CN110066671B - Catalyst regenerated biomass microwave catalytic pyrolysis method and integrated device thereof - Google Patents
Catalyst regenerated biomass microwave catalytic pyrolysis method and integrated device thereof Download PDFInfo
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- CN110066671B CN110066671B CN201910392371.1A CN201910392371A CN110066671B CN 110066671 B CN110066671 B CN 110066671B CN 201910392371 A CN201910392371 A CN 201910392371A CN 110066671 B CN110066671 B CN 110066671B
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- 239000003054 catalyst Substances 0.000 title claims abstract description 171
- 239000002028 Biomass Substances 0.000 title claims abstract description 65
- 238000007233 catalytic pyrolysis Methods 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000000197 pyrolysis Methods 0.000 claims abstract description 115
- 238000001833 catalytic reforming Methods 0.000 claims abstract description 99
- 230000008929 regeneration Effects 0.000 claims abstract description 75
- 238000011069 regeneration method Methods 0.000 claims abstract description 75
- 238000010438 heat treatment Methods 0.000 claims abstract description 31
- 230000001172 regenerating effect Effects 0.000 claims abstract description 17
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 9
- 239000007789 gas Substances 0.000 claims description 84
- 239000010453 quartz Substances 0.000 claims description 78
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 78
- 239000011261 inert gas Substances 0.000 claims description 14
- 238000007599 discharging Methods 0.000 claims description 12
- 239000012159 carrier gas Substances 0.000 claims description 11
- 238000012544 monitoring process Methods 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 229920000742 Cotton Polymers 0.000 claims description 3
- 230000004888 barrier function Effects 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 230000008021 deposition Effects 0.000 claims 1
- 239000003779 heat-resistant material Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 19
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 6
- 239000007787 solid Substances 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 230000009849 deactivation Effects 0.000 description 4
- 239000011229 interlayer Substances 0.000 description 4
- 230000001965 increasing effect Effects 0.000 description 3
- 239000012494 Quartz wool Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000012075 bio-oil Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005485 electric heating Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 229910000288 alkali metal carbonate Inorganic materials 0.000 description 1
- 150000008041 alkali metal carbonates Chemical class 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B47/00—Destructive distillation of solid carbonaceous materials with indirect heating, e.g. by external combustion
- C10B47/02—Destructive distillation of solid carbonaceous materials with indirect heating, e.g. by external combustion with stationary charge
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B57/00—Other carbonising or coking processes; Features of destructive distillation processes in general
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
- C10G1/002—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal in combination with oil conversion- or refining processes
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1011—Biomass
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/40—Characteristics of the process deviating from typical ways of processing
- C10G2300/4006—Temperature
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/70—Catalyst aspects
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Abstract
The invention discloses a biomass microwave catalytic pyrolysis method for regenerating a catalyst and an integrated device thereof. The method comprises the following steps: the biomass enters a pyrolysis zone to carry out pyrolysis reaction, the generated solid residues become biochar, pyrolysis gas is subjected to tar removal through a biochar layer, and enters a catalytic zone with a catalyst for further pyrolysis catalysis. The pyrolysis zone, the tar removal zone, the catalytic reforming zone and the catalyst regeneration zone are mainly heated by a microwave heating device, and the heat radiated outwards by the catalyst regeneration zone is used as auxiliary heat supply. The pyrolysis zone, the tar removal zone and the catalytic reforming zone receive radiant heat, so that the pyrolysis zone, the tar removal zone and the catalytic reforming zone can reach set temperatures quickly and stably. The integrated device links the two processes of catalytic pyrolysis and catalyst regeneration which are commonly separated in the same device, realizes the graded utilization of heat, has high energy utilization efficiency, saves energy and protects environment, can be widely applied to the field of biomass pyrolysis, and has wider application prospect.
Description
Technical Field
The invention relates to the field of biomass catalytic pyrolysis, in particular to a biomass microwave catalytic pyrolysis method for regenerating a catalyst and an integrated device thereof.
Background
With the increasing level of living of people, the consumption of energy and the generation of waste are increasing. On the one hand, fossil energy is exhausted daily, and on the other hand, waste is deposited and hilled due to incomplete utilization of energy. These two problems make efficient and rational use of energy source urgent. Compared with non-renewable resources such as fossil energy, renewable biomass resources have wide prospects. Biomass resources are abundant today, but the technology of conversion utilization is still immature, so that the search for better means of biomass conversion utilization is the direction that many researchers are striving to.
There are many studies on pyrolysis of biomass at home and abroad, and a certain theoretical basis is formed. In the field of bio-oil refining, the methods which are relatively common at present are a catalytic pyrolysis method and a catalytic hydrodeoxygenation method. The catalytic pyrolysis method mainly comprises the steps of carrying out pyrolysis experiments under the environment pressure, and then carrying out catalytic reforming on the generated pyrolysis gas in a catalyst to crack light oil components similar to gasoline. Compared with the catalytic hydrodeoxygenation method, the method omits the pressurizing process, and simplifies, facilitates and economizes the experimental operation flow.
