CN115584520A - Biomass pyrolysis steam intermediate-temperature electrochemical upgrading process - Google Patents
Biomass pyrolysis steam intermediate-temperature electrochemical upgrading process Download PDFInfo
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- C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
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- C25B3/00—Electrolytic production of organic compounds
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- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
- C25B9/60—Constructional parts of cells
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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- C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
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- 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
Abstract
The invention discloses a biomass pyrolysis steam moderate-temperature electrochemical upgrading process, relates to the technical field of biomass energy utilization, and solves the technical problems of poor thermal stability and low upgrading efficiency of bio-oil extracted from biomass pyrolysis steam; pyrolysis steam is directly introduced into a cathode channel of the proton ceramic exchange membrane electrolytic cell without being cooled, and water steam generated by a steam generator is introduced into an anode of the proton ceramic exchange membrane electrolytic cell; and the proton ceramic exchange membrane electrolytic cell is externally connected with a direct current power supply to carry out electrochemical reaction, so that the quality improvement of the bio-oil in the pyrolysis steam is completed. The biomass pyrolysis steam is directly electrochemically hydrogenated and upgraded without condensation, the number of unsaturated bonds of the biomass pyrolysis oil is obviously reduced, the acidity and viscosity of the biomass pyrolysis oil are reduced, the heat value and stability of the biomass pyrolysis oil are improved, and the quality of the biomass pyrolysis oil is improved.
Description
Technical Field
The application relates to the technical field of biomass energy utilization, in particular to a biomass pyrolysis steam intermediate-temperature electrochemical upgrading process.
Background
Bio-oil is the pyrolysis product of biomass and is the only carbon-containing renewable energy source present in liquid form. Compared with biomass, bio-oil has a high energy density, which is typically up to 10 times the energy density of biomass. The conversion of biomass into bio-oil is a promising low-cost utilization of biomass energy. However, bio-oils currently have no mature industrially applicable or processing technology. The fundamental reason for the difficulty in handling and applying bio-oil is its characteristic physicochemical properties. Bio-oil components are complex (including acids, phenols, alcohols, ketones, and carbohydrates), high in acid value, high in viscosity, and corrosive, making it difficult to transport and store on a large scale. Bio-oils are high in oxygen content (40-50 wt.%), low in calorific value (14-19 MJ/kg), resulting in difficulties in direct application to combustion equipment. Therefore, bio-oils must be refined and upgraded to improve fuel properties or to refine high value added chemicals. At present, the upgrading method of the bio-oil is mainly based on traditional methods such as thermochemical hydrodeoxygenation, catalytic cracking, steam reforming and the like, and the treatment process needs to be carried out in a high-temperature or high-pressure environment. However, the bio-oil has poor thermal stability, is easily coked by heating to form carbon deposition, causes reactor blockage or catalyst inactivation and has long reaction residence time, reduces the upgrading efficiency, and even causes difficult reaction. In addition, the researchers propose that the bio-oil is upgraded by adopting a low-temperature electrolytic cell, the low-temperature electrolytic cell is used for upgrading the liquid bio-oil at the working temperature lower than 100 ℃, and the problems of high energy consumption, incapability of continuous treatment, electrode corrosion and the like exist.
The patent application with publication number CN 104560102A discloses a method for improving quality of bio-oil, which comprises adding bio-oil generated by cracking into a high-pressure kettle, adding calcium oxide, reacting at 30-80 deg.C for 1-4 hr under nitrogen protection, heating to 160-180 deg.C for 0.5-2 hr, cooling to 80-120 deg.C, and keeping the temperatureReacting for 0.5-2 hours to obtain C 7 -C 15 A paraffin-like fuel precursor. The method can well reduce the acid content in the biological oil and improve the pH value and stability of the biological oil. However, the method mainly aims at the quality improvement of acid substances in the bio-oil, has no obvious quality improvement effect on other components in the bio-oil, does not improve the problems of high oxygen content, low heat value and the like of the bio-oil, has limited quality improvement effect, can not realize the continuous treatment of the bio-oil, and has no wide application value.
The patent application with publication number CN 102851062A discloses a process for catalytic hydrogenation of bio-oil promoted by organic solvent, which comprises placing a certain amount of organic solvent and catalyst into a continuous reactor, replacing air in the reaction system with hydrogen, stirring under 10-12MPa hydrogen pressure, heating to 280-320 deg.C, reacting for 2-4h, and supplementing new hydrogen with hydrogen-oil ratio of 1000-2000 during the reaction process. The method promotes the catalytic hydrogenation reaction of the bio-oil through the organic solvent, and solves the problem that the bio-oil is easy to polymerize and coke in the catalytic hydrogenation process. However, the method adopts hydrogen as a hydrogen atom source, has high cost, low hydrogen atom utilization rate and poor economy, and simultaneously, the reaction is carried out under high pressure, so that the requirement on the performance of equipment is high, the operation cost is increased, and the wide industrial application is greatly limited.
