WO2020010675A1 - Procédé et dispositif de pyrolyse de biomasse et d'élimination de goudron à basse température basée sur un point chaud de micro-ondes - Google Patents

Procédé et dispositif de pyrolyse de biomasse et d'élimination de goudron à basse température basée sur un point chaud de micro-ondes Download PDF

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Publication number
WO2020010675A1
WO2020010675A1 PCT/CN2018/102928 CN2018102928W WO2020010675A1 WO 2020010675 A1 WO2020010675 A1 WO 2020010675A1 CN 2018102928 W CN2018102928 W CN 2018102928W WO 2020010675 A1 WO2020010675 A1 WO 2020010675A1
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microwave
tar
biomass
biochar
pyrolysis
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PCT/CN2018/102928
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English (en)
Chinese (zh)
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罗虎
孔令照
鲍利伟
王昊
孙予罕
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中国科学院上海高等研究院
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Publication of WO2020010675A1 publication Critical patent/WO2020010675A1/fr

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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
    • 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
    • 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

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  • the invention relates to a method for removing pyrolysis tar, in particular to a method and a device for low-temperature removal of biomass pyrolysis tar based on microwave hot spots.
  • Biomass pyrolysis tar is a kind of liquid mixture containing low molecular and high molecular oxygen compounds with complex composition. It mainly contains acid, alcohol, ester, ketone, and phenol, etc. It has acidity and its pH value is 2 ⁇ 4. In the meantime, the candle is strong and easily decomposed and unstable. The elements are mainly composed of C, H, O, N and S, which will not only cause waste of energy, but also seriously endanger process equipment. How to convert tar to syngas to the greatest extent in the reaction process is not only of great value to the biomass-to-syngas technology itself, but also has a positive effect on reducing greenhouse gas emissions and reducing the blockage of pipes and rot candles by tar.
  • the biomass pyrolysis and gasification process often uses a two-stage or three-stage process, which separates the pyrolysis and gasification of the biomass, so that each reaction is performed under relatively independent conditions, thereby increasing the concentration of syngas.
  • the multi-stage structure increases the complexity of the reaction, increases the operating cost, limits the processing capacity of the equipment, and it is difficult to achieve the purpose of efficient and low-cost utilization of biomass.
  • a large amount of tar will be generated in the pyrolysis and gasification process.
  • the removal of tar mainly includes physical, thermal cracking and catalytic cracking.
  • the thermal cracking temperature is generally higher than 1000 ° C, which increases the operating cost and equipment requirements.
  • Catalytic reforming has attracted wide attention due to its faster reaction rate and higher removal efficiency.
  • Common catalysts include catalysts such as Ni. Reaction temperature The range is 700-900 ° C.
  • the carbon deposition, deactivation and wear of the catalyst are involved in the reaction process. How to remove tar in the process of biomass pyrolysis at low temperature, high efficiency and low cost, and increase the content of syngas in the product of biomass pyrolysis and gasification is of great significance.
  • Microwave heating has the advantages of immediacy, integrity, selectivity and high efficiency.
  • the content of synthesis gas in the product is higher than that of conventional pyrolysis.
  • biochar is a solid in the pyrolysis process.
  • the product which has a porous structure, contains more alkali metal carbonates in the ash, has the basic conditions for catalytic conversion and catalytic cracking of tar, and is a carbon catalyst with great application potential.
  • the hot spot effect during microwave heating is used to strengthen and promote the removal of tar, and a low-temperature removal of biomass pyrolysis tar based on microwave hot spots is provided.
  • the method and device realize low-temperature and high-efficiency removal of tar in a reactor.
  • the object of the present invention is to provide a method and a device for low-temperature removal of biomass pyrolysis tar based on microwave hotspots.
  • Microwaves are used as heating means to pyrolyze biomass and remove tar.
  • the two processes are coupled in a reactor, and the high-ash biochar generated by pyrolysis is used as a catalyst for tar removal and a carrier generated by microwave hot spots, and a high-temperature microwave hot spot area having both a microwave field and catalytic performance is formed on the surface of biochar .
  • the biomass pyrolysis tar is removed in situ in the microwave hotspot immediately after it is generated, thereby reducing the overall reaction temperature and shortening the reaction time.
  • a first aspect of the present invention provides a method for low-temperature removal of biomass pyrolysis tar based on microwave hot spots, including the following steps:
  • the biomass pyrolysis tar is removed in situ in the microwave hot spot immediately after it is generated.
  • the biomass pyrolysis process and the tar in-situ removal process are coupled in a reactor, that is, the tar in-situ removal is located below the biomass pyrolysis, and the pyrolysis solid product gradually accumulates into a bio-char bed for the in-situ removal of tar.
  • the mass ratio of the second biomass to the solid product obtained from the pyrolysis of the first biomass is 1: 5 to 1:15, such as 1: 5 to 1: 6.67, 1: 6.67 to 1:10, or 1:10 to 1:15;
