle 1-4 to be used as molten salt again, and the water is introduced into the reaction kettle 1-4 to be used as a gasifying agent.
Further, the top of the spray chamber 2-2 is also provided with a steam outlet, and when clean water is sprayed in the spray chamber 2-2 to cool the molten salt, part of water is vaporized at high temperature when meeting the molten salt to form steam; and water vapor discharged from a vapor outlet at the top of the spray chamber 2-2 is used as a gasifying agent and reused in the reaction system through a pipeline.
Further, the device of the application also comprises a rotary kiln 6, wet activated carbon filtered by the filter 4 is sent to the rotary kiln 6, pyrolysis gas formed by reaction in the reaction kettle 1-4 is discharged from a pyrolysis gas outlet at the upper part of the reaction kettle 1-4, is ignited by a heating sleeve 7 and is converted into flue gas, and then is sent to the rotary kiln 6 to be used as a heat source for heating the rotary kiln 6, moisture in the wet activated carbon is heated and vaporized to form water vapor, and the water vapor can be used as a gasifying agent to be reused in the reaction kettle 1-4.
Referring to fig. 2-4, the reaction system of the present application further comprises a sleeve assembly, the sleeve assembly is composed of sleeves 1-6 and turntables 1-7 vertically and fixedly installed at the outer sides of the lower ends of the sleeves 1-6, the sleeves 1-6 are rotatably installed at the tops of the reaction kettles 1-4, and the turntables 1-7 are installed in the reaction kettles 1-4; the rotary discs 1-7 are provided with notches, so that when biomass is fed through a biomass feed port at the upper parts of the reaction kettles 1-4, the biomass can enter molten salt through the notches on the rotary discs 1-7; when biomass and gasifying agent are subjected to catalytic reaction in molten salt in a reaction kettle 1-4, the rotary table 1-7 is slightly immersed below the surface of the molten salt, the sleeve 1-6 rotates to drive the rotary table 1-7 to rotate together, and the rotary table 1-7 can play a certain blocking role to prevent the biomass in the molten salt from floating up to the surface. The rotation mode of the sleeves 1-6 belongs to the prior conventional technology, for example: a belt pulley is fixedly arranged on the side portion of the sleeve 1-6, the motor is connected with the belt pulley on the side portion of the sleeve 1-6 through the belt, and the sleeve 1-6 is rotated under the transmission action of the belt.
Further, the reaction system of the application also comprises a coil assembly, wherein the coil assembly comprises hollow connecting rods 1-5 which are sleeved on the inner sides of the sleeves 1-6 and mosquito-repellent incense type coils 1-8 which are arranged at the lower ends of the hollow connecting rods 1-5, the upper ends of the hollow connecting rods 1-5 penetrate out of the sleeves 1-6, a plurality of air outlets are formed in the mosquito-repellent incense type coils 1-8, air inlet pipes for introducing gasifying agents can be arranged at the upper ports of the hollow connecting rods 1-5, and the upper ports of the hollow connecting rods 1-5 and the air inlet pipes are connected in a sealing and rotating mode. Wherein, the hollow connecting rod 1-5 and the sleeve 1-6 are connected in a rotating and sealing way.
When biomass and gasifying agent are subjected to catalytic reaction in molten salt in a reaction kettle 1-4, the mosquito-repellent incense coil 1-8 is immersed in the molten salt, the gasifying agent is introduced into the upper end opening of the hollow connecting rod 1-5 and is discharged through a plurality of air outlet holes in the mosquito-repellent incense coil 1-8, pneumatic stirring is also performed, and the gasifying agent is uniformly distributed in the molten salt to be subjected to contact reaction with the biomass. Wherein, the rotation mode of the hollow connecting rod 1-5 belongs to the prior conventional technology, for example: a belt pulley is fixedly arranged on the side portion of the hollow connecting rod 1-5, the motor is connected with the belt pulley on the side portion of the hollow connecting rod 1-5 through the belt, and the hollow connecting rod 1-5 is rotated under the transmission action of the belt.
