CN111117676A - Microwave continuous frequency modulation synergistic biomass directional depolymerization device and use method thereof - Google Patents

Microwave continuous frequency modulation synergistic biomass directional depolymerization device and use method thereof Download PDF

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Publication number
CN111117676A
CN111117676A CN202010063629.6A CN202010063629A CN111117676A CN 111117676 A CN111117676 A CN 111117676A CN 202010063629 A CN202010063629 A CN 202010063629A CN 111117676 A CN111117676 A CN 111117676A
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microwave
biomass
quartz tube
tube reactor
frequency modulation
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蒋剑春
王佳
周铭昊
孙云娟
刘朋
王奎
叶俊
李静
夏海虹
徐俊明
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Institute of Chemical Industry of Forest Products of CAF
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Institute of Chemical Industry of Forest Products of CAF
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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
    • C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
    • C10B53/02—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of cellulose-containing material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
    • B01J19/122—Incoherent waves
    • B01J19/126—Microwaves
    • 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
    • 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
    • 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
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00—Technologies for the production of fuel of non-fossil origin
    • Y02E50/10—Biofuels, e.g. bio-diesel
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/141—Feedstock
    • Y02P20/145—Feedstock the feedstock being materials of biological origin

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  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Health & Medical Sciences (AREA)
  • Electromagnetism (AREA)
  • Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Toxicology (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • General Chemical & Material Sciences (AREA)
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Abstract

The invention discloses a microwave continuous frequency modulation synergistic biomass directional depolymerization device and a use method thereof, and belongs to the technical field of biomass resource utilization. The device comprises a microwave continuous frequency modulation power supply, a microwave resonant cavity, a quartz tube reactor and a product treatment device; a microwave feed port is arranged on the microwave resonant cavity, and a microwave continuous frequency modulation power supply is connected with the microwave feed port; the quartz tube reactor is connected with an inert gas source, a biomass feed hopper is connected to the quartz tube reactor, a catalyst filling screen spacer is arranged in the middle of the quartz tube reactor, an infrared thermal imager is arranged above the quartz tube reactor, and an infrared thermometer is arranged at the position of the catalyst filling screen spacer; the product treatment device comprises a condensation system and a gas collection bag, wherein the condensation system is arranged at the outlet of the quartz tube reactor, and the gas collection bag is arranged at the outlet of the condensation system. The invention achieves the aims of reducing the cracking activation energy of the biomass and realizing the directional depolymerization by matching the microwave emission frequency with the three major components of the biomass and the intrinsic resonance frequency of the catalyst.