  • the ash content in the first biomass and the second biomass is 10-15% by weight, such as 10-13.24% by weight or 13.24-15% by weight.
  • the ash includes inorganic salts and metal oxides, and is mainly derived from crops in high saline-alkali areas. , Such as straw, reeds and cotton stalks growing in high saline soil (Shanghai Chongming);
  • the metal content in the biochar bed is 10-30% by weight, such as 10-11% by weight, 11-23% by weight, 23-29% by weight, or 29-30% by weight, ensuring the dielectric loss factor of the metal salt and the carbon skeleton in the biochar
  • the difference in the absorption of microwave energy causes the microwave energy to be non-uniform and induces the generation of microwave hotspots.
  • High-ash biochar produced by pyrolysis is used as a catalyst for tar removal and as a carrier for microwave hotspots.
  • the metal includes one or more of Al, K, Ca, Mg, Fe, and Co.
  • step 1), step 2) and step 3) obtain the anaerobic condition by passing inert gas.
  • the effective reaction temperature for microwave heating is 400-600 ° C, such as 400-450 ° C, 450-500 ° C, or 500-600 ° C.
  • the power range of the microwave heating equipment is 20 ⁇ 1500W, and the power can be adjusted steplessly according to the set temperature.
  • the method further comprises: condensing and separating the product obtained in step 3), and performing gas chromatographic analysis on the obtained gas phase product, realizing the online analysis test of the gas composition, and adjusting the flow rate through a regulating valve before entering the gas chromatography.
  • the condensation may adopt liquid nitrogen secondary condensation.
  • the gas phase product obtained by condensation and separation can also be separated to obtain an inert gas, which is recycled to step 1) as a carrier gas to promote the reforming reaction of carbon dioxide with methane and water, and improve the yield of synthesis gas after various reactions.
  • a device for low-temperature removal of biomass pyrolysis tar based on microwave hotspots includes a device body and a microwave heating component, and the microwave heating component is movably disposed around an outer wall of the device body.
  • the position of the microwave heating component can be appropriately adjusted according to changes in the height and position of the biochar bed to achieve the concentrated use of microwave energy.
  • the microwave heating power range is 20 ⁇ 1500W, and the power can be adjusted steplessly according to the set temperature.
  • the microwave heating component can be moved up and down along the outer wall of the device body.
  • the position of the microwave hotspot area can be adjusted according to the reaction process, that is, the position of the microwave hotspot area can be made according to the height and position of the biochar bed. Appropriate adjustment to achieve the concentrated use of microwave energy.
  • it further comprises a heat insulation layer, which is provided between the microwave heating component and the device body, and the heat insulation layer is provided around the outer wall of the device body.
  • an infrared temperature measuring unit is provided in the thermal insulation layer, and a mode in which the infrared temperature measurement and the thermocouple temperature measurement are mutually corrected can be used to measure and feedback the microwave heating temperature.
  • a biomass feed port is provided above the device body.
  • it further comprises a condensing component and a gas chromatograph, and the device body communicates with the gas chromatograph via the condensing component.
  • it further comprises an inert gas supply component, and the inert gas supply component is in communication with the device body.
  • the inert gas supplying component includes a connected inert gas storage unit and a gas flow meter.
  • the present invention has at least one of the following beneficial effects:
  • the microwave-enhanced area is adjusted according to the reaction process, which can make full use of microwave energy to achieve directional supply of energy and integrally strengthened heating, thereby reducing energy loss and improving reaction efficiency.
  • the present invention uses cheap biochar as a catalyst and uses microwave enhanced heating to avoid problems such as catalyst deactivation and regeneration, increases the tar removal rate, reduces the reaction cost, and increases the efficiency of biomass pyrolysis and gasification.
  • FIG. 1 is a conceptual diagram of a device for low-temperature removal of biomass pyrolysis tar based on microwave hot spots of the present invention.
  • FIG. 2 is a schematic diagram of a device for low-temperature removal of biomass pyrolysis tar based on microwave hot spots of the present invention.
  • FIG. 1 The conceptual diagram of the device for low-temperature biomass pyrolysis tar removal based on microwave hot spots of the present invention is shown in Figure 1.
  • A is a biomass pyrolysis stage
  • B is a mobile microwave-assisted tar removal stage
  • C is a gasification stage.
  • microwave is used as a heating means
  • the two processes of biomass pyrolysis and tar removal are coupled in one reactor
  • the high-ash biochar generated by pyrolysis is used as a catalyst for tar removal and a carrier generated by microwave hot spots.
  • a high-temperature microwave hotspot area with both a microwave field and catalytic properties is formed on the surface of biochar.
  • the biomass pyrolysis tar is removed in situ in the microwave hotspot immediately after it is generated, thereby reducing the overall reaction temperature and shortening the reaction time.
  • a device for low-temperature removal of biomass pyrolysis tar based on microwave hotspots includes a device body 1, a microwave heating component 2, and a thermal insulation layer 3.
  • the thermal insulation layer 3 is provided on the microwave heating component 2 and the device.
