CN108611109B - Three-section type heating device, and biological carbon preparation system and preparation method - Google Patents

Three-section type heating device, and biological carbon preparation system and preparation method Download PDF

Info

Publication number
CN108611109B
CN108611109B CN201810343070.5A CN201810343070A CN108611109B CN 108611109 B CN108611109 B CN 108611109B CN 201810343070 A CN201810343070 A CN 201810343070A CN 108611109 B CN108611109 B CN 108611109B
Authority
CN
China
Prior art keywords
section
gas
heating device
heating
biochar
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201810343070.5A
Other languages
Chinese (zh)
Other versions
CN108611109A (en
Inventor
张亚平
李飞
张会岩
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Southeast University
Original Assignee
Southeast University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Southeast University filed Critical Southeast University
Priority to CN201810343070.5A priority Critical patent/CN108611109B/en
Publication of CN108611109A publication Critical patent/CN108611109A/en
Application granted granted Critical
Publication of CN108611109B publication Critical patent/CN108611109B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
    • C10B53/02—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of cellulose-containing material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/75—Multi-step processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/77—Liquid phase processes
    • B01D53/78—Liquid phase processes with gas-liquid contact
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • 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
    • C10B57/02—Multi-step carbonising or coking processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
    • 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Environmental & Geological Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Biomedical Technology (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The invention discloses a three-section type heating device, a biochar preparation system and a preparation method, wherein the three-section type heating device comprises a heating furnace and a reducing reactor positioned in the heating furnace; the biochar preparation system comprises a three-section type heating device, wherein the feed end of the heating device is connected with a gas supply device, and the discharge end of the heating device is sequentially connected with a separator and a tail gas treatment device; the preparation method comprises the steps of adding reaction materials into the three-section type heating device, supplying gas to the three-section type heating device through the gas supply device, and carrying out pyrolysis reaction to generate biochar, bio-oil and gas, wherein the bio-oil and the gas are separated through the separator, the bio-oil is collected and obtained, and the gas is purified and treated by the tail gas treatment device and then is discharged. The invention has the following remarkable advantages: firstly, the three-section type heating device can improve the heat transfer speed and the airflow rate; secondly, the biochar preparation system can accurately prepare biochar with better adsorption effect on adsorption performance, and is environment-friendly and pollution-free; meanwhile, the preparation method is simple, easy to operate and low in energy consumption.