Description

Microwave continuous frequency modulation synergistic biomass directional depolymerization device and use method thereof
Technical Field
The invention belongs to the technical field of biomass resource utilization, and particularly relates to a microwave continuous frequency modulation synergistic biomass directional depolymerization device and a use method thereof.
Background
Lignocellulosic biomass is an ideal alternative to fossil energy. As a big agricultural country, China has abundant agriculture and forestry biomass resources. According to the calculation of 'world energy prospect-Chinese special report' in 2017, 3 hundred million tons of crop straw wastes and 3 hundred million tons of forestry wastes can be generated in China every year. Therefore, the method makes full use of agriculture and forestry biomass resources and is a feasible way for relieving the dependence of China on petrochemical energy. With the increasing exhaustion of fossil energy, the production and application of energy and fine chemicals in China are influenced, and further the daily life of people is seriously influenced. The biomass is used as an ideal substitute resource of fossil energy, and abundant wood fiber resources are efficiently utilized, so that the biomass has important significance on the sustainable development of China.
The wood fiber conversion technology mainly comprises a thermochemical conversion method, a biochemical method and the like. At present, most of biomass thermochemical conversion supplies heat through a traditional electric heating mode, and has the defects of high heating energy consumption, low heating speed, long heating time, unstable temperature control and the like. The wood fiber is a complex macromolecule formed by connecting cellulose, hemicellulose and lignin through a C-O bond, a C-C bond and the like, and in the high-value utilization process of the wood fiber, the selective breakage of the C-O bond and the C-C bond in the wood fiber macromolecule is difficult to realize due to the defects of non-uniformity, difficult temperature control and the like of the traditional heating mode. And the microwave heating has the advantages of low heating energy consumption, high heating speed, uniform heating and the like, so the microwave heating is widely concerned in the aspect of utilization of the wood fiber biomass. However, it is worth pointing out that the microwave heating shows better utilization prospect in various aspects of wood fiber liquefaction, pyrolysis, gasification and the like compared with the traditional heating mode. However, the microwave heating usually adopts a fixed frequency of 2.45GHz at present, mainly because the microwave emission frequency is consistent with the intrinsic resonance frequency of water molecules, so that the resonance of water molecules can be realized to achieve a better heating effect. Because the wood fiber biomass is composed of cellulose, hemicellulose and lignin, the eigenfrequency of the wood fiber biomass is different from that of water molecules, so that the conventional microwave heating can not realize the 'resonance' broken bond of three component molecules, and the catalyst is also composed of different active components and carriers, and the eigenfrequency of the wood fiber biomass is also different from that of the water molecules, so that the problem that how to realize the 'resonance' of the biomass components or the active components of the catalyst with different eigen resonance frequencies is solved, thereby achieving the aim of oriented depolymerization of the biomass.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a microwave continuous frequency modulation synergistic biomass directional depolymerization device, compared with the traditional microwave-assisted biomass pyrolysis device with a fixed emission frequency of 2.45GHz, the emission frequency of the microwave reactor can be matched with the intrinsic resonance frequency of three-component molecules of biomass cellulose, hemicellulose and lignin and a catalyst, so as to achieve the aims of reducing the cracking activation energy of biomass and realizing the directional depolymerization of the three major components of the biomass. The invention aims to solve another technical problem of providing a using method of the microwave continuous frequency modulation synergistic biomass directional depolymerization device, which has a simple structure and is convenient to operate, and can realize directional catalytic depolymerization of three major elements of biomass.
The technical scheme is as follows: in order to solve the problems, the technical scheme adopted by the invention is as follows:
a microwave continuous frequency modulation cooperated biomass directional depolymerization device comprises a microwave continuous frequency modulation power supply, a microwave resonant cavity, a quartz tube reactor and a product treatment device; a microwave feed port is arranged on the microwave resonant cavity, and the microwave continuous frequency modulation power supply is connected with the microwave feed port; the quartz tube reactor is arranged in the microwave resonant cavity and is connected with an inert gas source, a biomass feed hopper is connected to the quartz tube reactor, and a catalyst filling screen mesh spacer is arranged in the middle of the quartz tube reactor; an infrared thermal imager is arranged above the quartz tube reactor and used for monitoring the distribution condition of the cross-section temperature field of the catalyst bed layer in real time; an infrared thermometer is arranged at the position of the catalyst filling screen mesh spacer and is used for detecting the temperature condition of the catalyst bed layer along the axial section of the quartz tube reactor; the product treatment device comprises a condensation system and a gas collection bag, wherein the condensation system is arranged at an outlet of the quartz tube reactor, the gas collection bag is arranged at an outlet of the condensation system, condensable product components after reaction are condensed into liquid biological oil through the condensation system, and the non-condensable part is collected into the gas collection bag.
The microwave continuous frequency modulation is cooperated with the directional biomass depolymerization device, the product treatment device further comprises an online detection system, and the online detection system is arranged between the outlet of the quartz tube reactor and the condensation system.
The microwave continuous frequency modulation is cooperated with the biomass directional depolymerization device, and the infrared thermometer is in a non-contact type.
The microwave continuous frequency modulation is cooperated with the biomass directional depolymerization device, and the online detection system is a gas phase-mass spectrometer.
According to the microwave continuous frequency modulation collaborative biomass directional depolymerization device, the microwave continuous frequency modulation power supply is composed of different frequency modulation modules, the microwave emission frequency is continuously adjustable between 2.45GHz and 8GHz, and the output power is freely adjusted between 200W and 500W; the frequency adjustment range is 0.1-1000 MHz.
The microwave continuous frequency modulation is cooperated with the biomass directional depolymerization device, and the inner diameter of the quartz tube reactor is 10 mm.
The use method of the microwave continuous frequency modulation synergetic biomass directional depolymerization device specifically comprises the following steps:
