CN116855266A - Method for preparing high-performance biochar through pyrolysis and coupling energy recovery - Google Patents
Method for preparing high-performance biochar through pyrolysis and coupling energy recovery Download PDFInfo
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- 238000000197 pyrolysis Methods 0.000 title claims abstract description 82
- 238000000034 method Methods 0.000 title claims abstract description 40
- 238000010168 coupling process Methods 0.000 title claims abstract description 27
- 230000008878 coupling Effects 0.000 title claims abstract description 26
- 238000005859 coupling reaction Methods 0.000 title claims abstract description 26
- 238000011084 recovery Methods 0.000 title claims abstract description 26
- 235000017060 Arachis glabrata Nutrition 0.000 claims abstract description 111
- 235000010777 Arachis hypogaea Nutrition 0.000 claims abstract description 111
- 235000018262 Arachis monticola Nutrition 0.000 claims abstract description 111
- 235000020232 peanut Nutrition 0.000 claims abstract description 111
- 239000000843 powder Substances 0.000 claims abstract description 68
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 44
- 238000010438 heat treatment Methods 0.000 claims abstract description 25
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 23
- 239000011591 potassium Substances 0.000 claims abstract description 23
- 239000001103 potassium chloride Substances 0.000 claims abstract description 22
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 22
- 239000002028 Biomass Substances 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 13
- 238000001291 vacuum drying Methods 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 238000000227 grinding Methods 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- 230000004913 activation Effects 0.000 claims abstract description 4
- 238000002791 soaking Methods 0.000 claims abstract description 4
- 238000007873 sieving Methods 0.000 claims abstract description 3
- 239000007789 gas Substances 0.000 claims description 18
- 235000012054 meals Nutrition 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims description 3
- 244000105624 Arachis hypogaea Species 0.000 claims 7
- 235000000073 Amphicarpaea bracteata Nutrition 0.000 claims 1
- 240000002470 Amphicarpaea bracteata Species 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 241001553178 Arachis glabrata Species 0.000 abstract description 104
- 239000011148 porous material Substances 0.000 abstract description 5
- 239000003575 carbonaceous material Substances 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 33
- 239000000243 solution Substances 0.000 description 21
- 238000005303 weighing Methods 0.000 description 18
- 239000008367 deionised water Substances 0.000 description 10
- 229910021641 deionized water Inorganic materials 0.000 description 10
- 238000007654 immersion Methods 0.000 description 10
- 239000002699 waste material Substances 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 230000008859 change Effects 0.000 description 9
- 238000012216 screening Methods 0.000 description 8
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 6
- 238000004455 differential thermal analysis Methods 0.000 description 6
- 230000001360 synchronised effect Effects 0.000 description 6
- 230000003213 activating effect Effects 0.000 description 4
- 239000002154 agricultural waste Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000446 fuel Substances 0.000 description 3
- 238000001819 mass spectrum Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- JQMFQLVAJGZSQS-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-N-(2-oxo-3H-1,3-benzoxazol-6-yl)acetamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)NC1=CC2=C(NC(O2)=O)C=C1 JQMFQLVAJGZSQS-UHFFFAOYSA-N 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012527 feed solution Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
-
- 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
- C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
- C10J3/00—Production of combustible gases containing carbon monoxide from solid carbonaceous fuels
- C10J3/02—Fixed-bed gasification of lump fuel
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
- C10J2300/00—Details of gasification processes
- C10J2300/09—Details of the feed, e.g. feeding of spent catalyst, inert gas or halogens
- C10J2300/0913—Carbonaceous raw material
- C10J2300/0946—Waste, e.g. MSW, tires, glass, tar sand, peat, paper, lignite, oil shale
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- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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- Environmental & Geological Engineering (AREA)
- Combustion & Propulsion (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a method for preparing high-performance biochar by pyrolysis and coupling energy recovery, which comprises the following steps: crushing, grinding, sieving and drying peanut shell biomass to obtain peanut shell powder, adding the peanut shell powder into a potassium chloride solution, stirring and soaking for activation, and vacuum drying to evaporate the solution to obtain potassium-activated peanut shell powder; under inert atmosphere, heating the potassium activated peanut shell powder to 650-850 ℃ at a speed of 5-30 ℃/min for pyrolysis, and recovering pyrolysis gas and high-quality tar to realize energy recovery and prepare high-performance biochar. The invention realizes simultaneous energy recovery and preparation of the biological carbon material with higher specific surface area and pore volume by adopting a very small amount of potassium to activate peanut shell pyrolysis.