The outer sides of the reaction kettles 1-4 are provided with heating jackets in a matching manner, the heating jackets are electric heating jackets or interlayer sleeves, the electric heating jackets heat the reaction kettles 1-4 by electrifying, and a comparison figure 2 is a structural schematic diagram of an electric heating type. The interlayer sleeve heats the reaction kettles 1-4 by introducing high-temperature flue gas, a flue gas inlet and a flue gas outlet are arranged on the interlayer sleeve, and a structural schematic diagram of flue gas heating is shown in a comparison figure 3.
Referring to fig. 2-3, the outer side of the reaction kettle 1-4 is provided with a ceramic lining 1-3, and the ceramic lining 1-3 is provided with a heating jacket.
Further, the heating jackets comprise a side wall heating jacket 1-1 arranged at the outer side of the side part of the reaction kettle 1-4 and a bottom heating jacket 1-2 arranged at the outer side of the bottom part of the reaction kettle 1-4. The molten salt in the reaction kettle is heated to a molten state and is controlled by a side wall heating jacket and a bottom heating jacket, namely, when the reaction kettle is heated and heated, the side wall heating jacket 1-1 and the bottom heating jacket 1-2 are simultaneously opened; when the reaction kettle is cooled after the reaction is finished, the bottom heating jacket 1-2 is closed, the side wall heating jacket 1-1 is kept in an open state, the molten salt at the bottom layer of the reaction kettle is slowly cooled, the density of the molten salt at the bottom layer is slowly changed (the density of the molten salt at the bottom layer is slowly increased due to the slow cooling of the molten salt at the bottom layer, and the density of the molten salt at the upper layer is smaller than that of the molten salt at the bottom layer due to the higher temperature of the molten salt at the upper layer), and the activated carbon generated by the reaction in the molten salt can slowly float to the surface of.
Referring to fig. 2-3, the device of the present application further includes a heat exchanger 8, the steam generated by washing in the spray chamber 2-2 and the steam generated by drying wet activated carbon in the rotary kiln 6 can be introduced into a cold channel of the heat exchanger 8 together, the flue gas generated by reaction in the reaction kettle 1-4 can be introduced into a hot channel of the heat exchanger 8, and the steam and the flue gas exchange heat through the heat exchanger 8. For example: pyrolysis gas formed by reaction in the reaction kettles 1-4 is discharged from a pyrolysis gas outlet at the upper parts of the reaction kettles 1-4, is converted into flue gas by ignition in the heating sleeve 7, and then is discharged in two ways, wherein one way is used as a heat source for heating the rotary kiln 6, and the other way is introduced into a heat channel of the heat exchanger 8 and is used as a heat source for heating the heat exchanger 8.
The device of this application carries out the during operation:
the biomass and a gasifying agent are subjected to catalytic reaction in molten salt in a reaction kettle 1-4 to generate active carbon and pyrolysis gas, the active carbon can float to the surface of the molten salt and is conveyed into a spraying system through a pipeline along with a small amount of molten salt through an overflow port (when overflow is carried out, a control valve on an overflow pipe 1-9 needs to be opened); the spraying system sprays clean water to wash the entering activated carbon-molten salt mixture, part of water is gasified at high temperature when meeting molten salt to form water vapor, and the water vapor can be introduced into the reaction kettle again to be used as a gasifying agent. And (3) conveying the mixed solution of the saline solution and the activated carbon formed after spraying to a filter 4 by a conveying pump 3 for filtering, drying filter residues (namely wet activated carbon) to obtain an activated carbon product, conveying the filtrate (namely the saline solution) to a membrane separator 5 for desalination to obtain fresh water and concentrated salt solution, wherein the fresh water can be reused in a spraying system, and the concentrated salt solution can be reused in the reaction kettles 1-4 for catalytic reaction. According to the working process, no waste liquid is generated during operation of the reaction system, and all substances can be recycled.