Description

Three-section type heating device, and biological carbon preparation system and preparation method
Technical Field
The invention belongs to the field of preparation of biochar, and particularly relates to a three-section type heating device, a biochar preparation system and a preparation method.
Background
In recent years, the problem of heavy metal pollution of water and soil is very serious. Cd pollution in water is mainly caused by artificial reasons, including electroplating, non-ferrous metal smelting, alloy manufacturing, discharging of industrial Cd-containing wastewater such as pigment and Cd-Ni battery. Cd pollution of soil, sediments, surface water and groundwater is also receiving more and more attention due to the great harm of Cd to the environment and human body. At present, the solution of heavy metals in water and soil is the focus of current research. Statistically, 8 hundred million tons of crop straws are produced per year, and the majority of crops (rice, wheat and corn) are about 6 hundred million tons. Therefore, the unused crop straws are accumulated in farmlands, which not only occupies a large amount of land, wastes resources and causes serious environmental pollution, but also causes serious air environmental pollution even by direct incineration in the past.
The pyrolysis technology is a main way for reducing, harmlessly treating and recycling solid wastes, and is a new solid waste treatment technology researched and developed in recent years. Biomass pyrolysis can not only obtain renewable energy and co-produce chemicals (oil and gas), but also produce a large amount of biochar. The effective utilization of crop straw resources can save a large amount of fossil fuels and effectively reduce the emission of greenhouse gases, and the application of the obtained biochar to the current serious water and soil heavy metal pollution is an effective way. The biochar prepared from the straws has a large amount of microporous structures and large specific surface areas, has strong metal adsorption capacity, and can influence the migration and transformation of heavy metals in the environment, the biomass of crops and the like. The biochar can adsorb heavy metals and fix the heavy metals on the surface of the biochar and even in gaps, so that the biological effectiveness of most heavy metals is obviously reduced, the physical, chemical and biological properties of soil can be improved, and the soil fertility and the crop yield are improved. Has strong effect on adsorbing and removing heavy metal pollution of water body. Therefore, optimizing biomass preparation devices and systems to obtain a large amount of high-quality biochar materials is of great importance.
However, because of the strict requirements of pyrolysis on process technology and operation control and the high cost of equipment and treatment, the pyrolysis research on agricultural wastes was carried out in the early 80 s of the 20 th century. In recent years, due to the global energy crisis, research on pyrolysis technology is more intensive at home and abroad, wherein the research comprises preparing carbonaceous materials by using the pyrolysis technology. However, the traditional biochar preparation device and the traditional biochar preparation technology are relatively backward, have the defects of high energy consumption and high pollution, and cannot be applied to large-scale industrialization. The initial preparation device is a rotary kiln, the device has poor air tightness and poor carbon quality, and a large amount of heat energy is consumed to be gradually eliminated. With the further development of the device, a continuous feeding device and a fixed bed device appear, but the device does not effectively solve the problems of program heating and temperature control, and the actual temperature difference is large, so that the device is not beneficial to fine research and production. Therefore, if the preparation device can be improved and the biochar preparation technology can be well applied, the biochar which is economical, low in cost, easy to regenerate and excellent in performance can be prepared and used for treating water and soil heavy metal pollution, the application process of carbon storage can be promoted, and the problem of resource utilization of agricultural and forestry waste is solved.
Disclosure of Invention
The purpose of the invention is as follows: the first purpose of the invention is to provide a three-section heating device with stable temperature layer, fast heat transfer and high air flow rate;
the second purpose of the invention is to provide a system for preparing biochar by adopting the three-section type heating device, which not only can more accurately prepare high-performance biochar, but also is environment-friendly and pollution-free;
the third purpose of the invention is to provide a method for preparing the biochar by adopting the system, which omits the complicated process, is easy to operate and has low energy consumption, and the prepared biochar is uniform and has high quality.
The technical scheme is as follows: the three-section heating device comprises a heating furnace and a variable-diameter reactor positioned in the heating furnace, wherein the heating furnace comprises three heating sections from top to bottom, the variable-diameter reactor comprises an upper heated section, a lower heated section and a material reaction section positioned in the middle, and the three heating sections of the heating furnace respectively provide heat sources for the upper heated section, the lower heated section and the material reaction section; the diameter of the upper heated section is larger than that of the lower heated section, and the material reaction section is connected between the upper heated section and the lower heated section to form a diameter-variable section.