Description
Technical Field
The invention relates to the technical field of agricultural waste biomass conversion and utilization, in particular to a method for preparing high-performance biochar by pyrolysis and coupling energy recovery.
Background
The peanut shell is an agricultural waste which is cheap and easy to obtain and has rich sources, and is also a biomass resource with wide application. The peanut shell mainly comprises more than 80% of cellulose, hemicellulose and lignin, has the excellent characteristics of green, clean and renewable, and can effectively replace the traditional fossil resources to be used as clean energy, fuel and value-added products. The annual output of peanut shells is up to 1100 ten thousand tons worldwide, wherein the annual output of China is about 500 ten thousand tons. However, most peanut shells are treated in a landfill or stacking and incineration mode, so that biomass resources are wasted, and the environment is polluted.
Pyrolysis is a powerful means of thermochemical conversion of peanut shell biomass. Peanut shell pyrolysis can produce biochar, tar, and pyrolysis gases (e.g., CO/H) 2 ，CH 4 And C 2 H 4 ) They can be used as fuel and high added value products, thereby realizing the dual benefits of economic development and environmental protection. In the prior art, related researches on the pyrolysis conversion of peanut shells into energy or the preparation of high-performance biochar by the peanut shells are reported, but released tar and pyrolysis gas are ignored in the traditional process of preparing the biochar by the peanut shells, the oxygen-containing component of the tar generated in the process of recycling the energy by pyrolysis of the peanut shells is too high and easy to deteriorate, and the pore volume and specific surface area of the byproduct biochar are smaller, so that the application is limited. Therefore, coupling the process of pyrolyzing peanut shell agricultural waste to recover energy and preparing high-performance biochar has important significance for the maximum utilization of resources.
Disclosure of Invention
In order to solve the problems, the invention provides a method for preparing high-performance biochar by pyrolysis and coupling energy recovery.
The aim of the invention is realized by adopting the following technical scheme:
a method for preparing high-performance biochar by pyrolysis and coupling energy recovery comprises the following steps:
(1) Crushing, grinding, sieving and drying peanut shell biomass to obtain peanut shell powder, adding the peanut shell powder into a potassium chloride solution, stirring and soaking for activation, and vacuum drying to evaporate the solution to obtain potassium-activated peanut shell powder;
(2) Under inert atmosphere, heating the potassium activated peanut shell powder to 650-850 ℃ at a speed of 5-30 ℃/min for pyrolysis, recovering pyrolysis gas and high-quality tar, and simultaneously preparing high-performance biochar.
In some preferred embodiments, the peanut shell meal has a ground mesh size of 200 mesh.
In some preferred embodiments, the mass of potassium chloride is 1.0wt% to 3.0wt% of the peanut shell meal.
In some preferred embodiments, the ratio of feed solution of the peanut shell to the potassium chloride solution is from 0.5g/20mL to 2.0g/20mL.
In some preferred embodiments, the time of agitation impregnation is 12-36 hours.
In some preferred embodiments, the vacuum drying is at a temperature of 80 ℃ for a drying time of 24-72 hours.
In some preferred embodiments, the inert atmosphere is high purity nitrogen with a nitrogen flow rate of 20-100mL/min.
In some preferred embodiments, the time of pyrolysis is 2 hours or less.
The beneficial effects of the invention are as follows:
the invention takes renewable agricultural waste peanut shells as raw materials, provides a coupling method for simultaneously recovering energy and preparing high-performance biochar through potassium activation pyrolysis, has rich and easily available sources, low production cost and simple preparation process, is beneficial to large-scale industrial production, and can prepare the biochar material with higher specific surface area and pore volume while recovering pyrolysis gas and tar with lower oxygen content compared with other tar and biochar production methods. The method for preparing high-performance biochar by pyrolysis and coupling energy recovery adopts a very small amount of potassium to activate peanut shells for pyrolysis, so as to effectively promote the pyrolysis of oxygen-containing functional groups (such as m/z=18, 28, 29 and 44) of the peanut shells, thereby improving the yield of pyrolysis gas,improve the quality of tar and the BET specific surface area of the biochar is from 1.02m 2 The/g is obviously improved to 503.45m 2 Per gram, the micropore volume is also from 0m 3 The/g is increased to 0.17m 3 And/g, thus, the produced pyrolysis gas, high-quality tar and high-performance biochar have better application potential.