During biomass catalytic pyrolysis, tar is a substance which can be inevitably generated, and the characteristic of high volatile content of biomass determines that more tar is generated in the biomass pyrolysis process than coal, and the characteristic severely restricts the development of biomass pyrolysis technology. Tar removal is a critical issue in the development of biomass pyrolysis.
The solid product obtained after biomass pyrolysis is the biochar, and the biochar has the potential of becoming a cheap catalyst for removing tar because the biochar has a loose and porous structure and contains more alkali metal carbonate in ash, and has the basic conditions of catalytic conversion and catalytic pyrolysis of tar. The use of biochar for tar removal can reduce the deactivation and the use amount of commercial catalysts and reduce the reaction cost. But biochar only plays a role in tar removal above 700 ℃. While the optimum pyrolysis temperature of biomass is generally considered to be around 500 ℃.
ZSM-5 is often used in catalytic pyrolysis reactions of biomass, which can improve the quality of bio-oil to some extent. However, ZSM-5 has smaller pore diameter and larger reaction diffusion resistance for macromolecules, and reactants are easy to coke and deactivate on the surface of the ZSM-5, so that the reduction of the deactivation of the catalyst is an important aspect for the efficient utilization of the catalyst. ZSM-5 has high thermal stability, one of the highest thermal stability known for zeolites, and can withstand the high temperatures encountered in regenerating the catalyst. And normally, the carbon deposit in ZSM-5 can be burnt out at 900 ℃, the activity of the catalyst is recovered, and the regeneration recovery is realized.
The traditional heating mode is to transfer heat from outside to material according to heat conduction, convection and radiation principles, the heat is always transferred from outside to inside to heat the material, a temperature gradient inevitably exists in the material, so the heated material is uneven, the material is locally overheated, the microwave heating technology is different from the traditional heating mode, the internal friction heat is generated by the high-frequency reciprocating motion of dipole molecules in the heated body, the temperature of the heated material is increased, the internal and external parts of the material can be heated simultaneously without any heat conduction process, the heating speed is high and uniform, and the heating purpose can be achieved only by a fraction or a tenth of the energy consumption of the traditional heating mode.
In the conventional biomass pyrolysis technology, the catalytic pyrolysis and the catalyst regeneration of materials are carried out separately, and the reaction efficiency is low. A continuous reaction method and device integrating catalytic pyrolysis, tar removal and catalyst regeneration into a whole is developed, microwaves are used as heat sources, guiding heat supply is carried out according to the positions of different reaction areas and the temperature requirements, and the method and device are beneficial to improving the reaction efficiency and reducing the energy consumption.
Disclosure of Invention
In order to overcome the defects and shortcomings of the prior art, the invention aims to provide a biomass continuous catalytic pyrolysis method and an integrated device thereof, wherein microwaves are used as main heat sources, and the heat supply quantity is controlled according to the real-time temperature of different reaction areas.
In order to achieve the above object, the present invention is achieved by the following technical solutions.
The invention provides a biomass microwave catalytic pyrolysis integrated device for catalyst regeneration, which comprises a gas device, a vertical quartz tube, a microwave heating device, a catalyst regeneration zone, a catalytic reforming zone, an inactive catalyst collecting zone, a screw feeder and a condensing zone; the gas device is connected to the side wall of the vertical quartz tube, inert gas is introduced into the vertical quartz tube, biomass is placed in the vertical quartz tube, and the inert gas provides an anaerobic environment and carrier gas for the biomass; the vertical quartz tube sequentially comprises a feeding area, a pyrolysis area, a tar removal area and a discharging area from top to bottom, wherein an inlet is arranged on the feeding area, an outlet is arranged at the bottom of the discharging area, biomass is added from the inlet, pyrolysis gas and biochar are generated after the biomass is pyrolyzed in the pyrolysis area, the biochar enters the tar removal area to form a biochar bed layer, the pyrolysis gas flows downwards along with carrier gas to the tar removal area to remove tar, and the biochar is discharged from the outlet; one side of the catalytic reforming zone is connected with the side wall of the vertical quartz tube of the discharging zone, the other side of the catalytic reforming zone is connected with the condensing zone, a catalyst is placed in the catalytic reforming zone, pyrolysis gas flow after tar removal is cracked and catalyzed by the catalytic reforming zone, and pyrolysis gas after pyrolysis and catalysis enters the condensing zone to be collected; the lower part of the catalytic reforming zone is connected with an inactivated catalyst collecting zone, the inactivated catalyst collecting zone is used for collecting the inactivated catalyst in the catalytic reforming zone, the upper part of the catalytic reforming zone is connected with a catalyst regeneration zone, and the catalyst regeneration zone is used for regenerating the inactivated catalyst; a spiral feeder is connected between the deactivated catalyst collecting area and the catalyst regeneration area, the deactivated catalyst is added into the catalyst regeneration area through the spiral feeder, and after the deactivated catalyst is regenerated, the deactivated catalyst returns to the catalytic reforming area from the catalyst regeneration area; the microwave heating device is arranged between the vertical quartz tube and the catalyst regeneration zone, the guide device is arranged on the outer wall of the microwave heating device, and the microwave heating device supplies heat to the pyrolysis zone, the tar removal zone, the catalyst regeneration zone and the catalytic reforming zone through the guide device.