The invention adopts a three-section type heating device consisting of a heating furnace and a reducing reactor positioned in the heating furnace, a turbulent layer is formed in the reducing reactor along with the flow of air flow, the outer wall of the reducing reaction tube is connected with a heating system, and the temperature of the outer wall is higher than the internal temperature of the reducing reactor, so that the temperature layer is disturbed along with the air flow from the outer wall to the internal of the reducing reactor, the temperature change of the turbulent layer is larger, the central air flow of the reducing reactor is stable, the temperature change is small, the temperature of the wall layer of the reducing reactor is shifted upwards due to the deviation of the temperature layer, and the actual material monitoring temperature is lower. The invention adopts the three-section heating furnace for simultaneous heating, which can effectively weaken the deviation of the temperature layer and stabilize the temperature layer in the material reaction section. The lower end of the material layer is a lower heating section, and the air flow rate is accelerated by using a diameter-variable means, so that the heat transfer resistance is reduced, and the removal of impurities is accelerated, thereby realizing efficient and precise carbon preparation. Furthermore, the three-section heating device is not only used for preparing carbon, but also suitable for the fields of biomass oil refining, catalyst preparation or nano material preparation and the like, and has wide application value.
Preferably, the diameters of the upper heated section and the lower heated section of the reducing reactor can be 1.5-2: 1, the diameter ratio in the range can ensure that product crystals are not blocked, impurities can rapidly enter a condensation system along with air flow, and biological oil coking is avoided. If the diameter ratio is too large, blockage of reactant crystallization and coking of bio-oil in the lower heating section are caused, and if the diameter ratio is too small, the changed gas velocity is not obvious, and the effect is not obvious.
The system for preparing the biochar by adopting the three-section type heating device comprises the three-section type heating device, wherein the feeding end of the three-section type heating device is connected with the gas supply device, and the discharging end of the three-section type heating device is sequentially connected with the separator and the tail gas treatment device.
The system can continuously feed materials, has high energy efficiency, reduces the emission of pollutants, does not have the heat release operation of air inlet, and improves the energy efficiency and the yield; secondly, the byproducts can be recovered, the pollution discharge is reduced, the economy is improved, the characteristics of the biochar can be improved by controlling the preparation conditions, and the yield of the byproducts is changed; meanwhile, the pyrolysis raw materials are not limited, both woody and herbaceous biomass can be used, and the device has a good tail gas treatment system and can achieve harmless treatment.
The system disclosed by the invention can effectively control the temperature layer by combining the three-section heating device and the oil-liquid separator, solve the problem of impurity retention and realize rapid gas-liquid-solid three-phase separation, and simultaneously effectively prevent secondary pollution by combining the tail gas treatment device. Furthermore, the system also comprises three temperature control devices for respectively controlling the three heating sections of the heating furnace. A condenser is also arranged between the separator and the three-section type heating device. The tail gas treatment unit comprises a solid absorber and a liquid absorber which are connected with the separator. A flow control device is also arranged between the three-section type heating device and the air supply device.
The method for preparing the biochar by adopting the system comprises the following steps: reaction materials are added into the three-section type heating device, gas is supplied to the three-section type heating device through the gas supply device, the reaction materials are subjected to pyrolysis reaction to generate biochar, bio-oil and gas, the bio-oil and the gas are separated through the separator, the bio-oil is collected and obtained, and the gas is discharged after being purified by the tail gas treatment device.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages: firstly, the three-section type heating device combines the reducing reactor with the three-section type heating furnace, so that a temperature layer can be effectively controlled, impurity retention is solved, gas-liquid-solid three-phase separation is fast, the heat transfer speed and the gas flow speed are improved, and the effects of cleanness and low energy consumption are achieved; secondly, the biochar preparation system not only can accurately prepare biochar with better adsorption effect on adsorption performance, but also is combined with a tail gas treatment device to treat the discharged tail gas, so that the biochar is tasteless, harmless, environment-friendly and pollution-free; meanwhile, the method can efficiently prepare the biochar with uniform carbon quality and high quality, omits a complicated process, is easy to operate and has low energy consumption.
Drawings
FIG. 1 is a schematic structural diagram of a variable diameter reactor of the present invention;
FIG. 2 is a schematic view of a biochar production system of the present invention;
FIG. 3 is a surface topography of the rice straw biochar prepared by the present invention;
FIG. 4 is a graph showing the results of adsorption removal rates of biochar prepared according to the present invention at different times;
FIG. 5 is an adsorption diagram of Cd ions by biochar of different raw materials prepared by the invention under different pH values.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to the accompanying drawings.
The three-section heating device comprises a heating furnace 1, wherein a reducing reactor 2 is arranged in the heating furnace 1, as shown in figure 1, the reducing reactor 2 is in a three-section type and sequentially comprises an upper heated section 3, a material reaction section 5 and a lower heated section 4 from top to bottom, wherein the diameter of the upper heated section 3 is larger than that of the lower heated section 4, the material reaction section 5 is connected between the upper heated section 3 and the lower heated section 4 to form a reducing section, and the diameter of the material reaction section 5 is gradually reduced from top to bottom. In actual operation, the diameter ratio of the upper heated section 3 to the lower heated section 4 is 1.5-2: 1, so that the heat transfer rate is accelerated, the heat transfer resistance is reduced, the deviation on a temperature field can be effectively prevented, the stability of a temperature layer is ensured, the temperature control error is reduced, and the accuracy is higher. The heating furnace 1 is also a three-section heating furnace, that is, the heating furnace comprises three heating zones from top to bottom, the three heating zones respectively correspond to the three sections of the reducing reactor 2 one by one, and respectively provide heat sources for the three sections of the reducing reactor 2. In addition, quartz wool packing for supporting the reaction materials in the material reaction section 5 and preventing the reaction materials from falling down can be arranged in the lower heated section 4.