1) uniformly arranging a catalyst on a catalyst filling screen mesh spacer, and placing a biomass raw material in a biomass feeding system; starting an inert carrier gas source to purge the quartz tube reactor, and maintaining the inert gas atmosphere in the quartz tube reactor;
2) starting a microwave continuous frequency modulation power supply, enabling microwaves with continuously changed frequencies to enter a microwave resonant cavity through a microwave feed port, arranging a catalyst bed layer on a catalyst filling screen spacer, and gradually heating the catalyst bed layer by continuously absorbing the microwaves with different frequencies, on one hand, monitoring the temperature field change of the cross section of the catalyst bed layer in real time through a thermal imager vertically arranged at the top of a quartz tube, on the other hand, monitoring the temperature of the catalyst along the height section of the quartz tube in real time through a non-contact infrared thermometer, and observing the temperature of the catalyst when the reaction temperature is reached; entering step 3);
3) starting a biomass continuous feeding system, and uniformly feeding the biomass raw material into a quartz tube reactor 4 for a directional catalytic cracking reaction;
4) after the reaction is finished, the product enters a condensing system at the outlet of the quartz tube reactor, the gaseous product is condensed by the condensing system and then is collected into a liquid product, and the non-condensable gaseous product is collected into a gas collecting bag for subsequent off-line analysis.
Has the advantages that: compared with the prior art, the invention has the advantages that:
(1) compared with the traditional microwave-assisted biomass pyrolysis device with the fixed emission frequency of 2.45GHz, the emission frequency of the microwave reactor disclosed by the invention can be matched with the intrinsic resonance frequency of three-component molecules of biomass cellulose, hemicellulose and lignin, so that the pyrolysis activation energy of biomass is reduced, and the directional depolymerization of the three major components of the biomass is realized.
(2) The continuous frequency conversion microwave emission frequency can excite the resonance hot spot of more catalyst active components, thereby achieving the aim of selective catalysis.
Drawings
FIG. 1 is a schematic structural diagram of a microwave continuous frequency modulation synergistic biomass directional depolymerization device.
Detailed Description
The invention is further illustrated by the accompanying drawings and specific examples, which are intended to be illustrative only and not limiting of the scope of the invention, and various equivalent modifications of the invention will become apparent to those skilled in the art after reading the present patent application and are intended to fall within the scope of the appended claims.
Example 1
A microwave continuous frequency modulation cooperated biomass directional depolymerization device, as shown in figure 1. As can be seen from FIG. 1, the apparatus comprises a microwave continuous frequency modulation power supply 1, a microwave resonant cavity 3, a quartz tube reactor 4 and a product treatment apparatus; a microwave feed port 2 is formed in the microwave resonant cavity 3, a microwave continuous frequency modulation power supply 1 is connected with the microwave feed port 2, the microwave continuous frequency modulation power supply 1 is composed of different frequency modulation modules, the microwave transmitting frequency is continuously adjustable between 2.45GHz and 8GHz, and the output power is freely adjusted between 200W and 500W; the frequency adjustment amplitude is 0.1-1000 MHz; the quartz tube reactor 4 is arranged in the microwave resonant cavity 3, a feeding pipeline is arranged on the quartz tube reactor 4, one end of the feeding pipeline is connected with the quartz tube reactor 4, the other end of the feeding pipeline is provided with a biomass feed hopper 7, and the middle part of the feeding pipeline is provided with a catalyst filling screen spacer 5; the quartz tube reactor 4 is connected with an inert gas source, an infrared thermal imager 6 is arranged above the quartz tube reactor 4, a certain distance is reserved between the quartz tube reactor 4 and the infrared thermal imager, the quartz tube reactor and the infrared thermal imager are not in contact, and the distance can ensure that the distribution condition of the cross-section temperature field of the catalyst bed layer can be monitored in real time; a non-contact infrared thermometer 8 is arranged at the position of the catalyst filling screen mesh spacer 5 and is used for detecting the temperature condition of the catalyst bed layer along the axial section of the quartz tube reactor; the product treatment device comprises a condensation system 10, an air collecting bag and an online detection system 9, wherein the online detection system is a gas-mass spectrometer, the condensation system 10 is arranged at the outlet of the quartz tube reactor 4, the online detection system is arranged between the condensation system 10 and the outlet of the quartz tube reactor 4, and the online detection system can carry out real-time online detection on the product; the gas collection bag is arranged at the outlet of the condensing system 10, the condensable product components after reaction are condensed into liquid bio-oil by the condensing system 10, and the non-condensable part is collected into the gas collection bag.
The use method of the microwave continuous frequency modulation synergetic biomass directional depolymerization device specifically comprises the following steps:
1) uniformly arranging a catalyst at the center of a quartz tube reactor, and placing a biomass raw material in a biomass feeding system; starting an inert carrier gas source to purge the quartz tube, and maintaining the inert gas atmosphere in the reaction tube;
2) subsequently, the microwave continuous frequency modulation power supply 1 is turned on, and microwaves with continuously changing frequencies enter the microwave resonant cavity 3 through the feed port and are arranged in a quartz tube (inner diameter: 10mm) catalyst bed layer in the center continuously absorbs microwaves with different frequencies to gradually increase the temperature, on one hand, the temperature field change of the cross section of the catalyst bed layer is monitored in real time through a thermal imaging instrument vertically arranged at the top of the quartz tube, on the other hand, the temperature of the catalyst along the height section of the quartz tube is also monitored in real time through a non-contact infrared temperature measurement system, and the reaction temperature is reached; entering step 3);
3) starting a biomass continuous feeding system 7, uniformly feeding the biomass raw material into a quartz tube reactor 4 for catalytic cracking reaction, and performing biomass directional catalytic depolymerization reaction;
4) after the reaction is finished, the product is subjected to online detection by an online GC/MS detection system at the outlet of the quartz tube reactor, the composition of the reaction product is detected in real time, the gaseous product after the reaction is condensed by a condensation system and then collected into a liquid product, and the non-condensable gaseous product is collected into a gas collection bag for subsequent offline analysis.