  • an infrared temperature measuring unit 4 is provided inside the thermal insulation layer 3;
  • a biomass feed inlet 5 is provided above the device body 1;
  • It includes a condensing part 6 and a gas chromatograph 7.
  • the device body 1 is in communication with the gas chromatograph 7 via the condensing part 6.
  • It also includes an inert gas supply part, which is in communication with the device body 1.
  • the inert gas supply component includes a connected inert gas storage unit 8 and a gas flow meter 9.
  • the biochar bed was heated to 500 ° C by microwave, and 2g of original straw was added to the top (the ash content was 10.15 wt%, Shanghai Chongming).
  • the pyrolysis of the straw produced tar steam, which was purged with a carrier gas (N 2 100mL / min)
  • a carrier gas N 2 100mL / min
  • tar molecules undergo a removal reaction on the surface of the biochar (thermal cracking, catalytic reforming, and reforming reactions between gas molecules), and the reacted gases are fully condensed in a two-stage condenser of liquid nitrogen After that, the remaining tar product was obtained, and the tar removal rate was calculated from the original tar content after weighing.
  • the bed of biochar was heated to 600 ° C by microwave, and 4g of original straw (with an ash content of 10.15% by weight, Shanghai Chongming) was added to the top.
  • the pyrolysis of the straw produced tar steam and passed through the biochar bed under a carrier gas sweep. Layer, tar molecules undergo a removal reaction (thermal cracking, catalytic reforming, and reforming reactions between gas molecules) on the surface of the biochar.
  • the reacted gases are fully condensed in a liquid nitrogen two-stage condenser to obtain the remaining tar product.
  • the pyrolysis tar removal rate was calculated with the original tar content.
  • the biochar bed was heated to 400 ° C by microwave, and 1.3 raw reed straw was added to the top (the ash content was 15.08wt%, Shanghai Chongming).
  • the reed pyrolysis produced tar steam, which was purged with a carrier gas (N 2 100mL / min)
  • a carrier gas N 2 100mL / min
  • tar molecules undergo a removal reaction on the surface of the biochar (thermal cracking, catalytic reforming, and reforming reactions between gas molecules), and the reacted gases are fully condensed in a two-stage condenser of liquid nitrogen After that, the remaining tar product was obtained, and the tar removal rate was calculated from the original tar content after weighing.
  • the bed of biochar was heated to 600 ° C with microwave, and 3g of original reed straw (15.08wt%, Shanghai Chongming) was added on top of it. Pyrolysis of the reed produced tar steam, which was purged with carrier gas (N 2 100mL / min) Through the biochar bed, tar molecules undergo a removal reaction on the surface of the biochar (thermal cracking, catalytic reforming, and reforming reactions between gas molecules), and the reacted gases are fully condensed in a two-stage condenser of liquid nitrogen After that, the remaining tar product was obtained, and the tar removal rate was calculated from the original tar content after weighing.
  • carrier gas N 2 100mL / min
  • the biochar bed was heated to 600 ° C by microwave, and 4g of original cotton straw (13.24% by weight, Shanghai Chongming) was added on top of it.
  • the cotton straw was pyrolyzed to generate tar vapor, which was purged with carrier gas (N 2 100mL / min)
  • carrier gas N 2 100mL / min
  • tar molecules undergo a removal reaction (thermal cracking, catalytic reforming, and reforming reactions between gas molecules) on the surface of the biochar.
  • the reacted gas is fully contained in a two-stage condenser of liquid nitrogen. Residual tar product was obtained after condensation, and the tar removal rate was calculated from the original tar content after weighing.
  • the biochar bed was heated to 500 ° C by microwave, and 1.3g of original cotton straw (13.24% by weight, Shanghai Chongming) was added on top of it.
  • the cotton straw was pyrolyzed to generate tar steam, which was purged with carrier gas (N 2 100mL / min)
  • carrier gas N 2 100mL / min
  • tar molecules are removed on the surface of the biochar (thermal cracking, catalytic reforming, and reforming reactions between gas molecules), and the reacted gases are in a two-stage condenser of liquid nitrogen. After full condensation, the remaining tar product was obtained. After weighing, the tar removal rate was calculated from the original tar content.
  • the biochar bed was heated to 450 ° C by microwave, and 2g of original straw was added to the top (the ash content was 10.15 wt%, Shanghai Chongming).
  • the pyrolysis of the straw produced tar steam, which was purged with a carrier gas (N 2 100mL / min)
  • a carrier gas N 2 100mL / min
  • tar molecules undergo a removal reaction on the surface of the biochar (thermal cracking, catalytic reforming, and reforming reactions between gas molecules), and the reacted gases are fully condensed in a two-stage condenser of liquid nitrogen After that, the remaining tar product was obtained, and the tar removal rate was calculated from the original tar content after weighing.
  • the biochar bed was heated to 600 ° C by microwave, and 3g of original straw (with an ash content of 10.15% by weight, Shanghai Chongming) was added on top of it. Pyrolysis of the straw produced tar steam under a carrier gas purge (N 2 100mL / min) Through the biochar bed, tar molecules undergo a removal reaction on the surface of the biochar (thermal cracking, catalytic reforming, and reforming reactions between gas molecules), and the reacted gases are fully condensed in a two-stage condenser of liquid nitrogen After that, the remaining tar product was obtained, and the tar removal rate was calculated from the original tar content after weighing.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Processing Of Solid Wastes (AREA)
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Abstract