Preferably, an opening is arranged at the upper part of the catalyst regeneration zone, deactivated catalyst and air are added into the catalyst regeneration zone through the opening, the bottom of the catalyst regeneration zone is a heat insulation layer, the heat of the catalyst regeneration zone is prevented from directly radiating the catalytic reforming zone, the temperature of the catalytic reforming zone is overhigh, the side wall of the catalyst regeneration zone is a heat conduction layer, the heat of the catalyst regeneration zone radiates to the pyrolysis zone, the tar removal zone and the catalytic reforming zone of the vertical quartz tube through the side wall, and the pyrolysis zone is used for pyrolysis of biomass in the pyrolysis zone, tar removal of pyrolysis gas and pyrolysis catalytic auxiliary heat supply of pyrolysis gas.
Preferably, the integrated device further comprises a valve, wherein the valve comprises a first valve, a second valve and a third valve; a first pipeline is connected between the catalyst regeneration zone and the catalytic reforming zone, and a first valve and a second valve are distributed on the first pipeline from top to bottom; a second pipeline is connected between the catalytic reforming zone and the deactivated catalyst collecting zone, and third valves are distributed on the second pipeline.
Preferably, the integrated device further comprises a temperature controller, wherein the temperature controller comprises a first temperature controller, a second temperature controller and a third temperature controller, and the first temperature controller is arranged on the side wall of the vertical quartz tube of the pyrolysis zone and used for monitoring the temperature of the pyrolysis zone; the second temperature controller is arranged on the side wall of the vertical quartz tube in the tar removing area and is used for monitoring the temperature of the tar removing area; the third temperature controller is arranged on the catalytic reforming zone and is used for monitoring the temperature of the catalytic reforming zone.
Preferably, the integrated device further comprises a heat collection box, wherein the heat collection box is a cavity surrounded by a thermal resistance material layer, and the pyrolysis zone, the tar removal zone, the catalytic reforming zone and the catalyst regeneration zone of the vertical quartz tube are positioned in the cavity.
Preferably, the integrated device further comprises a flowmeter, the flowmeter comprises a first flowmeter and a second flowmeter, the gas device is connected with the vertical quartz tube through parallel pipelines, and the parallel pipelines comprise an upper pipeline and a lower pipeline; one end of the upper pipeline is connected with the gas device, and the other end of the upper pipeline is connected with the side wall of the vertical quartz tube in the feeding area; one end of the lower pipeline is connected with the gas device, and the other end of the lower pipeline is connected with the side wall of the vertical quartz tube in the discharging area; the first flowmeter is arranged on the upper pipeline and used for controlling the flow of inert gas in the upper pipeline; the second flowmeter is arranged on the lower pipeline and used for controlling the inert gas flow of the lower pipeline.
Preferably, the joint of the vertical quartz tube and the catalytic reforming zone and the joint of the catalytic reforming zone and the condensing zone are provided with quartz wool interlayers.
Preferably, the condensing zone comprises a condensing device and a gas collecting device, one side of the condensing device is connected with the catalytic reforming zone, the other side of the condensing device is connected with the gas collecting device, pyrolysis gas passing through the catalytic reforming zone is catalytically cracked and then enters the condensing device, condensable gas in the pyrolysis gas is condensed into liquid, and non-condensable gas enters the gas collecting device to be collected.
Preferably, the valve is an adiabatic valve, after the deactivated catalyst is regenerated in the catalyst regeneration zone, the first valve is opened, the second valve is closed, after the first pipeline between the first valve and the second valve is filled with the regenerated catalyst, the first valve is closed, the regenerated catalyst is stored in the first pipeline between the first valve and the second valve, when the temperature of the regenerated catalyst is reduced to the temperature of the catalytic reforming zone, the second valve is opened, and the regenerated catalyst returns to the catalytic reforming zone; the diameter of the inlet of the vertical quartz tube is larger than that of the outlet, so that the biomass is ensured to stay in the vertical quartz tube for a plurality of times.
Preferably, the microwave heating device is square, and the guiding device is arranged on the outer wall of the periphery of the microwave heating device.