Claims (7)

1. A microwave continuous frequency modulation cooperated biomass directional depolymerization device is characterized by comprising a microwave continuous frequency modulation power supply (1), a microwave resonant cavity (3), a quartz tube reactor (4) and a product treatment device; a microwave feed port (2) is formed in the microwave resonant cavity (3), and the microwave continuous frequency modulation power supply (1) is connected with the microwave feed port (2); the quartz tube reactor (4) is arranged in the microwave resonant cavity (3), the quartz tube reactor (4) is connected with an inert gas source, a biomass feed hopper (7) is connected to the quartz tube reactor (4), and a catalyst filling screen spacer (5) is arranged in the middle of the quartz tube reactor; an infrared thermal imager (6) is arranged above the quartz tube reactor (4), and an infrared thermometer (8) is arranged at the position of the catalyst filling screen spacer (5); the product treatment device comprises a condensation system and a gas collecting bag, wherein the condensation system (10) is arranged at the outlet of the quartz tube reactor (4), and the gas collecting bag is arranged at the outlet of the condensation system (10).
2. The microwave continuous frequency modulation cooperative biomass directional depolymerization device according to claim 1, wherein said product treatment device further comprises an on-line detection system (9), said on-line detection system (9) is disposed between the outlet of the quartz tube reactor (4) and the condensation system (10).
3. The microwave continuous frequency modulation cooperative biomass directional depolymerization device according to claim 1, wherein said infrared thermometer (8) is non-contact.
4. The microwave continuous frequency modulation cooperative biomass directional depolymerization device according to claim 2, wherein said on-line detection system (9) is a gas-mass spectrometer.
5. The microwave continuous frequency modulation collaborative biomass directional depolymerization device according to claim 1, wherein the microwave continuous frequency modulation power supply (1) is composed of different frequency modulation modules, the microwave emission frequency is 2.45-8 GHz, the frequency adjustment amplitude is 0.1-1000 MHz, and the output power is 200-500W.
6. The microwave continuous frequency modulation cooperative biomass directional depolymerization device according to claim 1, wherein an inner diameter of the quartz tube reactor (4) is 10 mm.
7. The use method of the microwave continuous frequency modulation cooperative biomass directional depolymerization device according to any one of claims 1 to 6, is characterized by comprising the following steps:
1) uniformly arranging a catalyst on a catalyst filling screen mesh spacer, and placing a biomass raw material in a biomass feeding system; starting an inert carrier gas source to purge the quartz tube reactor, and maintaining the inert gas atmosphere in the quartz tube reactor;
2) starting a microwave continuous frequency modulation power supply (1), allowing microwaves with continuously changed frequencies to enter a microwave resonant cavity (3) through a microwave feed port, arranging a catalyst bed layer on a catalyst filling screen spacer, and continuously absorbing the microwaves with different frequencies to gradually increase the temperature; detecting the temperature of the catalyst by a thermal imager and an infrared thermometer, and entering the step 3) when the temperature reaches the reaction temperature;
3) starting a biomass continuous feeding system (7), and uniformly feeding the biomass raw material into a quartz tube reactor (4) for biomass directional catalytic cracking reaction;
4) after the reaction is finished, the product enters a condensing system at the outlet of the quartz tube reactor, the gaseous product is condensed by the condensing system and then is collected into a liquid product, and the non-condensable gaseous product is collected into a gas collecting bag for subsequent off-line analysis.
CN202010063629.6A 2020-01-19 2020-01-19 Microwave continuous frequency modulation synergistic biomass directional depolymerization device and use method thereof Pending CN111117676A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112710697A (en) * 2020-12-23 2021-04-27 武汉理工大学 High-controllable high-stability automatic sample introduction type photo-thermal catalytic reactor and testing method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112710697A (en) * 2020-12-23 2021-04-27 武汉理工大学 High-controllable high-stability automatic sample introduction type photo-thermal catalytic reactor and testing method

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