Patent applications with publication numbers CN 111909736A and CN 113717746A respectively disclose a bio-oil electrochemical upgrading method and a bio-oil hydrodeoxygenation method, wherein the two methods both use an H-type electrolytic tank to carry out bio-oil electrochemical upgrading, the former uses mixed liquid of bio-oil, an organic solvent and a supporting electrolyte as catholyte, an acid solution as anolyte, the anolyte and the catholyte are separated by an ion exchange membrane and react for 2-8H under the current of 50-200mA to realize the electrochemical upgrading of bio-oil; the latter uses platinum net as anode, carbon paper as cathode and carries Pt/CeO 2 a/C catalyst. The two methods can reduce the content of biological oleic acid, aromatic components and heavy components, and simultaneously avoid the generation of carbon deposition in the quality improvement process. But will cause the corrosion of the electrode due to the acidity and corrosiveness of the bio-oil, and in addition, the low-temperature electrolysisThe working temperature of the pool is lower than 100 ℃, the quality improvement can only be carried out on the liquid bio-oil, the on-line continuous quality improvement can not be realized, the energy consumption is high, and the industrial application value is greatly limited.
Accordingly, there is a need for an upgrading process for upgrading bio-oil in biomass pyrolysis steam.
Disclosure of Invention
The application provides a biomass pyrolysis steam intermediate-temperature electrochemical quality-improving process, which aims to provide a mode of direct electrochemical hydrogenation without condensation for improving the quality of biomass pyrolysis steam, so that the number of unsaturated bonds of the biomass pyrolysis steam is reduced, the acidity and viscosity of biomass oil are reduced, the heat value and stability of the biomass oil are improved, the bio-oil is suitable for transportation and storage, and carbon deposition, high energy consumption and electrode corrosion are avoided in the quality-improving process.
The technical purpose of the application is realized by the following technical scheme:
a biomass pyrolysis steam moderate-temperature electrochemical quality improvement process is realized through an electrolytic cell reactor, the electrolytic cell reactor comprises a spiral feeder, a biomass fast pyrolysis furnace, a cyclone separator and a proton ceramic exchange membrane electrolytic cell which are sequentially connected, and a carbon bin is arranged at the bottom of the cyclone separator; the proton ceramic exchange membrane electrolytic cell maintains the temperature through an electric heating furnace, the proton ceramic exchange membrane electrolytic cell is of a symmetrical double electrolytic cell structure, each single electrolytic cell is of a sandwich structure supported by an anode, the double electrolytic cell structure sequentially comprises a proton ceramic exchange membrane electrolytic cell anode, an electrolyte, a proton ceramic exchange membrane electrolytic cell cathode, a cathode channel, a proton ceramic exchange membrane electrolytic cell cathode, an electrolyte and a proton ceramic exchange membrane electrolytic cell anode from top to bottom, the proton ceramic exchange membrane electrolytic cell anode is connected with a steam generator, and the quality improvement process comprises the following steps:
s1: continuously feeding biomass raw materials into a biomass fast pyrolysis furnace (2) through a screw feeder (1) for fast pyrolysis;
s2: introducing a product subjected to rapid pyrolysis in the biomass rapid pyrolysis furnace (2) into a cyclone separator (3) for gas-solid product separation to obtain pyrolytic carbon and pyrolytic steam, wherein the pyrolytic carbon falls into a carbon bin (4), the pyrolytic steam is directly introduced into a cathode channel between cathodes (9) of the proton ceramic exchange membrane electrolytic cell without cooling, and water vapor generated by a steam generator (6) is introduced into an anode (7) of the proton ceramic exchange membrane electrolytic cell;
s3: the proton ceramic exchange membrane electrolytic cell (8) is externally connected with a direct current power supply to carry out electrochemical reaction at the working temperature of 400-600 ℃, so as to carry out warm electrochemical upgrading on the pyrolysis steam.
The beneficial effect of this application lies in:
(1) Compared with the existing bio-oil upgrading technology, the biomass pyrolysis steam is the target, the bio-oil does not need to be condensed in advance, and the process is simple.
(2) The temperature of the biomass fast pyrolysis steam is matched with the working temperature of the proton ceramic exchange membrane electrolytic cell and is about 400-600 ℃, the biomass fast pyrolysis steam can provide heat for the proton ceramic exchange membrane electrolytic cell, and the energy utilization rate is improved.
