CN119463904A - A biomass viscosity-enhancing modification and tar hydrogenation utilization process - Google Patents
A biomass viscosity-enhancing modification and tar hydrogenation utilization process Download PDFInfo
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Abstract
The invention belongs to the technical field of biomass utilization, and particularly relates to a biomass tackifying modification and tar hydrogenation utilization process thereof, which comprises the following steps: selecting biomass, crushing and screening to prepare a framework material and a carbon main material, pyrolyzing, hydrogenating, desulfurizing and deoxidizing the obtained solid, mixing the obtained solid to prepare a binder, and preparing the carbon by the binder. According to the invention, hydrogen is not used as a raw material, and the supercritical/subcritical system is utilized to carry out hydrolysis transformation on biomass so that the biomass has a tackifier function and participates in subsequent biomass type carbon preparation. The hydrogenation tackifying of waste biomass solids and the hydrodeoxygenation desulfurization process of biomass tar are realized, and the green low-carbon cyclic development of biomass is realized.
Description
Technical Field
The invention belongs to the technical field of biomass utilization, and particularly relates to a biomass tackifying modification and tar hydrogenation utilization process thereof.
Background
The annual yield of the straw in rural areas in China exceeds 7 hundred million tons, the storage and transportation cost is high in the recycling process, the added value of the product is low, and the industrialization process is severely restricted. The waste residues of Chinese medicinal materials belong to high-humidity solid waste materials, the water content is more than 80%, and the waste residues are unfavorable for storage or reprocessing. Biomass represented by straw and Chinese medicinal residues is a high-water-content organic matter, and the biomass oil can be obtained through dehydration and pyrolysis. The biomass oil produced in the biomass pyrolysis process has higher oxygen content, and partial oxygen needs to be removed to convert the biomass oil into high-quality oil, but the biomass oil needs to be subjected to complicated and severe hydrodeoxygenation treatment to produce second-generation alkane biofuel, and the production cost is too high.
The bio-oil contains a large amount of oxygen-containing functional groups such as carbonyl groups, carboxyl groups and the like, and the oxygen-containing functional groups are root causes of high acidity, poor stability and low heat value of the bio-oil. The hydrodeoxygenation can effectively remove oxygen-containing groups in the biological oil, reduce the oxygen content and improve the quality of the biological oil. When the biomass oil is used for preparing the high-grade fuel, the oil hydrogenation process generally comprises the following two steps of converting unsaturated fatty acid and triglyceride into saturated fatty acid through catalytic hydrogenation, converting the saturated fatty acid into straight-chain alkane through hydrodeoxygenation, removing oxygen atoms in the form of H 2 O or carbon oxides, and carrying out hydrocracking and hydroisomerization on the straight-chain alkane obtained in the first step under the action of a catalyst to generate isoparaffin, thereby achieving the purposes of reducing a freezing point, improving low-temperature fluidity and the like, and improving the quality of the oil product.
The traditional biomass catalytic pyrolysis experiment is generally carried out by adopting a fixed bed reactor or a fluidized bed under the flow of nitrogen, and the catalyst comprises HZSM-5, ZSM-5, A1-SBA-15 and the like, when the HZSM-5 or HZSM-5/AL2O3 is adopted as the catalyst, the catalytic pyrolysis can lead the aromatic hydrocarbon content in the biological oil to be higher, and the catalyst has better deoxidization effect and is the most main method for the hydrogenation modification of the biomass oil. The reaction temperature of catalytic hydrogenation of bio-oil mainly comprising pyrolysis tar is usually 400 ℃ or less, and the bio-oil is hydrogenation reaction under the action of catalyst in the atmosphere of hydrogen or hydrogen-supplying solvent under high pressure, and the bio-oil quality improvement technology for removing original oxygen element in the form of water or carbon oxide is also usually accompanied by chemical reactions such as hydrodesulfurization, hydrodenitrogenation, and hydrogenation saturation of unsaturated hydrocarbon.