As shown in FIG. 2, the biochar preparation system of the invention can be built by using the three-stage heating device, and comprises the three-stage heating device, the gas supply device 6 and the separator 7, wherein the gas supply device 6 is connected with the feeding end of the three-stage heating device, and the separator 7 is connected with the discharging end of the three-stage heating device. The gas supply 6 may comprise CO2Gas cylinder and N2And the bottle is used for providing corresponding gas for the reaction, so that the reducing reactor 2 is in a state of no air or little air. The three-section type heating device regulates and controls the temperature of the three heating zones through three temperature control devices 11 respectively. In fig. 2, three temperature control devices 11 are located on both sides of the three-stage heating device. A flow control device 12 can be arranged between the three-section heating device and the gas supply device 6 and can be used for regulating and controlling the flow of the gas delivered by the gas supply device. A condenser 8 can also be arranged between the separator 7 and the three-stage heating device, and the condenser is used for condensingThe product is condensed, a tail gas treatment device can be arranged at the discharge port section of the separator 7 and comprises a solid absorber 9 and a liquid absorber 10, wherein the inlet of the solid absorber 9 is connected with the outlet of the separator 7, the outlet of the solid absorber 9 is connected with the inlet of the liquid absorber 10, meanwhile, the liquid absorber 10 can be arranged in a plurality of (two in the figure), and the whole tail gas treatment device can treat tail gas after pyrolysis reaction, reduce the emission of pollutants and achieve the effect of harmless treatment.
The method for preparing the biochar by adopting the system comprises the following steps:
(1) adding materials from the feed end of the reducing reactor 2 in the three-section heating device, respectively starting the three temperature control devices 11, controlling the temperature of the three-section heating device, and simultaneously, controlling the temperature of the three-section heating device by CO2Gas cylinder and N2The bottle provides gas for the reducing reactor 2, and the reducing reactor 2 is isolated from air or contains a small amount of air by adjusting the flow control device 12, so as to provide conditions for biomass pyrolysis reaction.
(2) After the biomass pyrolysis reaction, the charcoal is directly obtained from the reducing reactor 2, the bio-oil and the gas are condensed by the condenser 8 and enter the separator 7, the bio-oil is directly collected and obtained after being separated by the separator 7, the gas enters the tail gas treatment device to be subjected to tail gas purification treatment, the gas enters the solid absorber 9 in the tail gas treatment device firstly, and then the gas is sequentially introduced into the liquid absorbers 10 with different concentrations, so that the tail gas purification effect can be achieved.
Wherein, preferably, the flow rate of the pyrolysis gas can be 0.2-5L/min, the pyrolysis temperature can be 400-1000 ℃, the heating rate can be 5-25 ℃/min, and the pyrolysis time can be 0.5-3 h. After the pyrolysis reaction, the cooling rate can be 10-20 ℃/min, and the flow rate of the cooling gas can be 0.1-0.2L/min. By adopting the system and the preparation process parameters, the biochar with uniform carbon quality and high quality can be prepared, and the system and the preparation process have low energy consumption and are easy to operate.
Example 1
The method for preparing the biochar by adopting the coconut shells comprises the following steps:
(1) pretreatment of coconut shells: washing coconut shells with water, drying the coconut shells in the air, drying the coconut shells in an oven at the temperature of 80 ℃ to constant weight, and then crushing the coconut shells to the particle size of 5-10 mm by using an LFP-800 crusher;
(2) adding crushed coconut shells from the feed end of a reducing reactor 2 in a three-section type heating device, respectively starting three temperature control devices 11, setting the pyrolysis temperature to be 600 ℃, the temperature rise rate to be 20 ℃/min, simultaneously setting the pyrolysis gas velocity to be 0.5L/min by adjusting a gas flow control device 12, and carrying out pyrolysis reaction for 1 h;
(3) after the pyrolysis reaction, adjusting the cooling rate to be 20 ℃/min and reducing the temperature to be 300 ℃, setting the gas velocity of pyrolysis gas to be 0.2L/min, after the temperature is reduced to room temperature, directly obtaining the generated biological carbon from the reducing reactor 2, condensing the biological oil and the gas through a condenser 8 and then entering a separator 7, separating through the separator 7, directly collecting the biological oil to obtain the biological carbon, and introducing the gas into a tail gas treatment device for tail gas purification treatment, wherein the gas firstly enters a solid absorber 9 (in which the recovered biological carbon and the existing commercial adsorbent material are filled) in the tail gas treatment device, and then sequentially introducing H with the concentration of 5 percent respectively2 O 210% of HNO3The liquid absorber 10 of the solution achieves the effect of tail gas purification.
Example 2
The method for preparing the biochar by adopting the rice straws comprises the following steps:
(1) pretreatment of rice straws: washing and airing the rice straws, drying the rice straws in an oven at 70 ℃ to constant weight, and then crushing the rice straws to 5-10 mm in particle size by using an LFP-800 crusher;