(3) The bio-oil component in the biomass fast pyrolysis steam at the cathode of the proton ceramic exchange membrane electrolytic cell directly reacts with hydrogen protons, and the hydrogen protons are derived from water, so that compared with other bio-oil quality extraction technologies, the biomass fast pyrolysis steam hydrogen production system has high safety, low cost and high hydrogen atom utilization rate.
(4) Biological oil is easy to generate oxidation reaction at an anode in the electrochemical treatment process to polymerize, so that carbon is deposited on the surface of an electrode. The proton ceramic exchange membrane is adopted, so that the biomass fast pyrolysis steam is ensured to participate in the reaction only at one side of the cathode, and the biological oil is prevented from being polymerized and deposited at the anode.
(5) Compared with the technology for electrochemically upgrading the bio-oil by using the low-temperature electrolytic cell, the proton ceramic exchange membrane electrolytic cell has higher working temperature, on one hand, the electrolysis of the water vapor absorbs more and more heat along with the rise of the temperature, the Joule heat of the electrolytic cell is utilized in the process of electrolyzing the water vapor, on the other hand, the free energy change in the water vapor electrolysis reaction is reduced along with the rise of the temperature, so that the power loss caused by the overvoltage of the electrode can be reduced, and the two opposite sides can reduce the electrolysis power consumption. Furthermore, the electrodes of low-temperature electrolyzers present corrosion problems, whereas high-temperature electrolyzers based on ceramic solid oxide materials hardly corrode.
(6) All components of the bio-oil in the biomass fast pyrolysis steam are upgraded, unsaturated bonds in the bio-oil are hydrogenated and converted into saturated bonds, the number of the unsaturated bonds in the bio-oil can be reduced, the acidity and viscosity of the biomass oil are reduced, the heat value and stability of the bio-oil are improved, and the bio-oil is suitable for transportation and storage.
Drawings
FIG. 1 is a schematic diagram of the structure of an electrolytic cell reactor as described herein.
Detailed Description
The technical solution of the present application will be described in detail below with reference to the accompanying drawings.
The biomass pyrolysis steam moderate-temperature electrochemical upgrading process is realized through an electrolytic cell reactor. As shown in fig. 1, the electrolytic cell reactor comprises a spiral feeder, a biomass fast pyrolysis furnace, a cyclone separator and a proton ceramic exchange membrane electrolytic cell which are connected in sequence, wherein a carbon bin is arranged at the bottom of the cyclone separator; the proton ceramic exchange membrane electrolytic cell maintains the temperature through the electric heating furnace, the proton ceramic exchange membrane electrolytic cell is of a symmetrical double-electrolytic-cell structure, each single electrolytic cell is of a sandwich structure supported by an anode, the double-electrolytic-cell structure sequentially comprises a proton ceramic exchange membrane electrolytic cell anode, an electrolyte, a proton ceramic exchange membrane electrolytic cell cathode, a cathode channel, a proton ceramic exchange membrane electrolytic cell cathode, an electrolyte and a proton ceramic exchange membrane electrolytic cell anode from top to bottom, and the proton ceramic exchange membrane electrolytic cell anode is connected with the steam generator.
The biomass pyrolysis steam moderate-temperature electrochemical upgrading process specifically comprises the following steps:
s1: the biomass raw material is continuously put into a biomass fast pyrolysis furnace 2 through a spiral feeder 1 for fast pyrolysis.
Specifically, the pyrolysis temperature of the biomass fast pyrolysis furnace is 400-600 ℃. The biomass raw materials comprise wood processing residues, forestry felling residues and crop straw agricultural biomass.
S2: and introducing the product subjected to the rapid pyrolysis of the biomass rapid pyrolysis furnace 2 into the cyclone separator 3 to perform gas-solid product separation to obtain pyrolytic carbon and pyrolytic steam, wherein the pyrolytic carbon falls into the carbon bin 4, the pyrolytic steam is directly introduced into a cathode channel between cathodes 9 of the proton ceramic exchange membrane electrolytic cell without being cooled, and the water vapor generated by the steam generator 6 is introduced into an anode 7 of the proton ceramic exchange membrane electrolytic cell.
Specifically, the cathode of the proton ceramic exchange membrane electrolytic cell is a mixture of Ni and BCY in any proportion or a mixture of Pt or BSCF and BCZY in any proportion; wherein, the BCY is BaCe x Y 1-x O 3-δ BSCF is Ba x Sr 1-x Co y Fe 1-y O 3-δ BCZY is BaCe x Zr y Y 1-x-y O 3-δ 。
The anode of the proton ceramic exchange membrane electrolytic cell is LSM or a mixture of NiO and BZY in any proportion or a mixture of NiO and BCZY in any proportion, wherein the LSM is La x Sr 1-x MnO 3-δ BZY is BaZr x Y 1-x O 3-δ The anode of the proton ceramic exchange membrane electrolytic cell is prepared by a tabletting method and a sintering method.
The proton ceramic exchange membrane in the proton ceramic exchange membrane electrolytic cell is BCY or BZY or BCZY.
The sandwich structure is prepared by a screen printing method and a calcining method.
The proton ceramic exchange membrane electrolytic cell is maintained at 400-600 ℃ by an electric heating furnace.
S3: the proton ceramic exchange membrane electrolytic cell 8 is externally connected with a direct current power supply to carry out electrochemical reaction at the working temperature of 400-600 ℃, thereby carrying out the temperature electrochemical upgrading on the pyrolysis steam.
Specifically, the direct-current power supply voltage is 1-2V.
The experimental effect of the application is mainly evaluated by the quality of the upgraded pyrolysis steam condensed bio-oil product.
TABLE 1 oil properties of Pinus sylvestris
The following are specific examples:
the first embodiment is as follows:
the embodiment specifically comprises the following steps:
s1: continuously putting biomass raw material pinus sylvestris wood chips into a biomass fast pyrolysis furnace through a spiral feeder, raising the temperature to 550 ℃ at the temperature rise rate of more than 10000 ℃/s, and staying for 1s to finish fast pyrolysis, wherein the physical parameters of the bio-oil in the fast pyrolysis steam are shown in table 1.
S2: mixing Ni powder and BCY powder according to the mass ratio of 6 and preparing a porous Ni-BCY anode substrate by using a tabletting and calcining method, depositing a BCY electrolyte layer on the anode substrate by a screen printing and calcining method, and preparing an LSM cathode layer on the surface of the electrolyte by the screen printing and calcining method.
S3: the fast pyrolysis steam is directly introduced into a cathode of a proton ceramic exchange membrane electrolytic cell without being cooled, water vapor generated by a steam generator is introduced into an anode of the proton ceramic exchange membrane electrolytic cell, the proton ceramic exchange membrane electrolytic cell works under the conditions that the temperature is 600 ℃ and the voltage of an external direct-current power supply is 1.5V, therefore, the biomass pyrolysis steam upgrading can be realized, and the physical property parameters of the bio-oil of the upgraded pyrolysis steam are shown in Table 2.
TABLE 2 physical Properties of upgraded Bio-oil
Example two:
the embodiment specifically comprises the following steps:
s1: continuously feeding biomass raw material pinus sylvestris wood chips into a biomass fast pyrolysis furnace through a spiral feeder, heating to 550 ℃ at a heating rate of more than 10000 ℃/s, and staying for 1s to complete fast pyrolysis, wherein physical parameters of bio-oil in fast pyrolysis steam are shown in table 1.
S2: mixing NiO powder and BZY powder in a mass ratio of 6 and preparing a porous Ni-BCY anode substrate by using a tabletting and calcining method, depositing a BZY electrolyte layer on the anode substrate by a screen printing and calcining method, and preparing a Pt cathode layer on the surface of the electrolyte by the screen printing and calcining method.
S3: the fast pyrolysis steam is directly introduced into a cathode of a proton ceramic exchange membrane electrolytic cell without being cooled, water vapor generated by a steam generator is introduced into an anode of the proton ceramic exchange membrane electrolytic cell, the proton ceramic exchange membrane electrolytic cell works under the conditions that the temperature is 600 ℃ and the voltage of an external direct current power supply is 1.5V, therefore, the quality improvement of the biomass pyrolysis steam can be realized, and the physical property parameters of the bio-oil in the upgraded pyrolysis steam are shown in table 3.
TABLE 3 upgrading bio-oil physical parameters
Example three:
the embodiment specifically comprises the following steps:
s1: continuously putting biomass raw material pinus sylvestris wood chips into a biomass fast pyrolysis furnace through a spiral feeder, raising the temperature to 550 ℃ at the temperature rise rate of more than 10000 ℃/s, and staying for 1s to finish fast pyrolysis, wherein the physical parameters of the bio-oil in the fast pyrolysis steam are shown in table 1.
S2: mixing NiO powder and BCZY powder in a mass ratio of 6 and preparing a porous Ni-BCZY anode substrate by using a tabletting and calcining method, depositing a BCZY electrolyte layer on the anode substrate by a screen printing and calcining method, and preparing a BSCF-BCZY cathode layer on the surface of the electrolyte by a screen printing and calcining method.
S3: the fast pyrolysis steam is directly introduced into a cathode of a proton ceramic exchange membrane electrolytic cell without being cooled, water vapor generated by a steam generator is introduced into an anode of the proton ceramic exchange membrane electrolytic cell, the proton ceramic exchange membrane electrolytic cell works under the conditions that the temperature is 600 ℃ and the current of an external direct current power supply is 1.5V, so that the biomass pyrolysis steam upgrading can be realized, and the physical property parameters of the bio-oil in the upgraded pyrolysis steam are shown in Table 2
TABLE 4. Upgrading of Bio-oil physical parameters
The foregoing shows and describes the general principles and features of the present invention, together with the advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are given by way of illustration of the principles of the present invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, and such changes and modifications are within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. A biomass pyrolysis steam moderate-temperature electrochemical quality improvement process is realized through an electrolytic cell reactor, the electrolytic cell reactor comprises a spiral feeder, a biomass fast pyrolysis furnace, a cyclone separator and a proton ceramic exchange membrane electrolytic cell which are sequentially connected, and a carbon bin is arranged at the bottom of the cyclone separator; the proton ceramic exchange membrane electrolytic cell maintains the temperature through an electric heating furnace, the proton ceramic exchange membrane electrolytic cell is of a symmetrical double electrolytic cell structure, each single electrolytic cell is of a sandwich structure supported by an anode, and the double electrolytic cell structure sequentially comprises a proton ceramic exchange membrane electrolytic cell anode, an electrolyte, a proton ceramic exchange membrane electrolytic cell cathode, a cathode channel, a proton ceramic exchange membrane electrolytic cell cathode, an electrolyte and a proton ceramic exchange membrane electrolytic cell anode from top to bottom, wherein the proton ceramic exchange membrane electrolytic cell anode is connected with a steam generator, and the quality improvement process is characterized by comprising the following steps of:
s1: continuously feeding biomass raw materials into a biomass fast pyrolysis furnace (2) through a spiral feeder (1) for fast pyrolysis;
s2: introducing a product subjected to rapid pyrolysis in the biomass rapid pyrolysis furnace (2) into a cyclone separator (3) for gas-solid product separation to obtain pyrolytic carbon and pyrolytic steam, wherein the pyrolytic carbon falls into a carbon bin (4), the pyrolytic steam is directly introduced into a cathode channel between cathodes (9) of the proton ceramic exchange membrane electrolytic cell without cooling, and water vapor generated by a steam generator (6) is introduced into an anode (7) of the proton ceramic exchange membrane electrolytic cell;
s3: the proton ceramic exchange membrane electrolytic cell (8) is externally connected with a direct current power supply to carry out electrochemical reaction at the working temperature of 400-600 ℃, thereby carrying out warm electrochemical upgrading on the pyrolysis steam.
2. The upgrading process according to claim 1, wherein in step S1, the pyrolysis temperature of the biomass fast pyrolysis furnace (2) is 400-600 ℃.
3. The upgrading process of claim 1, wherein in step S1, the biomass feedstock comprises wood processing residues, forestry felling residues, and crop straw agricultural biomass.
4. The upgrading process according to claim 1, wherein the proton ceramic exchange membrane cell cathode is a mixture of Ni and BCY in any ratio or Pt or a mixture of BSCF and BCZY in any ratio; wherein, the BCY is BaCe x Y 1- x O 3-δ BSCF is Ba x Sr 1-x Co y Fe 1-y O 3-δ BCZY is BaCe x Zr y Y 1-x-y O 3-δ 。
5. The upgrading process of claim 1, wherein the proton ceramic exchange membrane electrolytic cell anode is LSM, or any ratio mixture of NiO and BZY, or any ratio mixture of NiO and BCZY, and the LSM is La x Sr 1-x MnO 3-δ BZY is BaZr x Y 1-x O 3-δ The anode of the proton ceramic exchange membrane electrolytic cell is prepared by a tabletting method and a sintering method.
6. The upgrading process of claim 1, wherein the proton ceramic exchange membrane in the proton ceramic exchange membrane electrolytic cell is BCY or BZY or BCZY.
7. The upgrading process of claim 1, wherein the sandwich structure is prepared by screen printing and firing.
8. The upgrading process of claim 1, wherein the proton ceramic exchange membrane electrolytic cell is maintained at a temperature of 400-600 ℃ by an electric heating furnace.
9. The upgrading process according to claim 1, wherein the dc supply voltage is 1-2V.
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