Drawings
The invention will be further described with reference to the accompanying drawings, in which embodiments do not constitute any limitation of the invention, and other drawings can be obtained by one of ordinary skill in the art without inventive effort from the following drawings.
FIG. 1 is a process flow diagram of a method for pyrolysis to produce high performance biochar and energy recovery coupling according to the present invention;
FIG. 2 is a TG-DSC curve of KCl-PS at 10deg.C/min in example 1;
FIG. 3 is a TG-DSC curve of KCl-PS at 20℃per minute in example 2;
FIG. 4 is a TG-DSC curve of KCl-PS at 30℃per minute in example 3;
FIG. 5 is mass spectra of KCl-PS and PS pyrolysis main pyrolysis gas in example 4 and comparative example 4;
FIG. 6 is a TG-DSC curve of PS at 10deg.C/min in comparative example 1;
FIG. 7 is a TG-DSC curve of PS at 20℃per minute in comparative example 2;
FIG. 8 is a TG-DSC curve of PS at 30℃per minute in comparative example 3;
FIG. 9 is N before and after KCl-PS and PS pyrolysis in example 5 and comparative example 5 2 Adsorption and desorption isotherms and pore size distribution diagrams of KCl-PS pyrolytic biochar;
FIG. 10 is SEM images of the KCl-PS and PS before and after pyrolysis in example 5 and comparative example 5: PS (a 1, a 2) and its derivative biochar (b), KCl-PS (c 1, c 2) and its derivative biochar (d).
Detailed Description
The invention will be further described with reference to the following examples.
Example 1
A method for preparing high-performance biochar by pyrolysis and coupling energy recovery, which comprises the following steps:
(1) Crushing, grinding, screening and drying waste peanut shell biomass from Guangdong province to obtain 200-mesh peanut shell powder, respectively weighing 1.5g of the peanut shell powder and 1.56wt% of potassium chloride, completely dissolving the potassium chloride in 20mL of deionized water, adding the peanut shell powder into a potassium chloride solution by adopting an immersion method at room temperature, stirring and activating for 24 hours, and then vacuum drying for 48 hours at 80 ℃ to evaporate the solution to obtain potassium-activated peanut shell powder, which is marked as KCl-PS;
(2) Weighing 3.5+ -0.3 mg of potassium activated peanut shell powder (KCl-PS) and adding N in a synchronous thermal analyzer (TG-DSC) 2 And (3) heating the sample from room temperature to 800 ℃ under the conditions of flow rate of 40mL/min and heating rate of 10 ℃/min, performing pyrolysis, wherein pyrolysis residence time of 800 ℃ is 0h, measuring the change rate of sample mass and heat along with temperature/time on line, recovering pyrolysis gas and high-quality tar, and simultaneously preparing high-performance biochar.
The thermogravimetric-differential thermal analysis (TG-DSC) curve of the potassium activated peanut shell meal is shown in fig. 2.
Example 2
A method for preparing high-performance biochar by pyrolysis and coupling energy recovery, which comprises the following steps:
(1) Crushing, grinding, screening and drying waste peanut shell biomass from Guangdong province to obtain 200-mesh peanut shell powder, respectively weighing 1.5g of the peanut shell powder and 1.56wt% of potassium chloride, completely dissolving the potassium chloride in 20mL of deionized water, adding the peanut shell powder into a potassium chloride solution by adopting an immersion method at room temperature, stirring and activating for 24 hours, and then vacuum drying for 48 hours at 80 ℃ to evaporate the solution to obtain potassium-activated peanut shell powder, which is marked as KCl-PS;
(2) Weighing 3.5+ -0.3 mg of potassium activated peanut shell powder (KCl-PS) and adding N in a synchronous thermal analyzer (TG-DSC) 2 And (3) heating the sample from room temperature to 800 ℃ under the conditions of flow rate of 40mL/min and heating rate of 20 ℃/min, performing pyrolysis, wherein pyrolysis residence time of 800 ℃ is 0h, and on-line measuring the change rate of sample mass and heat along with temperature/time, recovering pyrolysis gas and high-quality tar, and simultaneously preparing high-performance biochar.