(2) adding crushed rice straws from the feed end of a reducing reactor 2 in the three-section type heating device, respectively starting three temperature control devices 11, setting pyrolysis temperature to be 600 ℃, heating rate to be 15 ℃/min, simultaneously setting pyrolysis gas speed to be 0.5L/min by adjusting a gas flow control device 12, and carrying out pyrolysis reaction for 1 h;
(3) after the pyrolysis reaction, the temperature reduction rate is adjusted to be 20 ℃/min and reduced to 300 ℃, the gas velocity of pyrolysis gas is set to be 0.2L/min, after the temperature is reduced to the room temperature, the generated biochar is directly obtained from the reducing reactor 2, and the biological oil and gas pass throughThe condensed gas enters a condenser 8 and enters a separator 7, the bio-oil is directly collected and obtained after being separated by the separator 7, the gas enters a tail gas treatment device for tail gas purification treatment, the gas enters a solid absorber 9 (containing recycled biochar and the existing commercial adsorbent material) in the tail gas treatment device, and then H with the concentration of 5 percent is sequentially introduced2 O 210% of HNO3The liquid absorber 10 of the solution achieves the effect of tail gas purification.
The morphology of the biochar prepared in the example is observed, the obtained result is shown in fig. 3, and as can be seen from fig. 3, the biochar prepared by the system of the invention has the advantages of rich surface structure, uniform carbon quality and high quality.
Example 3
The method for preparing the biochar by adopting the apricot shells comprises the following steps:
(1) pretreating apricot shells: washing and airing apricot shells, drying the apricot shells to constant weight in an oven at the temperature of 60 ℃, and then crushing the apricot shells to the particle size of 5-10 mm by using an LFP-800 crusher;
(2) adding crushed apricot shells from the feed end of a reducing reactor 2 in a three-section type heating device, respectively starting three temperature control devices 11, setting pyrolysis temperature to be 600 ℃, heating rate to be 10 ℃/min, simultaneously setting pyrolysis gas velocity to be 0.5L/min by adjusting a gas flow control device 12, and carrying out pyrolysis reaction for 1 h;
(3) after the pyrolysis reaction, adjusting the cooling rate to be 20 ℃/min and reducing the temperature to 300 ℃, setting the gas velocity of pyrolysis gas to be 0.2L/min, after the temperature is reduced to room temperature, directly obtaining the generated biological carbon from the reducing reactor 2, condensing the biological oil and the gas through a condenser 8 and then entering a separator 7, separating through the separator 7, directly collecting the biological oil to obtain the biological oil, introducing the gas into a tail gas treatment device to carry out tail gas purification treatment, wherein the gas enters a solid absorber 9 (in which the recovered biological carbon and the existing commercial adsorbent material are filled) in the tail gas treatment device, and then sequentially introducing H with the concentration of 5 percent respectively2 O 210% of HNO3The liquid absorber 10 of the solution achieves the effect of tail gas purification.
Example 4
The method for preparing the biochar by using willow comprises the following steps:
(1) pretreatment of willow: washing willow, drying in the air, drying in an oven at 90 ℃ to constant weight, and then crushing to 5-10 mm of particle size by using an LFP-800 crusher;
(2) adding a bed material sodium chloride catalyst and crushed willow from the feed end of a reducing reactor 2 in a three-section type heating device, respectively starting three temperature control devices 11, setting pyrolysis temperature to be 500 ℃, heating rate to be 5 ℃/min, simultaneously setting pyrolysis gas speed to be 0.2L/min by adjusting a gas flow control device 12, and carrying out pyrolysis reaction for 3 hours;
(3) after the pyrolysis reaction, adjusting the cooling rate to be 20 ℃/min and reducing the temperature to be 260 ℃, setting the gas velocity of pyrolysis gas to be 0.2L/min, reducing the temperature to room temperature, directly obtaining the generated biological carbon from the reducing reactor 2, condensing the biological oil and the gas through a condenser 8 and then entering a separator 7, separating through the separator 7, directly collecting the biological oil, and introducing the gas into a tail gas treatment device for tail gas purification treatment, wherein the gas firstly enters a solid absorber 9 (in which the recovered biological carbon and the existing commercial adsorbent material are filled) in the tail gas treatment device, and then sequentially introducing H with the concentration of 5 percent respectively2 O 210% of HNO3The liquid absorber 10 of the solution achieves the effect of tail gas purification.
Example 5
The method for preparing the biochar by adopting the ryegrass comprises the following steps:
(1) pretreatment of ryegrass: washing willow, drying in the air, drying in an oven at 60 ℃ to constant weight, and then crushing to 5-10 mm of particle size by using an LFP-800 crusher;
(2) adding crushed ryegrass from the feed end of a reducing reactor 2 in a three-section type heating device, respectively starting three temperature control devices 11, setting pyrolysis temperature to be 500 ℃, heating rate to be 25 ℃/min, simultaneously setting pyrolysis gas velocity to be 0.5L/min by adjusting a gas flow control device 12, and carrying out pyrolysis reaction for 1 h;
(3) after the pyrolysis reaction, the temperature is adjusted and reducedThe speed of 20 ℃/min is reduced to 250 ℃, the gas velocity of pyrolysis gas is set to be 0.2L/min, the generated biochar is directly obtained from the reducing reactor 2 after being reduced to the room temperature, the bio-oil and the gas enter a separator 7 after being condensed by a condenser 8, the bio-oil is directly collected and obtained after being separated by the separator 7, the gas enters a tail gas treatment device for tail gas purification treatment, wherein the gas firstly enters a solid absorber 9 (which is filled with the recycled biochar and the existing commercial adsorbent material) in the tail gas treatment device, and then H with the concentration of 5 percent is sequentially introduced2 O 210% of HNO3The liquid absorber 10 of the solution achieves the effect of tail gas purification.
Performance test 1