The reaction system of the present application, which performs a catalytic reaction of biomass and a gasifying agent in molten salt in a reaction vessel, includes the following steps (see fig. 1):
1) starting a side wall heating jacket on the outer side of the side part of the reaction kettle and a bottom heating jacket on the outer side of the bottom of the reaction kettle for heating, heating the reaction kettle to 700-1000 ℃, adding biomass into molten salt in the reaction kettle through a gap on a rotary table, slightly immersing the rotary table of a sleeve assembly below the surface of the molten salt, rotating the sleeve assembly to fully contact the biomass with the molten salt, immersing a mosquito-repellent incense coil of the coil assembly in the molten salt, introducing a gasifying agent, discharging the gasifying agent through a plurality of air outlet holes in the mosquito-repellent incense coil, and pneumatically stirring to fully contact and react the gasifying agent with the biomass in the molten salt;
2) after biomass is gasified and cracked, the sleeve pipe assembly and the coil pipe assembly are lifted to be above the liquid level of the molten salt, the bottom heating jacket on the outer side of the bottom of the reaction kettle is closed, the molten salt is slowly cooled to 400-plus-500 ℃, the density of the molten salt on the bottom is changed, the active carbon generated by the reaction slowly floats to the surface of the molten salt, and the active carbon is conveyed into a spraying system through an overflow port and a pipeline along with a small amount of molten salt;
3) the spraying system sprays clean water to cool the entering activated carbon-molten salt mixture, part of the clean water is gasified at high temperature when meeting molten salt, is preheated and then circulates to the reaction kettle to be used as a gasifying agent for reutilization, the sprayed mixture is filtered by a filter to obtain wet activated carbon, and then is subjected to heat exchange with pyrolysis gas in a heat exchanger to obtain dry activated carbon, and steam generated in the heat exchange process is preheated and then circulates to the reaction kettle to be used as the gasifying agent for reutilization; and (3) after spraying, enabling the mixture to pass through a filter to obtain a saline solution, and then performing desalination treatment through a membrane separator to obtain fresh water and a strong brine solution, wherein the fresh water can be reused in a spraying system, and the strong brine solution can be reused in a reaction kettle to perform catalytic reaction.
The molten salt is a binary eutectic of sodium carbonate and potassium carbonate, and the mass ratio of the sodium carbonate to the potassium carbonate is 55.5: 44.5; the reaction temperature is 700-1000 ℃, and the gasifying agent is steam; the biomass is coconut shells, walnut shells, chestnut shells, bamboo powder or cellulose monomers, and the cellulose monomers are glucose or cellobiose.
After the reaction is finished, air or oxygen can be introduced into the molten salt in the reaction kettle so as to remove tar carbon generated in the molten salt in the reaction kettle
The reaction system can be used for producing hydrogen by molten salt decoking, producing hydrogen by biomass gasification, producing activated carbon by biomass gasification or producing a supercapacitor by biomass gasification.
When the reaction system is used for molten salt decoking hydrogen production and biomass gasification hydrogen production, CO is introduced through the coil assembly2And removing carbon in the molten salt in the reaction kettle.
When the reaction system is used for preparing activated carbon by biomass gasification and preparing a supercapacitor by biomass gasification, air or oxygen needs to be introduced into the molten salt in the reaction kettle after the reaction is finished so as to remove tar carbon generated in the molten salt in the reaction kettle.
Example 1:
200g of a mixture of sodium carbonate and potassium carbonate (i.e. molten salt) in a mass ratio of 55.5: 44.5 as a heat medium and a catalyst (melting point 710.3 ℃) were added to the reaction vessel through the turntable notch, and the side wall heating jacket and the bottom heating jacket were started and the reaction vessel was warmed to 750 ℃. Keeping an oxygen-free atmosphere, extending a coil pipe into the fused salt, introducing water vapor with the flow rate of 10 g/h, adding 10g of crushed and dried cedar wood chip raw material into a reaction kettle, carbonizing/activating the cedar wood chips in the reaction kettle at 750 ℃ for 15min, and continuously discharging pyrolysis gas generated by the reaction from a pyrolysis gas outlet at the upper part of the reaction kettle. The gasification rate of the cedar chips is between 78.6 and 81.3 percent (mass percent), and the synthesis gas (H) in the pyrolysis gas generated by the reaction2And CO) in a volume percentage of 79.2% to 84.7%, H in the synthesis gas2And CO in a volume ratio of 3.9-4.2: 1.