The invention also provides a method for carrying out biomass catalytic pyrolysis by using the biomass microwave catalytic pyrolysis integrated device regenerated by the catalyst, which comprises the following steps:
1) Opening a gas device, and introducing inert gas into the integrated device to ensure the anaerobic environment of biomass;
2) Starting a microwave heating device, controlling the microwave emission amount and the wavelength, and heating a pyrolysis zone, a tar removal zone, a catalytic reforming zone and a catalyst regeneration zone of the vertical quartz tube at the same time, so that the pyrolysis zone of the vertical quartz tube reaches a temperature of 500-550 ℃, the tar removal zone of the vertical quartz tube reaches a temperature of 700-750 ℃, the catalytic reforming zone reaches a temperature of 450-500 ℃, the catalyst regeneration zone is heated to 850-900 ℃, and the pyrolysis zone, the tar removal zone and the catalytic reforming zone of the vertical quartz tube receive corresponding radiant heat of the catalyst regeneration zone;
3) Biomass is added from an inlet of a feeding zone, pyrolysis gas and biochar are generated after the biomass is pyrolyzed in a pyrolysis zone of a vertical quartz tube, the biochar forms a biochar bed layer, namely a tar removal zone, in the vertical quartz tube, the pyrolysis gas downwards flows through the tar removal zone along with carrier gas to remove tar, pyrolysis gas flow after tar removal is pyrolyzed and catalyzed by a catalytic reforming zone, and pyrolysis gas after pyrolysis and catalysis enters a condensing zone to be collected;
4) The catalyst in the catalytic reforming zone is deactivated and then is collected in a deactivated catalyst collecting zone, and then is sent to a catalyst regenerating zone through a screw feeder, the deactivated catalyst is calcined for 3-5 hours at 850-900 ℃ in the catalyst regenerating zone, carbon deposit is burnt out, the regeneration of the deactivated catalyst is realized, and then the deactivated catalyst is returned to the catalytic reforming zone.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the invention, two processes of catalytic pyrolysis and catalyst regeneration which are commonly separated in the existing catalytic pyrolysis technology are connected in the same set of device, so that the reaction efficiency is improved, and the occupied space of the device is greatly reduced;
(2) The invention utilizes the microwave heating device to supply heat to the pyrolysis zone, the tar removing zone, the catalytic reforming zone and the catalyst regeneration zone in the integrated device, and adjusts the emission amount and wavelength of microwaves according to the real-time temperature of different reaction zones, thereby enhancing the adjustment flexibility of the device. The pyrolysis zone and the tar removal zone can reach the control temperature faster by utilizing microwave heating, and the reaction heat efficiency is improved. The excess heat quantity after the high-temperature reaction at 850-900 ℃ required by the catalyst regeneration is also utilized to radiate heat to the pyrolysis zone, the tar removal zone and the catalytic reforming zone, so that the energy utilization efficiency is improved;
(3) According to the invention, solid residues after biomass pyrolysis reaction are used as a biochar layer, and the characteristics of loose and porous biochar are utilized to remove tar from pyrolysis gas, so that the deactivation rate of a catalyst in a subsequent catalytic reforming zone is slowed down, and the utilization efficiency of biomass and the catalyst is improved.
Drawings
Fig. 1 is a schematic diagram of a biomass microwave catalytic pyrolysis integrated device for catalyst regeneration provided in the examples.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Examples
The embodiment provides a biomass microwave catalytic pyrolysis integrated device for catalyst regeneration, which comprises a gas device 1, a vertical quartz tube 4, a microwave heating device 7, a catalyst regeneration zone 8, a catalytic reforming zone 11, an inactive catalyst collecting zone 13, a screw feeder 16 and a condensing zone; the gas device 1 is connected to the side wall of the vertical quartz tube 4, inert gas is introduced into the vertical quartz tube 4, biomass is placed in the vertical quartz tube 4, and the inert gas provides an oxygen-free environment and carrier gas for the biomass; the vertical quartz tube 4 sequentially comprises a feeding area, a pyrolysis area, a tar removal area and a discharging area from top to bottom, wherein an inlet is arranged on the feeding area, an outlet is arranged at the bottom of the discharging area, biomass is added from the inlet, pyrolysis gas and biochar are generated after the biomass is pyrolyzed in the pyrolysis area, the biochar enters the tar removal area to form a biochar bed layer, the pyrolysis gas downwards flows through the tar removal area along with carrier gas to remove tar, and the biochar is discharged from the outlet; one side of the catalytic reforming zone 11 is connected with the bottom end of the side wall of the vertical quartz tube 4 of the discharging zone, the other side is connected with the condensing zone, a catalyst is placed in the catalytic reforming zone 11, pyrolysis gas after tar removal is cracked and catalyzed by the catalytic reforming zone 11, and pyrolysis gas after cracking and catalysis enters the condensing zone to be collected; the lower part of the catalytic reforming zone 11 is connected with an inactivated catalyst collecting zone 13, the inactivated catalyst collecting zone 13 is used for collecting the inactivated catalyst in the catalytic reforming zone 11, the upper part of the catalytic reforming zone 11 is connected with a catalyst regenerating zone 8, and the catalyst regenerating zone 8 is used for regenerating the inactivated catalyst; a screw feeder 16 is connected between the deactivated catalyst collecting zone 13 and the catalyst regeneration zone 8, the deactivated catalyst is added into the catalyst regeneration zone 8 through the screw feeder 16, and after the deactivated catalyst is regenerated, the deactivated catalyst returns to the catalytic reforming zone 11 from the catalyst regeneration zone 8; the microwave heating device 7 is arranged between the vertical quartz tube 4 and the catalyst regeneration zone 8, a guiding device is arranged on the outer wall of the microwave heating device 7, and the microwave heating device 7 supplies heat to the pyrolysis zone, the tar removal zone, the catalyst regeneration zone 8 and the catalytic reforming zone 11 through the guiding device.
The upper portion of the catalyst regeneration zone 8 is provided with an opening, deactivated catalyst and air are added into the catalyst regeneration zone 8 through the opening, the bottom of the catalyst regeneration zone 8 is a heat insulation layer, heat provided by the catalyst regeneration zone 8 is prevented from directly radiating the catalytic reforming zone 11, the temperature of the catalytic reforming zone 11 is overhigh, the side wall of the catalyst regeneration zone 8 is a heat conduction layer, the heat of the catalyst regeneration zone 8 radiates to the pyrolysis zone and the tar removal zone of the vertical quartz tube 4 and the catalytic reforming zone 11 through the side wall, and the pyrolysis zone is used for pyrolysis of biomass, tar removal of pyrolysis gas and pyrolysis catalytic auxiliary heat supply of pyrolysis gas.
The integrated device also comprises valves, wherein the valves comprise a first valve 9, a second valve 10 and a third valve 12; a first pipeline is connected between the catalyst regeneration zone 8 and the catalytic reforming zone 11, and a first valve 9 and a second valve 10 are distributed on the first pipeline from top to bottom; a second conduit is connected between the catalytic reforming zone 11 and the deactivated catalyst collection zone 13, and a third valve 12 is distributed over the second conduit.
The integrated device further comprises a temperature controller, wherein the temperature controller comprises a first temperature controller 5, a second temperature controller 6 and a third temperature controller 15, and the first temperature controller 5 is arranged on the side wall of the vertical quartz tube 4 of the pyrolysis zone and is used for monitoring the temperature of the pyrolysis zone; the second temperature controller 6 is arranged on the side wall of the vertical quartz tube 4 arranged in the tar removal zone and is used for monitoring the temperature of the tar removal zone; the third temperature controller 15 is disposed on the catalytic reforming zone 11 and is used for monitoring the temperature of the catalytic reforming zone 11.
The integrated device further comprises a heat collection box 14, wherein the heat collection box 14 is a cavity surrounded by a thermal resistance material layer, and the pyrolysis zone, the tar removal zone, the catalytic reforming zone 11 and the catalyst regeneration zone 8 of the vertical quartz tube 4 are positioned in the cavity.
The integrated device also comprises a flowmeter, wherein the flowmeter comprises a first flowmeter 2 and a second flowmeter 3, the gas device 1 is connected with the vertical quartz tube 4 through parallel pipelines, and the parallel pipelines comprise an upper pipeline and a lower pipeline; one end of the upper pipeline is connected with the gas device 1, and the other end is connected with the side wall of the vertical quartz tube 4 in the feeding area; one end of the lower pipeline is connected with the gas device 1, and the other end is connected with the side wall of the vertical quartz tube 4 in the discharging area; the first flowmeter 2 is arranged on the upper pipeline and is used for controlling the flow of inert gas in the upper pipeline; the second flowmeter 3 is provided on the lower pipe for controlling the flow rate of the inert gas in the lower pipe.
The joint of the vertical quartz tube 4 and the catalytic reforming zone 11 and the joint of the catalytic reforming zone 11 and the condensation zone are provided with quartz wool interlayers.
The condensing zone comprises a condensing device 17 and a gas collecting device 18, one side of the condensing device 17 is connected with the catalytic reforming zone 11, the other side of the condensing device 17 is connected with the gas collecting device 18, pyrolysis gas passing through the catalytic reforming zone 11 is catalytically cracked and then enters the condensing device 17, condensable gas in the pyrolysis gas is condensed into liquid, and non-condensable gas enters the gas collecting device 18 and is collected.
The valve is an adiabatic valve, after the deactivated catalyst is regenerated in the catalyst regeneration zone 8, the first valve 9 is opened, the second valve 10 is closed, after a first pipeline between the first valve 9 and the second valve 10 is filled with the regenerated catalyst, the first valve 9 is closed, the regenerated catalyst is stored in the first pipelines of the first valve 9 and the second valve 10, when the temperature of the regenerated catalyst is reduced to the temperature of the catalytic reforming zone 11, the second valve 10 is opened, and the regenerated catalyst returns to the catalytic reforming zone 11; the diameter of the inlet of the vertical quartz tube 4 is larger than that of the outlet, so that the biomass is ensured to stay in the vertical quartz tube 4 for a plurality of times.
The embodiment provides a method for carrying out biomass catalytic pyrolysis by using a biomass microwave catalytic pyrolysis integrated device regenerated by the catalyst, which comprises the following steps:
1) The gas device 1 is filled with nitrogen, the gas device 1 is opened, the nitrogen is introduced into the integrated device, the anaerobic condition of the pyrolysis reaction is ensured, and the gas flow of the upper pipeline and the lower pipeline is respectively controlled by the first flowmeter 2 and the second flowmeter 3 so as to ensure that the requirement of the integrated device is met;
2) Starting a microwave heating device 7, controlling the microwave emission amount and wavelength, heating a pyrolysis zone, a tar removal zone, a catalytic reforming zone 11 and a catalyst regeneration zone 8 to raise the temperature, enabling the temperature reached by the pyrolysis zone of a vertical quartz tube 4 to be 500 ℃, enabling the temperature reached by the tar removal zone of the vertical quartz tube 4 to be 750 ℃, enabling the temperature reached by a catalytic reforming zone 12 to be 450 ℃, heating the catalyst regeneration zone 8 to raise the temperature to 900 ℃, enabling the pyrolysis zone and the tar removal zone of the vertical quartz tube 4 and the catalytic reforming zone 11 to receive corresponding radiant heat, and adjusting the first microwave heating device 7 and a guiding device thereof according to feedback of a first temperature controller 5, a second temperature controller 6 and a third temperature controller 15 so as to control the temperature; the heat collection box 14 surrounds the vertical quartz tube 4, the catalyst regeneration zone 8 and the catalytic reforming zone 11, and plays a role of collecting the radiant heat of the box-type electric heating furnace, so that the pyrolysis zone, the tar removal zone and the catalytic reforming zone of the vertical quartz tube 4 can reach the set temperature more easily. The heat collection box 14 can ensure a certain heat dissipation capacity to the outside, so that heat is prevented from accumulating in the heat collection box 14, and the heat stability of the whole integrated device is maintained;
3) The biomass is put in from the opening of the vertical quartz tube 4, and the structure of the wide-in and narrow-out of the vertical quartz tube 4 can ensure that the biomass has a certain residence time in the flowing process. Biomass is pyrolyzed in a pyrolysis zone of a vertical quartz tube 4 to generate pyrolysis gas and biochar, the biochar forms a biochar bed layer, namely a tar removal zone, in the vertical quartz tube 4, the pyrolysis gas downwards flows through the tar removal zone along with carrier gas to remove tar, pyrolysis gas flow after tar removal is pyrolyzed and catalyzed in a catalytic reforming zone 11, pyrolysis gas after pyrolysis catalysis enters a condensing device 17 of a condensing zone, condensable gas is condensed into liquid, and non-condensable gas is collected in a gas collecting device and a gas collecting bag 18; in addition, a path of carrier gas is transversely blown into the upper part of the opening of the vertical quartz tube 4 to form a gas barrier, so that pyrolysis gas cannot escape along with biomass from the outlet. A quartz cotton interlayer is arranged between the vertical quartz tube 4 and the catalytic reforming zone 11, so that pyrolysis gas can flow smoothly and materials can be prevented from passing through;
4) After deactivation of the catalytic reforming zone 11, the third valve 12 is opened to allow the deactivated catalyst to fall into the deactivated catalyst collection zone 13. The deactivated catalyst is then fed into the catalyst regeneration zone 8 via a screw feeder 16 to burn off the carbon deposits and effect catalyst regeneration. The deactivated catalyst was calcined and regenerated in a box-type electric heating furnace at a high temperature of 900 c for 5 hours. The first valve 9 is then opened and the second valve 10 remains closed. When the pipe between the first valve 9 and the second valve 10 is full, the first valve 9 is closed. The regenerated catalyst is temporarily stored in the pipeline between the first valve 9 and the second valve 10, and simultaneously radiates heat to the periphery outwards for cooling. After the regenerated catalyst temperature is reduced to 500 ℃, the first valve 9 is kept closed, and the second valve 10 is opened, so that the regenerated catalyst falls into the catalytic reforming zone 11 to participate in the reaction. The joint of the catalytic reforming zone 11 and the pyrolysis gas channels at the left end and the right end is also provided with a quartz cotton interlayer, so that the flow of the pyrolysis gas is ensured and the catalyst is prevented from flowing out from the left end and the right end.
The embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principles of the invention should be made and equivalents should be construed as falling within the scope of the invention.
Claims (6)
1. The biomass microwave catalytic pyrolysis integrated device for regenerating the catalyst is characterized by comprising a gas device (1), a vertical quartz tube (4), a microwave heating device (7), a catalyst regeneration zone (8), a catalytic reforming zone (11), an inactive catalyst collecting zone (13), a spiral feeder (16) and a condensing zone; the gas device (1) is connected to the side wall of the vertical quartz tube (4), inert gas is introduced into the vertical quartz tube (4), biomass is placed in the vertical quartz tube (4), and the inert gas provides an anaerobic environment and carrier gas for the biomass; the vertical quartz tube (4) is sequentially provided with a feeding area, a pyrolysis area, a tar removal area and a discharging area from top to bottom, wherein an inlet is arranged on the feeding area, an outlet is arranged at the bottom of the discharging area, biomass is added from the inlet, pyrolysis gas and biochar are generated after the biomass is pyrolyzed in the pyrolysis area, the biochar enters the tar removal area to form a biochar bed layer, the pyrolysis gas downwards flows through the tar removal area along with carrier gas to remove tar, and the biochar is discharged from the outlet; one side of the catalytic reforming zone (11) is connected with the side wall of the vertical quartz tube (4) of the discharging zone, the other side is connected with the condensing zone, a catalyst is placed in the catalytic reforming zone (11), pyrolysis gas flow after tar removal is subjected to pyrolysis catalysis through the catalytic reforming zone (11), and pyrolysis gas after pyrolysis catalysis enters the condensing zone to be collected; the lower part of the catalytic reforming zone (11) is connected with an inactive catalyst collecting zone (13), the inactive catalyst collecting zone (13) is used for collecting inactive catalyst in the catalytic reforming zone (11), the upper part of the catalytic reforming zone (11) is connected with a catalyst regenerating zone (8), and the catalyst regenerating zone (8) is used for regenerating the inactive catalyst; a screw feeder (16) is connected between the deactivated catalyst collecting zone (13) and the catalyst regeneration zone (8), the deactivated catalyst is added into the catalyst regeneration zone (8) through the screw feeder (16), and after being regenerated, the deactivated catalyst returns to the catalytic reforming zone (11) from the catalyst regeneration zone (8); the microwave heating device (7) is arranged between the vertical quartz tube (4) and the catalyst regeneration zone (8), a guiding device is arranged on the outer wall of the microwave heating device (7), and the microwave heating device (7) supplies heat to the pyrolysis zone, the tar removal zone, the catalyst regeneration zone (8) and the catalytic reforming zone (11) through the guiding device; an opening is arranged at the upper part of the catalyst regeneration zone (8), deactivated catalyst is added into the catalyst regeneration zone (8) through the opening, air is introduced into the catalyst regeneration zone (8), the bottom of the catalyst regeneration zone (8) is a heat insulation layer, the residual heat after the deactivated catalyst in the catalyst regeneration zone (8) directly irradiates the catalytic reforming zone (11), the temperature of the catalytic reforming zone (11) is overhigh, the side wall of the catalyst regeneration zone (8) is a heat conduction layer, the residual heat after the deactivated catalyst in the catalyst regeneration zone (8) is irradiated to the pyrolysis zone, the tar removal zone and the catalytic reforming zone (11) of the vertical quartz tube (4) through the side wall, the pyrolysis catalyst is used for auxiliary heat supply for pyrolysis of biomass in a pyrolysis zone, tar removal of pyrolysis gas and pyrolysis catalysis of the pyrolysis gas; the integrated device also comprises valves, wherein the valves comprise a first valve (9), a second valve (10) and a third valve (12); a first pipeline is connected between the catalyst regeneration zone (8) and the catalytic reforming zone (11), and a first valve (9) and a second valve (10) are distributed on the first pipeline from top to bottom; a second pipeline is connected between the catalytic reforming zone (11) and the deactivated catalyst collecting zone (13), and a third valve (12) is distributed on the second pipeline; the integrated device further comprises a temperature controller, wherein the temperature controller comprises a first temperature controller (5), a second temperature controller (6) and a third temperature controller (15), and the first temperature controller (5) is arranged on the side wall of the vertical quartz tube (4) of the pyrolysis zone and is used for monitoring the temperature of the pyrolysis zone; the second temperature controller (6) is arranged on the side wall of the vertical quartz tube (4) of the tar removal zone and is used for monitoring the temperature of the tar removal zone; the third temperature controller (15) is arranged on the catalytic reforming zone (11) and is used for monitoring the temperature of the catalytic reforming zone (11); the integrated device also comprises a flowmeter, wherein the flowmeter comprises a first flowmeter (2) and a second flowmeter (3), the gas device (1) is connected with the vertical quartz tube (4) through parallel pipelines, and the parallel pipelines comprise an upper pipeline and a lower pipeline; one end of the upper pipeline is connected with the gas device (1), and the other end is connected with the side wall of the vertical quartz tube (4) of the feeding area; one end of the lower pipeline is connected with the gas device (1), and the other end is connected with the side wall of the vertical quartz tube (4) of the discharging area; the first flowmeter (2) is arranged on the upper pipeline and is used for controlling the inert gas flow of the upper pipeline; the second flowmeter (3) is arranged on the lower pipeline and is used for controlling the inert gas flow of the lower pipeline; the arrangement of the lower pipeline enables a path of carrier gas to be transversely blown into the upper side of the opening of the vertical quartz tube, so that a gas barrier is formed, and pyrolysis gas is ensured not to escape along with biochar from the outlet.
2. The biomass microwave catalytic pyrolysis integrated device for regenerating catalysts according to claim 1, characterized in that the integrated device further comprises a heat collection box (14), wherein the heat collection box (14) is a cavity surrounded by a heat-resistant material layer, and the pyrolysis zone and tar removal zone of the vertical quartz tube (4), the catalytic reforming zone (11) and the catalyst regeneration zone (8) are positioned in the cavity.
3. The biomass microwave catalytic pyrolysis integrated device for regenerating catalysts according to claim 1, characterized in that the junction of the vertical quartz tube (4) and the catalytic reforming zone (11) and the junction of the catalytic reforming zone (11) and the condensation zone are provided with quartz cotton barriers.
4. The biomass microwave catalytic pyrolysis integrated device for regenerating catalysts according to claim 1, wherein the condensing zone comprises a condensing device (17) and a gas collecting device (18), one side of the condensing device (17) is connected with the catalytic reforming zone (11), the other side of the condensing device is connected with the gas collecting device (18), pyrolysis gas passing through the catalytic reforming zone (11) is catalytically cracked and then enters the condensing device (17), condensable gas in the pyrolysis gas is condensed into liquid, and non-condensable gas enters the gas collecting device (18) and is collected.
5. The biomass microwave catalytic pyrolysis integrated device for regenerating a catalyst according to claim 1, wherein the valve is an adiabatic valve, after the catalyst regeneration zone (8) regenerates, the first valve (9) is opened, the second valve (10) is closed, after a first pipeline between the first valve (9) and the second valve (10) is filled with the regenerated catalyst, the first valve (9) is closed, the regenerated catalyst is stored in the first pipelines of the first valve (9) and the second valve (10), when the temperature of the regenerated catalyst is reduced to the temperature of the catalytic reforming zone (11), the second valve (10) is opened, and the regenerated catalyst returns to the catalytic reforming zone (11); the diameter of the inlet of the vertical quartz tube (4) is larger than that of the outlet, so that the biomass is ensured to stay in the vertical quartz tube (4) for a plurality of times.
6. A method of biomass catalytic pyrolysis using the catalyst regenerated biomass microwave catalytic pyrolysis integrated apparatus of any one of claims 1 to 5, comprising the steps of:
1) Opening a gas device (1), and introducing inert gas into the integrated device to ensure the anaerobic environment of biomass;
2) Starting a microwave heating device (7), controlling the microwave emission and wavelength, and heating a pyrolysis zone, a tar removal zone, a catalytic reforming zone (11) and a catalyst regeneration zone (8) of a vertical quartz tube (4) at the same time, so that the temperature of the pyrolysis zone of the vertical quartz tube (4) is 500-550 ℃, the temperature of the tar removal zone of the vertical quartz tube (4) is 700-750 ℃, the temperature of the catalytic reforming zone (11) is 450-500 ℃, and the catalyst regeneration zone (8) is heated to 850-900 ℃, and the pyrolysis zone, the tar removal zone and the catalytic reforming zone (11) of the vertical quartz tube (4) receive corresponding radiant heat of the catalyst regeneration zone (8);
3) Biomass is added from an inlet of a feeding zone, pyrolysis gas and biochar are generated after the biomass is pyrolyzed in a pyrolysis zone of a vertical quartz tube (4), the biochar forms a biochar bed layer, namely a tar removal zone, in the vertical quartz tube (4), the pyrolysis gas flows downwards along with carrier gas through the tar removal zone to remove tar, pyrolysis gas flow after tar removal is pyrolyzed and catalyzed by a catalytic reforming zone (11), and pyrolysis gas after pyrolysis catalysis enters a condensing zone to be collected;
4) After the catalyst in the catalytic reforming zone (11) is deactivated, the catalyst is collected in a deactivated catalyst collecting zone (13), then is sent into a catalyst regeneration zone (8) through a screw feeder (16), the deactivated catalyst is calcined for 3-5 hours under the condition of 850-900 ℃ in the catalyst regeneration zone (8), carbon deposition is burnt out, the regeneration of the deactivated catalyst is realized, and then the catalyst returns to the catalytic reforming zone (11).
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