The biochar prepared in the examples 1-5 is used for removing cadmium pollution in water, 0.1g of coconut shell, rice straw, apricot shell, willow and ryegrass biochar are respectively weighed and placed in a 50ml glass bottle, a prepared 50mg/L cadmium solution is added into the glass bottle, the glass bottle is vibrated (180r/min) for 12 hours at the temperature of 25 ℃ and under the condition that the pH value is 7, then filtration is carried out (a filter membrane is a Waterman micropore of 0.45um), the filtrate is used for measuring the content of residual cadmium in the solution by an ICP-OES spectrometer, and the removal rates are respectively 78%, 96%, 82%, 84% and 93%. Therefore, the biochar prepared by the system has strong cadmium adsorption capacity.
Performance test 2
To investigate the influence of different treatment times on the adsorption performance of biochar prepared in examples 1-5, 0.1g of coconut shell, rice straw, apricot shell, willow and rye grass biochar was weighed and placed in a 50ml glass bottle, and a prepared 50mg/L cadmium solution was added to the glass bottle, and the mixture was shaken (180r/min) at 25 ℃ and pH 7 for 5min, 10min, 30min, 60min, 2h, 4h, 8h, 12h, 16h and 24h, and then filtered (filter membrane is Waterman micropore 0.45um), and the filtrate was measured for the residual cadmium content in the solution by ICP-OES spectrometer, and the obtained results are shown in FIG. 4. From the figure, the biochar prepared by the invention has excellent adsorption effect on each component, the removal rate gradually increases and then becomes stable along with the prolonging of time, and the biochar adsorption is close to saturation after 4 hours. In comparison, the adsorption performance of the biochar prepared from the rice straws is superior to that of biochar prepared from other biomasses, and the removal rate of cadmium can reach about 95 percent, which is one of the reasons that the biochar prepared from the rice straws has a developed pore structure and is good in adsorption capacity.
Performance test 3
To investigate the influence of different pH values on the adsorption performance of biochar prepared in examples 1-5, 0.1g of coconut shell, rice straw, apricot shell, willow and rye grass biochar was weighed and placed in a 50ml glass bottle, and a prepared 50mg/L cadmium solution was added to the glass bottle, and the solution was shaken for 12 hours at 25 ℃ and pH values of 2, 3, 4, 5, 6 and 7, and then filtered (the filter membrane was Waterman micropore 0.45um), and the filtrate was measured for the residual cadmium content in the solution with an ICP-OES spectrometer, and the obtained result is shown in FIG. 5. From the figure, the biochar prepared by the invention has excellent adsorption effect on cadmium, the adsorption performance of 5 raw materials of the biochar shows an increasing trend in the process of pH 2-6, when the pH is 6, the optimal adsorption amount is obtained, the pH is continuously increased, the adsorption amount is slowly reduced, and the pH adsorption has important influence.
Example 6
The method for preparing the biochar by adopting the coconut shells comprises the following steps:
(1) pretreatment of coconut shells: washing coconut shells with water, drying the coconut shells in the air, drying the coconut shells in an oven at the temperature of 80 ℃ to constant weight, and then crushing the coconut shells to the particle size of 5-10 mm by using an LFP-800 crusher;
(2) adding crushed coconut shells from the feed end of a reducing reactor 2 in a three-section type heating device, respectively starting three temperature control devices 11, firstly setting the pyrolysis temperature to be 400 ℃, the temperature rise rate to be 20 ℃/min, simultaneously setting the pyrolysis gas velocity to be 0.5L/min by adjusting a gas flow control device 12, and carrying out pyrolysis reaction for 1 h;
(3) after the pyrolysis reaction, setting the gas velocity of pyrolysis gas to be 0.2L/min, cooling to room temperature, directly obtaining the generated biochar from the reducing reactor 2, condensing the bio-oil and the gas through a condenser 8, then entering a separator 7, separating through the separator 7, directly collecting the bio-oil, and introducing the gas into a tail gas treatment deviceThe tail gas purification treatment is carried out, wherein the gas firstly enters a solid absorber 9 (containing recycled biochar and the existing commercial adsorbent material) in the tail gas treatment device, and then H with the concentration of 5 percent respectively is sequentially introduced2 O 210% of HNO3The liquid absorber 10 of the solution achieves the effect of tail gas purification.
(4) Continuously adding the same amount of crushed coconut shells from the feed end of the reducing reactor 2 in the three-section type heating device, starting the three temperature control devices 11, respectively adjusting the temperature to be 500 ℃, 600 ℃, 700 ℃ and 800 ℃, and the heating rate to be 20 ℃/min, simultaneously setting the pyrolysis gas speed to be 0.5L/min by adjusting the gas flow control device 12, and carrying out pyrolysis reaction for 1 h; thereby preparing the biochar at different temperatures. After the pyrolysis reaction, setting the gas velocity of pyrolysis gas to be 0.2L/min, cooling to room temperature, directly obtaining the generated biochar from the reducing reactor 2, condensing the bio-oil and the gas through a condenser 8, then entering a separator 7, separating through the separator 7, directly collecting the bio-oil, and then entering the gas into a tail gas treatment device for tail gas purification treatment, wherein the gas firstly enters a solid absorber 9 (in which the recycled biochar and the existing commercial adsorbent material are filled) in the tail gas treatment device, and then sequentially introducing a plurality of H containing H with the concentration of 5 percent respectively2 O 210% of HNO3The liquid absorber 10 of the solution achieves the effect of tail gas purification.
According to the embodiment, the biochar with uniform carbon quality and high quality can be accurately produced by adopting the biochar preparation system provided by the invention under the conditions that the flow rate of pyrolysis gas is 0.2-5L/min, the pyrolysis temperature is 400-1000 ℃, the temperature rise rate is 5-25 ℃/min, the pyrolysis time is 0.5-3 h, the temperature reduction rate can be 10-20 ℃/min and the flow rate of cooling gas can be 0.1-0.2L/min after pyrolysis reaction, the energy consumption is low, and the biochar preparation system is environment-friendly.