The research shows that water is an excellent solvent for hydrocarbon near the critical point (340 ℃ and 22.1 MPa) or in the supercritical state, has very high solubility, is beneficial to the dissolution of small molecular components in biomass, and provides a suitable reaction environment for the hydrogenation of biomass oil. By utilizing the characteristic of high water content of biomass, water is used as a raw material, and hydrogen (active hydrogen, not hydrogen) generated by water-CO supercritical reaction under the condition of CO atmosphere has higher activity, so that certain bonds of oxygen-containing functional groups in biomass oil are easily broken by hydrogenolysis to generate small molecular compounds. Meanwhile, the water-CO supercritical system can consume water generated by biomass, and reduce the water discharge.
Patent CN200710017449.9 proposes a method for hydrotreating coal tar by using supercritical solvent, adding coal tar raw material into a reactor, adding solvent A and catalyst B, in which the volume ratio of solvent A to coal tar raw material is 1:1-1:3 and 1wt% -18wt% of coal tar raw material, making light reaction under the condition of hydrogen gas, and making the liquid product discharged from the reactor undergo the process of distillation and cutting to obtain water, solvent, heavy oil and light oil fraction.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a biomass tackifying modification and tar hydrogenation utilization process, solves the problems of insufficient biomass carbon cohesiveness, biomass water utilization and biomass tar deoxidation hydrogenation process, and provides a biomass tackifying modification and tar hydrogenation utilization process.
The technical scheme adopted by the invention is as follows:
a biomass tackifying modification and tar hydrogenation utilization process comprises the following steps:
firstly, selecting a certain mass part of biomass, crushing and screening the biomass to obtain a solid mixture A;
dividing the solid mixture A obtained in the first step into three parts according to the proportion, carrying out hydrolysis and fermentation treatment on the first part of solid mixture A for a certain time, and filtering to obtain a solid mixture B and a liquid C;
Thirdly, heating the second part of solid mixture A prepared in the second step to 650 ℃ for pyrolysis, and collecting the solid mixture D, tar E and pyrolysis gas F after pyrolysis is completed;
Fourthly, mixing the solid mixture D obtained in the second step and the solid mixture D obtained in the third step with the tar E obtained in the third step, and then placing the mixture into a CO-water critical reactor to complete CO-water supercritical hydrogenation reaction of the tar, and finally obtaining a hydrogenated biomass solid part G and tar H for completing hydrodeoxygenation and desulfurization processes;
Fifthly, uniformly mixing the solid mixture B obtained in the second step with the biomass solid part G obtained in the fourth step to serve as a binder J;
step six, uniformly mixing the third solid mixture A prepared in the step two with the binder J prepared in the step five according to a certain proportion, completing hot melting and pressurizing forming, extruding residual tar H under a certain pressure, and simultaneously obtaining biomass carbon K;
And seventh, heating the biomass carbon J to 650 ℃ at a certain heating rate, and collecting biomass carbon K, tar L and pyrolysis gas M after pyrolysis is completed.
Further, the biomass in the first step comprises any one or any combination of two of straw and Chinese medicinal residues in any proportion, the moisture of the solid mixture A exceeds 20wt%, the mass fraction is 100, and the granularity of the crushed and sieved solid mixture A is 1-20mm.
Further, in the second step, the solid mixture A is divided into three parts according to the mass ratio of the first part to the second part of 0.2:0.2-0.4:0.6-0.4, the first part of the solid mixture A is used for manufacturing a framework material of a biomass formed coke binder, the second part of the solid mixture A is used for dehydrating to obtain a water source of a subsequent CO-water supercritical process, the third part of the solid mixture A is used for preparing a main material of formed carbon, the hydrolysis process in the second step is to add KOH hydrolytic agent and ammonia water, the first part of the solid mixture A is mixed with KOH, ammonia water and water according to the mass ratio of 1:0.1-0.3:0.05-0.1:1-10, and the hydrolysis and fermentation processes are carried out for 3-10 days after the solid mixture is uniformly mixed.
Further, the heating rate of pyrolysis in the third step is 3-5 ℃ per min, and the residence time after the temperature is raised to 650 ℃ is 1-3h.
Further, in the fourth step, the mass ratio of the liquid C, the solid mixture D and the tar E is 5:1:1-5.
Further, in the seventh step, the tar L can be used as the tar E in the fourth step to enter CO-water supercritical hydrogenation reaction, and finally the tar H in the hydrodeoxygenation and desulfurization processes is collected.
Further, the CO-water supercritical hydrogenation reaction in the fourth step is carried out by introducing CO gas at the initial stage under normal temperature anaerobic condition to enable the pressure in the reactor to reach 5MPa, introducing CO and adjusting the pressure to 5-10MPa when heating is started, supplementing CO before 250 ℃, keeping the space velocity of CO at 10-500h -1, heating the CO-water supercritical reactor at the heating rate of 3-5 ℃ per minute, finally heating to reach the 340+/-10 ℃ critical temperature of the CO-water system, and staying for 1-5h under the critical temperature and the critical pressure of 10-20 MPa.
Further, the mixing ratio of the solid mixture B to the biomass solid part G in the fifth step is 1:1-2.
Further, in the sixth step, the mixing ratio of the solid mixture A to the binder J is 1:5-10, and the hot melting and pressurizing molding is carried out, wherein the extrusion pressure of 100-1000KN mainly extrudes the tar H liquid part, and simultaneously, the biomass forms blocky carbon.
Further, in the seventh pyrolysis step, the tar L comprises tar E remained in the solid part G in the fifth step, the pyrolysis heating rate is 3-5 ℃ per minute, and the residence time is 1-3h after the temperature is raised to 650 ℃.
The beneficial effects of the invention are as follows:
The invention does not use hydrogen as raw material, but utilizes active hydrogen generated by CO and water reaction to complete the hydrogenation process of supercritical/subcritical biomass and biomass tar at 340 ℃.
In the process of preparing clean carbon from biomass, the binder is needed to participate, and the supercritical/subcritical system is utilized to hydrolyze and reform biomass so that the biomass has a tackifier function and participates in subsequent biomass carbon preparation. Biomass oil is prepared by pyrolyzing biomass such as straw, chinese medicinal residues and the like, the biomass oil is subjected to a deoxidization and hydrogenation process, oxygen-containing functional groups are reduced, and partial sulfur compounds are removed by hydrogenation. The strength of the obtained biomass charcoal is required to be more than 550N/piece, and the porosity is more than or equal to 20%. The processes of biomass oil and clean carbon are prepared by biomass pyrolysis of straws, chinese medicinal residues and the like, so that the processes of hydrogenation tackifying of waste biomass solids and hydrodeoxygenation and desulfurization of biomass tar are realized, and the green low-carbon cyclic development of biomass is realized.
Detailed Description
Example 1
Firstly, selecting biomass containing any one or combination of two of straw and Chinese medicinal residues in any proportion, crushing and screening to obtain a crushed and screened solid mixture A with the granularity of 1-10mm, wherein the moisture content of the solid mixture A exceeds 20wt% and the mass fraction is 100.
And secondly, dividing the solid mixture A obtained in the first step into three parts according to the mass ratio of 0.2:0.2:0.6. The first part of solid mixture A is used for manufacturing framework materials of the biomass formed coke binder. The hydrolysis process comprises the steps of adding a KOH hydrolysis agent and ammonia water, mixing a first part of solid mixture A with KOH, ammonia water and water according to a mass ratio of 1:0.1:0.05:5, carrying out hydrolysis and fermentation for 3 days after uniformly mixing, filtering to obtain a solid mixture B and a liquid C, dehydrating a second part of the solid mixture A to obtain a water source for a subsequent CO-water supercritical process, and preparing a third part of the solid mixture A as a main material for preparing carbon.
And thirdly, heating the second part of solid mixture A prepared in the second step to 650 ℃ at a heating rate of 3 ℃ per minute for pyrolysis, heating to 650 ℃ for final temperature, and then keeping for 3 hours, and collecting the solid mixture D, tar E and pyrolysis gas F after pyrolysis is completed.
And fourthly, mixing the solid mixture D obtained in the second step and the solid mixture D obtained in the third step with the tar E obtained in the third step, and then placing the mixture into a CO-water critical reactor, wherein the mass ratio of the liquid C to the solid mixture D to the tar E is 5:1:1, so as to complete the CO-water supercritical hydrogenation reaction of the tar. The CO-water supercritical hydrogenation reaction process includes introducing CO gas at normal temperature and in the initial stage under anaerobic condition to reach pressure of 5MPa. When heating is started, CO gas is introduced and the pressure is regulated to 5MPa, CO is supplemented before 250 ℃, the space velocity of CO is 500H -1, a CO-water critical reactor heats at the temperature rising rate of 3 ℃ per minute, the temperature is finally raised to reach the 340 ℃ critical temperature of a CO-water system, the tar L stays for 1 to H time under the critical temperature and the critical pressure of 20MPa, and in the seventh step, the tar L can be used as the tar E in the fourth step to enter CO-water supercritical hydrogenation reaction, and finally the hydrogenated biomass solid part G and the tar H which completes the hydrodeoxygenation and desulfurization process are obtained.
And fifthly, uniformly mixing the solid mixture B obtained in the second step with the biomass solid part G obtained in the fourth step according to the ratio of 1:1 to serve as a binder J.
And sixthly, uniformly mixing the third solid mixture A prepared in the second step with the binder J prepared in the fifth step according to the ratio of 1:5, finishing hot melting and pressurizing to form, extruding residual tar H at the extrusion pressure of 1000KN, and simultaneously obtaining biomass massive carbon K.
And seventh, heating the biomass type carbon J to 650 ℃ at a heating rate of 3 ℃ per minute, staying for 1-3 hours, and collecting the biomass type carbon K, tar L and pyrolysis gas M after pyrolysis is completed. Wherein tar L comprises tar E remaining in solid fraction G in the fifth step.
Example 2
Firstly, selecting biomass containing any one or combination of two of straw and Chinese medicinal residues in any proportion, crushing and screening to obtain a crushed and screened solid mixture A with the granularity of 10-20mm, wherein the moisture content of the solid mixture A exceeds 20wt% and the mass fraction of the solid mixture A is 100 parts.
And secondly, dividing the solid mixture A obtained in the first step into three parts according to the mass ratio of 0.2:0.4:0.4. The first part of solid mixture A is used for manufacturing framework materials of the biomass formed coke binder. The hydrolysis process comprises the steps of adding a KOH hydrolysis agent and ammonia water, mixing a first part of solid mixture A with KOH, ammonia water and water according to a mass ratio of 1:0.3:0.1:10, carrying out hydrolysis and fermentation for 3-10 days after uniformly mixing, filtering to obtain a solid mixture B and a liquid C, dehydrating a second part of the solid mixture A to obtain a water source for a subsequent CO-water supercritical process, and preparing a third part of the solid mixture A as a main material for preparing carbon.
And thirdly, heating the second part of solid mixture A prepared in the second step to 650 ℃ at a heating rate of 5 ℃ per min for pyrolysis, heating to 650 ℃ for final temperature, and then keeping for 3 hours, and collecting the solid mixture D, tar E and pyrolysis gas F after pyrolysis is completed.
And fourthly, mixing the solid mixture D obtained in the second step and the solid mixture D obtained in the third step with the tar E obtained in the third step, and then placing the mixture into a CO-water critical reactor, wherein the mass ratio of the liquid C to the solid mixture D to the tar E is 5:1:3, so as to complete the CO-water supercritical hydrogenation reaction of the tar. The CO-water supercritical hydrogenation reaction process includes introducing CO gas at normal temperature and in the initial stage under anaerobic condition to reach pressure of 5MPa. When heating is started, CO is introduced and the pressure is regulated to 5-10MPa, CO is supplemented before 250 ℃, the airspeed of CO is 10-500H -1, the CO-water critical reactor heats at the heating rate of 3-5 ℃ per minute, the temperature is finally raised to reach the critical temperature of 340+/-10 ℃ of the CO-water system, and the tar L stays for 5H under the critical temperature and the critical pressure of 20MPa, and in the seventh step, the tar L can be used as the tar E in the fourth step to enter CO-water supercritical hydrogenation reaction, and finally the hydrogenated biomass solid part G and the tar H which completes the hydrodeoxygenation and desulfurization process are obtained.
And fifthly, uniformly mixing the solid mixture B obtained in the second step with the biomass solid part G obtained in the fourth step according to the ratio of 1:1.5 to obtain a binder J.
And step six, uniformly mixing the third solid mixture A prepared in the step two with the binder J prepared in the step five according to the proportion of 1:10, completing hot melting and pressurizing forming, extruding residual tar H at the extruding pressure of 500KN, and simultaneously obtaining biomass massive carbon K.
And seventh, heating the biomass type carbon J to 650 ℃ at a heating rate of 3-5 ℃ per minute, staying for 1h, and collecting the biomass type carbon K, tar L and pyrolysis gas M after pyrolysis is completed. Wherein tar L comprises tar E remaining in solid fraction G in the fifth step.
Example 3
Firstly, selecting biomass containing any one or combination of two of straw and Chinese medicinal residues in any proportion, crushing and screening to obtain a crushed and screened solid mixture A with the granularity of 10-20mm, wherein the moisture content of the solid mixture A exceeds 20wt% and the mass fraction of the solid mixture A is 100 parts.
And secondly, dividing the solid mixture A obtained in the first step into three parts according to the mass ratio of 0.2:0.3:0.5. The first part of solid mixture A is used for manufacturing framework materials of the biomass formed coke binder. The hydrolysis process comprises the steps of adding a KOH hydrolysis agent and ammonia water, mixing a first part of solid mixture A with KOH, ammonia water and water according to a mass ratio of 1:0.2:0.075:1, carrying out hydrolysis and fermentation for 3-10 days after uniform mixing, filtering to obtain a solid mixture B and a liquid C, dehydrating a second part of the solid mixture A to obtain a water source of a subsequent CO-water supercritical process, and preparing a third part of the solid mixture A as a main material for preparing carbon.
And thirdly, heating the second part of solid mixture A prepared in the second step to 650 ℃ at a heating rate of 3-5 ℃ per minute for pyrolysis, heating to 650 ℃ for final temperature, and then keeping for 1-3 hours, and collecting the solid mixture D, tar E and pyrolysis gas F after pyrolysis.
And fourthly, mixing the solid mixture D obtained in the second step and the solid mixture D obtained in the third step with the tar E obtained in the third step, and then placing the mixture into a CO-water critical reactor, wherein the mass ratio of the liquid C to the solid mixture D to the tar E is 5:1:4, so as to complete the CO-water supercritical hydrogenation reaction of the tar. The CO-water supercritical hydrogenation reaction process includes introducing CO gas at normal temperature and in the initial stage under anaerobic condition to reach pressure of 5MPa. When heating is started, CO is introduced and the pressure is regulated to 7.5 MPa, CO is supplemented before 250 ℃, the space velocity of CO is 10H -1, the CO-water critical reactor heats at the temperature rising rate of 4 ℃ per min, the temperature is finally raised to reach the critical temperature of 340+/-10 ℃ of the CO-water system, and the tar L stays for 3H under the critical temperature and the critical pressure of 15MPa, and in the seventh step, the tar L can be used as the tar E in the fourth step to enter CO-water supercritical hydrogenation reaction, and finally the hydrogenated biomass solid part G and the tar H which completes the hydrodeoxygenation and desulfurization process are obtained.
And fifthly, uniformly mixing the solid mixture B obtained in the second step with the biomass solid part G obtained in the fourth step according to the ratio of 1:2, and taking the mixture as a binder J.
And sixthly, uniformly mixing the third solid mixture A prepared in the second step with the binder J prepared in the fifth step according to the proportion of 1:7.5, finishing hot melt compression molding, extruding residual tar H at the extrusion pressure of 100KN, and simultaneously obtaining biomass blocky carbon K.
And seventh, heating the biomass type carbon J to 650 ℃ at a heating rate of 4 ℃ per minute, staying for 2 hours, and collecting the biomass type carbon K, tar L and pyrolysis gas M after pyrolysis is completed. Wherein tar L comprises tar E remaining in solid fraction G in the fifth step.
Claims (10)
1. A biomass tackifying modification and tar hydrogenation utilization process is characterized by comprising the following steps:
firstly, selecting a certain mass part of biomass, crushing and screening the biomass to obtain a solid mixture A;
dividing the solid mixture A obtained in the first step into three parts according to the proportion, carrying out hydrolysis and fermentation treatment on the first part of solid mixture A for a certain time, and filtering to obtain a solid mixture B and a liquid C;
Thirdly, heating the second part of solid mixture A prepared in the second step to 650 ℃ for pyrolysis, and collecting the solid mixture D, tar E and pyrolysis gas F after pyrolysis is completed;
Fourthly, mixing the solid mixture D obtained in the second step and the solid mixture D obtained in the third step with the tar E obtained in the third step, and then placing the mixture into a CO-water critical reactor to complete CO-water supercritical hydrogenation reaction of the tar, and finally obtaining a hydrogenated biomass solid part G and tar H for completing hydrodeoxygenation and desulfurization processes;
Fifthly, uniformly mixing the solid mixture B obtained in the second step with the biomass solid part G obtained in the fourth step to serve as a binder J;
step six, uniformly mixing the third solid mixture A prepared in the step two with the binder J prepared in the step five according to a certain proportion, completing hot melting and pressurizing forming, extruding residual tar H under a certain pressure, and simultaneously obtaining biomass carbon K;
And seventh, heating the biomass carbon J to 650 ℃ at a certain heating rate, and collecting biomass carbon K, tar L and pyrolysis gas M after pyrolysis is completed.
2. The biomass tackifying modification and tar hydrogenation utilization process according to claim 1, wherein in the first step, biomass contains any one or combination of two of straw and Chinese medicine residues in any proportion, the moisture of the solid mixture A exceeds 20wt%, the mass fraction is 100, and the granularity of the crushed and sieved solid mixture A is 1-20mm.
3. The biomass tackifying modification and tar hydrogenation utilization process according to claim 1 is characterized in that in the second step, the solid mixture A is divided into three parts according to the mass ratio of 0.2:0.2-0.4:0.6-0.4, the first part of the solid mixture A is used for preparing a framework material of a biomass formed coke binder, the second part of the solid mixture A is used for dehydrating to obtain a water source of a subsequent CO-water supercritical process, the third part of the solid mixture A is used for preparing a main material of formed carbon, the hydrolysis process is to add KOH hydrolytic agent and ammonia water, the first part of the solid mixture A is mixed with KOH, ammonia water and water according to the mass ratio of 1:0.1-0.3:0.05-0.1:1-10, and hydrolysis and fermentation processes are carried out for 3-10 days after the uniform mixing.
4. The biomass tackifying modification and tar hydrogenation utilization process according to claim 1, wherein the heating rate of pyrolysis in the third step is 3-5 ℃ per minute, and the residence time after heating to 650 ℃ is 1-3h.
5. The biomass tackifying modification and tar hydrogenation process according to claim 1, wherein the mass ratio of the liquid C, the solid mixture D and the tar E in the fourth step is 5:1:1-5.
6. The biomass tackifying modification and tar hydrogenation utilization process according to claim 1, wherein in the seventh step, tar L can be used as tar E in the fourth step to enter CO-water supercritical hydrogenation reaction, and finally tar H in hydrodeoxygenation and desulfurization processes is collected.
7. The biomass tackifying modification and tar hydrogenation utilization process according to claim 1, wherein in the fourth step, CO gas is introduced at the initial stage of normal temperature anaerobic condition to enable the pressure in the reactor to reach 5MPa, CO is introduced and the pressure is regulated to 5-10MPa when heating is started, CO is supplemented before 250 ℃, the space velocity of CO is 10-500h -1, the CO-water critical reactor is heated at the heating rate of 3-5 ℃ per minute, the final heating reaches the 340+/-10 ℃ critical temperature of the CO-water system, and the CO stays for 1-5h under the critical temperature and the critical pressure of 10-20 MPa.
8. The biomass tackifying modification and tar hydrogenation process according to claim 1, wherein the mixing ratio of the solid mixture B and the solid biomass part G in the fifth step is 1:1-2.
9. The biomass tackifying modification and tar hydrogenation utilization process according to claim 1, wherein in the sixth step, the mixing ratio of the solid mixture A to the binder J is 1:5-10, the hot melt compression molding is carried out, and the extrusion pressure of 100-1000KN mainly extrudes the tar H liquid part, and simultaneously enables the biomass to form blocky carbon.
10. The biomass tackifying modification and tar hydrogenation utilization process according to claim 1, wherein in the seventh pyrolysis step, the tar L comprises tar E remained in the solid part G in the fifth pyrolysis step, the temperature rising rate of pyrolysis is 3-5 ℃ per minute, and the residence time after the temperature rises to 650 ℃ is 1-3h.
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| CN119463904B (en) | 2025-04-01 |
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