After the reaction is finished, the bottom heating jacket is closed, the temperature of the molten salt is reduced to about 450 ℃, the density of the molten salt at the bottom layer is changed, and the active carbon slowly floats upwards and enters a spraying system through an overflow port. And spraying clear water to cool the molten salt, filtering the sprayed mixture through a filter to obtain wet activated carbon, and exchanging heat between the wet activated carbon and pyrolysis gas in a heat exchanger to obtain dry activated carbon. The specific surface area of the finished activated carbon prepared in this example, as characterized by BET, is 855.945 m2The pore volume is 0.4416 mL/g, and the average pore diameter is 1.1065 nm.
Example 2:
200g of a mixture of sodium carbonate and potassium carbonate (i.e. molten salt) in a mass ratio of 55.5: 44.5 were used as the heat medium and catalyst (melting point 710.3 ℃ C.) and were added to the reactor through the turntable notch to start the side and bottom heating jackets and to raise the temperature to 750 ℃. And (2) keeping an oxygen-free atmosphere, introducing water vapor with the flow rate of 10 g/h when the coil pipe extends below the liquid level of the molten salt, adding 10g of warp knitting waste leather which is cut into uniform small blocks into the reaction kettle, and continuously carrying out decoking reaction for 20 hours, wherein the decoking efficiency is kept stable, and a detection result shows that the tar yield is reduced by more than 95%, and the gas yield is increased by more than 15%.
The statements in this specification merely set forth a list of implementations of the inventive concept and the scope of the present invention should not be construed as limited to the particular forms set forth in the examples.
Claims (10)
1. An environment-friendly binary carbonate circulating reaction system is characterized by comprising a reaction system, a spraying system, a delivery pump (3), a filter (4) and a membrane separator (5), wherein the reaction system comprises a reaction kettle (1-4); the reaction kettle (1-4) is filled with molten salt, the upper part of the reaction kettle (1-4) is provided with a biomass feed inlet, a molten salt inlet, a gasifying agent inlet and a pyrolysis gas outlet, the upper part of the side wall of the reaction kettle (1-4) is provided with an overflow port, and the liquid level of the molten salt in the reaction kettle (1-4) is slightly higher than the overflow port on the upper part of the side wall; overflow ports of the reaction kettles (1-4) are connected with a spraying system (2) through overflow pipes (1-9), a liquid outlet of the spraying system is connected with a filter (4) through a pipeline through a delivery pump (3), a filtrate outlet of the filter (4) is connected with a membrane separator (5) through a pipeline, and control valves are arranged on corresponding pipelines;
the biomass and the gasifying agent are subjected to catalytic reaction in the molten salt in the reaction kettle (1-4) to generate active carbon and pyrolysis gas, the active carbon can float to the surface of the molten salt and is conveyed to a spraying system through a pipeline along with a small amount of molten salt through the overflow port; the spraying system sprays clean water to wash an entered activated carbon-molten salt mixture, steam generated in the washing process is reused for the catalytic reaction of the reaction kettle (1-4), mixed liquid of a salt water solution and activated carbon is formed at the same time, the mixed liquid is conveyed to the filter (4) by the conveying pump (3) to be filtered, wet activated carbon filter residue is dried to obtain an activated carbon product, filtrate is conveyed to the membrane separator (5) to be desalted to obtain fresh water and a concentrated salt solution, the fresh water can be reused for the spraying system, and the concentrated salt solution can be reused for the catalytic reaction of the reaction kettle (1-4).
2. The environment-friendly binary carbonate circulating reaction system according to claim 1, wherein the spraying system comprises a spraying chamber (2-2), a spraying head (2-1) and a clean water inlet pipe, the spraying head (2-1) and the clean water inlet pipe are arranged inside the upper end of the spraying chamber (2-2), the clean water inlet pipe penetrates into the spraying chamber (2-2) and is connected with the spraying head (2-1) so that clean water is sprayed into the spraying chamber (2-2) to wash the molten salt, and a mixed solution of a saline solution and activated carbon is formed in the spraying chamber (2-2);
the fresh water side outlet of the membrane separator (5) is connected with the side part of the fresh water inlet pipe through a pipeline, so that the fresh water obtained by the desalination treatment of the membrane separator (5) is sprayed into the spray chamber (2-2) through the spray header (2-1); the concentrated water side outlet of the membrane separator (5) is connected with the side part of the fused salt inlet of the reaction kettle (1-4) by a pipeline, so that the concentrated salt solution obtained by desalination treatment of the membrane separator (5) can be reused in the reaction kettle (1-4) for catalytic reaction.
3. The environment-friendly binary carbonate circulating reaction system as claimed in claim 2, wherein the top of the spray chamber (2-2) is further provided with a steam outlet, when clean water is sprayed in the spray chamber (2-2) to cool the molten salt, part of water is vaporized at high temperature in the molten salt to form steam; the water vapor discharged from the vapor outlet at the top of the spray chamber (2-2) is used as a gasifying agent and reused in the reaction kettle (1-4) through a pipeline.
4. The environment-friendly binary carbonate circulating reaction system as claimed in claim 1, further comprising a rotary kiln (6), wherein the wet activated carbon filtered by the filter (4) is sent to the rotary kiln (6), the pyrolysis gas formed by the reaction in the reaction kettle (1-4) is discharged from a pyrolysis gas outlet at the upper part of the reaction kettle (1-4), is ignited in a heating sleeve and is converted into flue gas, and then is sent to the rotary kiln (6) to be used as a heat source for heating the rotary kiln (6), moisture in the wet activated carbon is heated and vaporized to form steam, and the steam can be reused as a gasifying agent in the reaction kettle (1-4).
5. The environment-friendly binary carbonate cycle reaction system according to claim 1, wherein the reaction system further comprises a sleeve assembly, the sleeve assembly comprises a sleeve (1-6) and a rotating disc (1-7) vertically and fixedly installed at the outer side of the lower end of the sleeve (1-6), the sleeve (1-6) is rotatably installed at the top of the reaction vessel (1-4), and the rotating disc (1-7) is installed in the reaction vessel (1-4); the rotary discs (1-7) are provided with notches, so that when biomass is fed through a biomass feed port at the upper parts of the reaction kettles (1-4), the biomass can enter molten salt through the notches on the rotary discs (1-7); when biomass and gasifying agent are subjected to catalytic reaction in molten salt in the reaction kettle (1-4), the rotary table (1-7) is slightly immersed below the surface of the molten salt, and the sleeve (1-6) rotates to drive the rotary table (1-7) to rotate together, so that the biomass in the molten salt is prevented from floating up to the surface.
6. The environment-friendly binary carbonate circulating reaction system according to claim 5, wherein the reaction system further comprises a coil assembly, the coil assembly comprises a hollow connecting rod (1-5) sleeved inside the casing (1-6) and a mosquito coil (1-8) arranged at the lower end of the hollow connecting rod (1-5), the upper end of the hollow connecting rod (1-5) penetrates out of the casing (1-6), and the mosquito coil (1-8) is provided with a plurality of air outlets; wherein the hollow connecting rod (1-5) is connected with the sleeve (1-6) in a rotating and sealing way;
when biomass and a gasifying agent are subjected to catalytic reaction in molten salt in a reaction kettle (1-4), the mosquito-repellent incense type coil (1-8) is immersed in the molten salt, the hollow connecting rod (1-5) rotates to drive the mosquito-repellent incense type coil (1-8) to rotate together, meanwhile, the gasifying agent is introduced into the upper end opening of the hollow connecting rod (1-5), is discharged through a plurality of air outlet holes in the mosquito-repellent incense type coil (1-8), and is uniformly distributed in the molten salt to be in contact reaction with the biomass.
7. The environment-friendly binary carbonate circulating reaction system according to claim 1, wherein a heating jacket is cooperatively arranged outside the reaction kettle (1-4), the heating jacket is an electric heating jacket or a sandwich sleeve, the electric heating jacket heats the reaction kettle (1-4) by electrifying, the sandwich sleeve heats the reaction kettle (1-4) by introducing high-temperature flue gas, and the sandwich sleeve is provided with a flue gas inlet and a flue gas outlet; wherein the heating jacket comprises a side wall heating jacket (1-1) arranged on the outer side of the side part of the reaction kettle (1-4) and a bottom heating jacket (1-2) arranged on the outer side of the bottom of the reaction kettle (1-4).
8. An environment-friendly binary carbonate circulating reaction system is characterized in that the catalytic reaction of biomass and a gasifying agent is carried out in molten salt in a reaction kettle, and the method comprises the following steps:
1) starting a side wall heating jacket on the outer side of the side part of the reaction kettle and a bottom heating jacket on the outer side of the bottom of the reaction kettle for heating, heating the reaction kettle to 700-1000 ℃, adding biomass into molten salt in the reaction kettle through a gap on a rotary table, slightly immersing the rotary table of a sleeve assembly below the surface of the molten salt, rotating the sleeve assembly to fully contact the biomass with the molten salt, immersing a mosquito-repellent incense coil of the coil assembly in the molten salt, introducing a gasifying agent, discharging the gasifying agent through a plurality of air outlet holes in the mosquito-repellent incense coil, and pneumatically stirring to fully contact and react the gasifying agent with the biomass in the molten salt;
2) after biomass is gasified and cracked, the sleeve pipe assembly and the coil pipe assembly are lifted to be above the liquid level of the molten salt, the bottom heating jacket on the outer side of the bottom of the reaction kettle is closed, the molten salt is slowly cooled to 400-plus-500 ℃, the density of the molten salt on the bottom is changed, the active carbon generated by the reaction slowly floats to the surface of the molten salt, and the active carbon is conveyed into a spraying system through an overflow port and a pipeline along with a small amount of molten salt;
3) the spraying system sprays clean water to wash the entering activated carbon-molten salt mixture, part of the clean water is gasified at high temperature when meeting molten salt, is preheated and then circulates to the reaction kettle to be used as a gasifying agent for reutilization, the sprayed mixture is filtered by a filter to obtain wet activated carbon, and then is subjected to heat exchange with pyrolysis gas in the rotary kiln to obtain dry activated carbon, and steam generated in the heat exchange process is preheated and then circulates to the reaction kettle to be used as the gasifying agent for reutilization; and (3) after spraying, enabling the mixture to pass through a filter to obtain a saline solution, and then performing desalination treatment through a membrane separator to obtain fresh water and a strong brine solution, wherein the fresh water can be reused in a spraying system, and the strong brine solution can be reused in a reaction kettle to perform catalytic reaction.
9. The environment-friendly binary carbonate circulating reaction system as claimed in claim 8, wherein the molten salt is a binary eutectic of sodium carbonate and potassium carbonate, and the mass ratio of the sodium carbonate to the potassium carbonate is 60:40-40:60, preferably 55.5: 44.5; the reaction temperature is 700-1000 ℃, and the gasifying agent is steam; the biomass is coconut shells, walnut shells, chestnut shells, bamboo powder or cellulose monomers, and the cellulose monomers are glucose or cellobiose.
10. The environment-friendly binary carbonate cyclic reaction system as claimed in claim 1, wherein the reaction system can be applied to hydrogen production by molten salt catalytic decoking, hydrogen production by biomass gasification, activated carbon production by biomass gasification or super capacitor production by biomass gasification.
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| CN114774142A (en) * | 2022-05-16 | 2022-07-22 | 华中科技大学 | Processing system of living beings pyrolysis gas |
| CN114853611A (en) * | 2022-05-16 | 2022-08-05 | 华中科技大学 | Method for treating biomass pyrolysis gas |
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| CN114774142A (en) * | 2022-05-16 | 2022-07-22 | 华中科技大学 | Processing system of living beings pyrolysis gas |
| CN114853611A (en) * | 2022-05-16 | 2022-08-05 | 华中科技大学 | Method for treating biomass pyrolysis gas |
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