Claims (7)

1. A three-section heating device is characterized in that: comprises a heating furnace (1) and a variable-diameter reactor (2) positioned in the heating furnace; the heating furnace (1) comprises three heating sections from top to bottom, the reducing reactor (2) comprises an upper heating section (3), a lower heating section (4) and a material reaction section (5) positioned in the middle, the air inlet end of the reducing reactor is positioned on the upper heating section (3), and the three heating sections of the heating furnace (1) respectively provide heat sources for the upper heating section (3), the lower heating section (4) and the material reaction section (5); the diameter ratio of the upper heated section (3) to the lower heated section (4) is 1.5-2: 1, and the material reaction section (5) is connected between the upper heated section (3) and the lower heated section (4) to form a reducer section.
2. A system for preparing biochar using the three-stage heating device of claim 1, wherein: comprises a three-section heating device, wherein the feed end of the three-section heating device is connected with a gas supply device (6), and the discharge end of the three-section heating device is sequentially connected with a separator (7) and a tail gas treatment device.
3. The system of claim 2, wherein: a condenser (8) is also arranged between the separator (7) and the three-section type heating device.
4. The system of claim 2, wherein: the tail gas treatment device comprises a solid absorber (9) and a liquid absorber (10) which are connected with the separator (7).
5. The system of claim 2, wherein: the system also comprises three temperature control devices (11) which respectively control the three heating sections of the heating furnace (1).
6. The system of claim 2, wherein: a flow control device (12) is also arranged between the three-section type heating device and the air supply device (6).
7. A method for preparing biochar using the system of claim 2, comprising the steps of: reaction materials are added into the three-section type heating device, and gas is supplied to the three-section type heating device through the gas supply device (6), so that the reaction materials are subjected to pyrolysis reaction to generate biochar, bio-oil and gas, wherein the bio-oil and the gas are separated through the separator (7), the bio-oil is collected and obtained, and the gas is discharged after being purified by the tail gas treatment device.
CN201810343070.5A 2018-04-17 2018-04-17 Three-section type heating device, and biological carbon preparation system and preparation method Active CN108611109B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810343070.5A CN108611109B (en) 2018-04-17 2018-04-17 Three-section type heating device, and biological carbon preparation system and preparation method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810343070.5A CN108611109B (en) 2018-04-17 2018-04-17 Three-section type heating device, and biological carbon preparation system and preparation method