The thermogravimetric-differential thermal analysis (TG-DSC) curve of the potassium activated peanut shell meal is shown in fig. 3.
Example 3
A method for preparing high-performance biochar by pyrolysis and coupling energy recovery, which comprises the following steps:
(1) Crushing, grinding, screening and drying waste peanut shell biomass from Guangdong province to obtain 200-mesh peanut shell powder, respectively weighing 1.5g of the peanut shell powder and 1.56wt% of potassium chloride, completely dissolving the potassium chloride in 20mL of deionized water, adding the peanut shell powder into a potassium chloride solution by adopting an immersion method at room temperature, stirring and activating for 24 hours, and then vacuum drying for 48 hours at 80 ℃ to evaporate the solution to obtain potassium-activated peanut shell powder, which is marked as KCl-PS;
(2) Weighing 3.5+ -0.3 mg of potassium activated peanut shell powder (KCl-PS) and adding N in a synchronous thermal analyzer (TG-DSC) 2 And (3) heating the sample from room temperature to 800 ℃ under the conditions of flow rate of 40mL/min and heating rate of 30 ℃/min, performing pyrolysis, wherein pyrolysis residence time of 800 ℃ is 0h, and on-line measuring the change rate of sample mass and heat along with temperature/time, recovering pyrolysis gas and high-quality tar, and simultaneously preparing high-performance biochar.
The thermogravimetric-differential thermal analysis (TG-DSC) curve of the potassium activated peanut shell meal is shown in fig. 4.
Example 4
A method for preparing high-performance biochar by pyrolysis and coupling energy recovery, which comprises the following steps:
(1) Crushing, grinding, screening and drying waste peanut shell biomass from Guangdong province to obtain 200-mesh peanut shell powder, respectively weighing 1.5g of the peanut shell powder and 1.56wt% of potassium chloride, completely dissolving the potassium chloride in 20mL of deionized water, adding the peanut shell powder into a potassium chloride solution by adopting an immersion method at room temperature, stirring and activating for 24 hours, and then vacuum drying for 48 hours at 80 ℃ to evaporate the solution to obtain potassium-activated peanut shell powder, which is marked as KCl-PS;
(2) Weighing 6.5+ -0.3 mg of potassium activated peanut shell powder (KCl-PS) in thermogravimetric-mass spectrometer (TG-MS)N 2 And (3) heating the sample from room temperature to 800 ℃ under the conditions of flow rate of 100mL/min and heating rate of 10 ℃/min, performing pyrolysis, wherein pyrolysis residence time of 800 ℃ is 0h, and measuring the mass of the sample and the change rate of pyrolysis gas along with temperature/time on line.
The mass spectrum of the main pyrolysis gas of the potassium-activated peanut shell meal is shown in fig. 5.
Example 5
A method for preparing high-performance biochar by pyrolysis and coupling energy recovery, which comprises the following steps:
(1) Waste peanut shell biomass from Guangdong province is crushed, ground, screened and dried to obtain 200-mesh peanut shell powder, 1.5g of the peanut shell powder and 1.56wt% of potassium chloride are respectively weighed, the potassium chloride is firstly completely dissolved in 20mL of deionized water, the peanut shell powder is added into a potassium chloride solution by an immersion method at room temperature, stirred and activated for 24 hours, then the solution is dried in vacuum for 48 hours at 80 ℃ to evaporate, the potassium-activated peanut shell powder is obtained, the obtained peanut shell powder is recorded as KCl-PS, and the high heat value and BET surface area of the KCl-PS are respectively 15.91MJ/kg and 1.02m 2 /g；
(2) Weighing 300mg of potassium activated peanut shell powder (KCl-PS) in a tube furnace with N 2 Pyrolysis is carried out from room temperature to 800 ℃ under the conditions of flow rate of 40mL/min and heating rate of 10 ℃/min, pyrolysis residence time of 0h at 800 ℃, pyrolysis gas and high-quality tar are recovered, high-performance biochar is prepared, and the high heat value and BET surface area of the biochar are measured to be 22.68MJ/kg and 503.45m respectively 2 High heating value and BET surface area increase significantly after heat treatment per gram.
Comparative example 1
A method for preparing high-performance biochar by pyrolysis and coupling energy recovery, which comprises the following steps:
(1) Crushing, grinding, screening and drying waste peanut shell biomass from Guangdong province to obtain peanut shell powder with 200 meshes, weighing 1.5g of the peanut shell powder, adding the peanut shell powder into 20mL of deionized water at room temperature by adopting an immersion method, stirring and immersing for 24 hours, and then vacuum drying for 48 hours at 80 ℃ to evaporate the solution to obtain comparative peanut shell powder, and marking the comparative peanut shell powder as PS;
(2) Weighing 3.5+ -0.3 mg of the comparative peanut shell Powder (PS), and adding N in a synchronous thermal analyzer (TG-DSC) 2 And (3) heating the sample from room temperature to 800 ℃ under the conditions of flow rate of 40mL/min and heating rate of 10 ℃/min, performing pyrolysis, and measuring the change rate of the sample mass and heat along with temperature/time on line, wherein the pyrolysis residence time of 800 ℃ is 0 h.
The thermogravimetric-differential thermal analysis (TG-DSC) curve of the comparative peanut shell meal is shown in fig. 6.
Comparative example 2
A method for preparing high-performance biochar by pyrolysis and coupling energy recovery, which comprises the following steps:
(1) Crushing, grinding, screening and drying waste peanut shell biomass from Guangdong province to obtain peanut shell powder with 200 meshes, weighing 1.5g of the peanut shell powder, adding the peanut shell powder into 20mL of deionized water at room temperature by adopting an immersion method, stirring and immersing for 24 hours, and then vacuum drying for 48 hours at 80 ℃ to evaporate the solution to obtain comparative peanut shell powder, and marking the comparative peanut shell powder as PS;
(2) Weighing 3.5+ -0.3 mg of the comparative peanut shell Powder (PS), and adding N in a synchronous thermal analyzer (TG-DSC) 2 And (3) heating the sample from room temperature to 800 ℃ under the conditions of flow rate of 40mL/min and heating rate of 20 ℃/min, performing pyrolysis, and measuring the change rate of the sample mass and heat along with temperature/time on line, wherein the pyrolysis residence time of 800 ℃ is 0 h.
The thermogravimetric-differential thermal analysis (TG-DSC) curve of the comparative peanut shell meal is shown in fig. 7.
Comparative example 3
A method for preparing high-performance biochar by pyrolysis and coupling energy recovery, which comprises the following steps:
(1) Crushing, grinding, screening and drying waste peanut shell biomass from Guangdong province to obtain peanut shell powder with 200 meshes, weighing 1.5g of the peanut shell powder, adding the peanut shell powder into 20mL of deionized water at room temperature by adopting an immersion method, stirring and immersing for 24 hours, and then vacuum drying for 48 hours at 80 ℃ to evaporate the solution to obtain comparative peanut shell powder, and marking the comparative peanut shell powder as PS;
(2) Weighing 3.5+ -0.3 mg of the comparative peanut shell Powder (PS), and adding N in a synchronous thermal analyzer (TG-DSC) 2 And (3) heating the sample from room temperature to 800 ℃ under the conditions of flow rate of 40mL/min and heating rate of 30 ℃/min, performing pyrolysis, and measuring the change rate of the sample mass and heat along with temperature/time on line, wherein the pyrolysis residence time of 800 ℃ is 0 h.
The thermogravimetric-differential thermal analysis (TG-DSC) curve of the comparative peanut shell meal is shown in fig. 8.
Comparative example 4
A method for preparing high-performance biochar by pyrolysis and coupling energy recovery, which comprises the following steps:
(1) Crushing, grinding, screening and drying waste peanut shell biomass from Guangdong province to obtain peanut shell powder with 200 meshes, weighing 1.5g of the peanut shell powder, adding the peanut shell powder into 20mL of deionized water at room temperature by adopting an immersion method, stirring and immersing for 24 hours, and then vacuum drying for 48 hours at 80 ℃ to evaporate the solution to obtain comparative peanut shell powder, and marking the comparative peanut shell powder as PS;
(2) Weighing 6.5+ -0.3 mg of the comparative peanut shell Powder (PS) and using N in a thermogravimetric-mass spectrometer (TG-MS) 2 And (3) heating the sample from room temperature to 800 ℃ under the conditions of flow rate of 100mL/min and heating rate of 10 ℃/min, performing pyrolysis, wherein pyrolysis residence time of 800 ℃ is 0h, and measuring the mass of the sample and the change rate of pyrolysis gas along with temperature/time on line.
The mass spectrum of the main pyrolysis gas of the comparative peanut shell meal is shown in fig. 5.
Comparative example 5
A method for preparing high-performance biochar by pyrolysis and coupling energy recovery, which comprises the following steps:
(1) Waste peanut shell biomass from Guangdong province is crushed, ground, screened and dried to obtain peanut shell powder with 200 meshes, 1.5g of the peanut shell powder is weighed, the peanut shell powder is added into 20mL of deionized water at room temperature by adopting an immersion method, stirred and immersed for 24 hours, then the solution is evaporated in vacuum for 48 hours at 80 ℃ to obtain comparative peanut shell powder, the comparative peanut shell powder is marked as PS, and the high heat value and BET surface area of the PS are respectively 16.56MJ/kg and 2.99m 2 /g；
(2) Weighing 300mg of the comparative peanut shell meal (PS) in a tube furnace with N 2 Flow rate is 40mL/min, heating rate is 10 ℃/minHeating from room temperature to 800 ℃ for pyrolysis, wherein the pyrolysis residence time of 800 ℃ is 0h; determination of the high calorific value and BET surface area of the biochar of 22.62MJ/kg and 1.59m, respectively 2 After heat treatment, the high calorific value increases significantly and the BET surface area decreases.
TABLE 1 high heating value and pore Structure property Change data for KCl-PS and PS products before and after pyrolysis in example 5 and comparative example 5
Compared with the biological carbon material prepared by pyrolysis of peanut shells, the biological carbon material prepared by the comparative example provided by the invention has the advantages that the BET surface area and the micropore volume are obviously improved, and the biological carbon material has better application potential in the aspects of adsorption, catalysis, soil remediation and the like; meanwhile, compared with pyrolysis gas and tar produced by pyrolysis of peanut shells, the pyrolysis gas and tar produced by the comparative example have higher yield, lower oxygen content of tar and better application potential in the aspects of synthetic fuel and high added value products.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention.
Claims (8)
1. The method for preparing high-performance biochar by pyrolysis and coupling energy recovery is characterized by comprising the following steps of:
(1) Crushing, grinding, sieving and drying peanut shell biomass to obtain peanut shell powder, adding the peanut shell powder into a potassium chloride solution, stirring and soaking for activation, and vacuum drying to evaporate the solution to obtain potassium-activated peanut shell powder;
(2) Under inert atmosphere, heating the potassium activated peanut shell powder to 650-850 ℃ at a speed of 5-30 ℃/min for pyrolysis, recovering pyrolysis gas and high-quality tar, and simultaneously preparing high-performance biochar.
2. The method for coupling high performance biochar production and energy recovery by pyrolysis according to claim 1, wherein the ground peanut shell meal is 200 mesh in mesh size.
3. The method for preparing high-performance biochar and recycling and coupling energy by pyrolysis according to claim 1, wherein the mass of the potassium chloride is 1.0-3.0 wt% of the peanut shell powder.
4. The method for preparing high-performance biochar and energy recovery coupled according to claim 1, wherein the feed liquid ratio of the peanut shell to the potassium chloride solution is 0.5g/20mL to 2.0g/20mL.
5. The method for coupling high-performance biochar preparation and energy recovery by pyrolysis according to claim 1, wherein the stirring and soaking time is 12-36h.
6. The method for coupling high-performance biochar preparation and energy recovery by pyrolysis according to claim 1, wherein the vacuum drying temperature is 80 ℃ and the drying time is 24-72h.
7. The method for preparing high-performance biochar and recycling energy and coupling according to claim 1, wherein the inert atmosphere is high-purity nitrogen, and the nitrogen flow is 20-100mL/min.
8. The method for preparing high-performance biochar and coupling energy recovery by pyrolysis according to claim 1, wherein the pyrolysis time is less than or equal to 2h.
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