La présente invention concerne un procédé et un dispositif de pyrolyse de biomasse et d'élimination de goudron à basse température basée sur un point chaud de micro-ondes, le procédé comprenant les étapes suivantes : 1) sous des conditions anaérobies, la pyrolyse d'une première biomasse pour obtenir un lit de biocharbon solide ; 2) sous des conditions anaérobies, la soumission de la couche de lit de biocharbon obtenue dans l'étape 1) au chauffage par micro-ondes pour former une région de point chaud de micro-ondes ; et 3) sous des conditions anaérobies, l'addition d'une seconde biomasse pour former une couche de lit de pyrolyse de biomasse au-dessus de la couche de lit de biocharbon, sa pyrolyse, et ensuite l'élimination in situ de goudron de la couche de lit de biocharbon à travers la région de point chaud de micro-ondes. Dans la présente invention, les micro-ondes sont utilisées comme moyen de chauffage, et un biocharbon à haute teneur en cendres générées par la pyrolyse est utilisé comme catalyseur pour l'élimination de goudron et comme support pour la génération de point chaud de micro-ondes pour former une région de point chaud de micro-ondes à haute température ayant à la fois un champ de micro-ondes et une performance catalytique sur la surface du biocharbon. Après la génération de goudron de pyrolyse de biomasse, l'élimination immédiate in situ dans la région de point chaud de micro-ondes est réalisée, la température réactionnelle globale est réduite, et la durée de la réaction est raccourcie.
PCT/CN2018/102928 2018-07-12 2018-08-29 Procédé et dispositif de pyrolyse de biomasse et d'élimination de goudron à basse température basée sur un point chaud de micro-ondes WO2020010675A1 (fr)

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CN110066670A (zh) * 2019-05-13 2019-07-30 华南理工大学 催化剂再生的生物质连续催化热解方法及一体化装置
CN110066671A (zh) * 2019-05-13 2019-07-30 华南理工大学 催化剂再生的生物质微波催化热解方法及其一体化装置
CN113897208B (zh) * 2021-10-09 2023-01-10 重庆三峡学院 一种循环热解焦油的方法
CN115254126B (zh) * 2022-08-24 2023-05-26 云南大学 一种生物炭基双功能型催化剂的制备方法

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