Publications (2)

Publication Number Publication Date
CN108611109A CN108611109A (en) 2018-10-02
CN108611109B true CN108611109B (en) 2020-04-24

Family

ID=63660418

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810343070.5A Active CN108611109B (en) 2018-04-17 2018-04-17 Three-section type heating device, and biological carbon preparation system and preparation method

Country Status (1)

Country Link
CN (1) CN108611109B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110079349A (en) * 2019-05-30 2019-08-02 青岛科技大学 It is a kind of using inclined tube moving-burden bed reactor as the biomass through pyrolysis production technology of core
CN112574766B (en) * 2020-10-22 2022-01-07 浙江科技学院 Intelligent carbonization hot water integrated system for kitchen garbage

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2578337Y (en) * 2002-10-18 2003-10-08 山东理工大学 Biomass pyrolytic liquefier
CN101130698A (en) * 2007-08-15 2008-02-27 胜利油田胜利动力机械有限公司 Method and apparatus for pyrolysis of biomass gas tar oil
CN101144022A (en) * 2007-11-01 2008-03-19 上海交通大学 Three-section type biomass gasifying furnace
CN101781584A (en) * 2010-02-06 2010-07-21 周开根 Method and equipment for gasifying coal by using plasma
JP2016204235A (en) * 2015-04-28 2016-12-08 清水建設株式会社 Gasification apparatus and gas production method
CN106336885A (en) * 2016-10-11 2017-01-18 天津科技大学 System for preparing activated carbon or bio-oil by fast activation or fast pyrolysis of biomass
CN106635084A (en) * 2016-09-14 2017-05-10 重庆大学 Preparation device and method of biomass crucible coke
CN106675660A (en) * 2017-03-15 2017-05-17 张守军 Efficient circulating fluidized bed gasification device and method

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2578337Y (en) * 2002-10-18 2003-10-08 山东理工大学 Biomass pyrolytic liquefier
CN101130698A (en) * 2007-08-15 2008-02-27 胜利油田胜利动力机械有限公司 Method and apparatus for pyrolysis of biomass gas tar oil
CN101144022A (en) * 2007-11-01 2008-03-19 上海交通大学 Three-section type biomass gasifying furnace
CN101781584A (en) * 2010-02-06 2010-07-21 周开根 Method and equipment for gasifying coal by using plasma
JP2016204235A (en) * 2015-04-28 2016-12-08 清水建設株式会社 Gasification apparatus and gas production method
CN106635084A (en) * 2016-09-14 2017-05-10 重庆大学 Preparation device and method of biomass crucible coke
CN106336885A (en) * 2016-10-11 2017-01-18 天津科技大学 System for preparing activated carbon or bio-oil by fast activation or fast pyrolysis of biomass
CN106675660A (en) * 2017-03-15 2017-05-17 张守军 Efficient circulating fluidized bed gasification device and method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
内循环串行流化床生物质催化热解试验研究;叶江明;《动力工程学报》;20120315;第31卷(第3期);第220-226页 *

Also Published As

Publication number Publication date
CN108611109A (en) 2018-10-02

Similar Documents

Publication Publication Date Title
CN109603749B (en) Preparation method and application of modified straw stalk biochar
CN105731752A (en) Method for preparing biochar by carrying out copyrolysis on excess sludge and hazelnut shell
CN102344234B (en) Printing and dyeing sludge pyrolysis treatment device and sludge treatment method
CN112387269A (en) Method for preparing biochar by co-pyrolysis of excess sludge and hazelnut shells and photocatalytic modification method of biochar
CN107364860B (en) A kind of method that efficient cryogenic carbonization prepares straw biological charcoal
CN108144581B (en) Alkali modified pig manure biochar and preparation method and application thereof
CN108611109B (en) Three-section type heating device, and biological carbon preparation system and preparation method
CN102161541A (en) Method for extracting salt from coking desulphurization waste solution and special device thereof
CN109173999A (en) A kind of preparation method and applications of biology carbon microspheres
CN101164877A (en) Biomass double fluidized-bed device for preparing active carbon
CN110302751A (en) Composite biomass charcoal material and preparation method and application thereof
CN112619630A (en) Useless active carbon regeneration system
CN113856630B (en) Straw carbon magnesium lanthanum LDH nano phosphorus adsorption material and preparation method and application thereof
CN110882676A (en) Preparation method and application of magnetic adsorption biochar material
CN107142125A (en) A kind of sludge chemical chain gasification orientation produces synthetic gas method and realizes the device of this method
CN113019323B (en) Ultrasonic activated biochar and preparation method and application thereof
CN113980695A (en) Treatment method of plant biomass for enriching heavy metals
CN114029034A (en) Phosphorus-based biochar adsorbing material, preparation method and application thereof
CN113401900A (en) Process and device for preparing biomass activated carbon and co-producing biomass synthesis gas by physical and chemical coupling activation
CN104910935A (en) Biomass carbon, gas, oil, liquid, heat, electricity poly-generation device and method
CN104192799A (en) Device for preparing hydrogen-rich gas by gasifying biomass under catalysis of high-temperature metallurgical slag particles and method
CN116161658A (en) Bamboo columnar activated carbon and preparation method and application thereof
CN115254018A (en) Biochar prepared from industrial solid waste and wetland biomass and preparation method thereof
CN112808234A (en) Method for preparing multilayer structure charcoal bag by using biological resources and charcoal bag prepared by same
Zeng et al. Effect of iron salt modification on the adsorption of hydrogen sulfide by sludge-based activated carbon

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant