CN215924409U - Device for preparing biomass activated carbon and co-producing biomass synthesis gas through physical and chemical coupling activation - Google Patents
Device for preparing biomass activated carbon and co-producing biomass synthesis gas through physical and chemical coupling activation Download PDFInfo
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- CN215924409U CN215924409U CN202121665205.3U CN202121665205U CN215924409U CN 215924409 U CN215924409 U CN 215924409U CN 202121665205 U CN202121665205 U CN 202121665205U CN 215924409 U CN215924409 U CN 215924409U
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 133
- 239000002028 Biomass Substances 0.000 title claims abstract description 70
- 230000004913 activation Effects 0.000 title claims abstract description 46
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 29
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 29
- 238000012412 chemical coupling Methods 0.000 title claims description 23
- 239000007789 gas Substances 0.000 claims abstract description 186
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 49
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000003860 storage Methods 0.000 claims abstract description 34
- 239000000047 product Substances 0.000 claims abstract description 28
- 239000002994 raw material Substances 0.000 claims abstract description 26
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 17
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 13
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 239000012263 liquid product Substances 0.000 claims abstract description 8
- 230000003213 activating effect Effects 0.000 claims description 35
- 239000003795 chemical substances by application Substances 0.000 claims description 33
- 238000002309 gasification Methods 0.000 claims description 30
- 238000010438 heat treatment Methods 0.000 claims description 25
- 238000005406 washing Methods 0.000 claims description 25
- 239000007788 liquid Substances 0.000 claims description 13
- 238000003763 carbonization Methods 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 6
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 238000005485 electric heating Methods 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 3
- 230000008016 vaporization Effects 0.000 claims 2
- 239000007795 chemical reaction product Substances 0.000 claims 1
- 229910052783 alkali metal Inorganic materials 0.000 abstract description 15
- -1 alkali metal salt Chemical class 0.000 abstract description 15
- 239000012190 activator Substances 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 6
- 238000012546 transfer Methods 0.000 abstract description 5
- 230000008878 coupling Effects 0.000 abstract description 4
- 238000010168 coupling process Methods 0.000 abstract description 4
- 238000005859 coupling reaction Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 2
- 238000003756 stirring Methods 0.000 abstract description 2
- 241000197194 Bulla Species 0.000 abstract 1
- 208000002352 blister Diseases 0.000 abstract 1
- 238000001994 activation Methods 0.000 description 70
- 239000003054 catalyst Substances 0.000 description 18
- 238000004519 manufacturing process Methods 0.000 description 15
- 238000002156 mixing Methods 0.000 description 13
- 239000011148 porous material Substances 0.000 description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 10
- 238000001035 drying Methods 0.000 description 10
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 10
- 150000003839 salts Chemical class 0.000 description 10
- 229910052799 carbon Inorganic materials 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 5
- 229910052808 lithium carbonate Inorganic materials 0.000 description 5
- 230000007935 neutral effect Effects 0.000 description 5
- 229910000027 potassium carbonate Inorganic materials 0.000 description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 description 5
- 238000012512 characterization method Methods 0.000 description 4
- 238000012216 screening Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000000197 pyrolysis Methods 0.000 description 3
- 239000010902 straw Substances 0.000 description 3
- 241000218645 Cedrus Species 0.000 description 2
- 244000050510 Cunninghamia lanceolata Species 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000002154 agricultural waste Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000005539 carbonized material Substances 0.000 description 2
- 238000010000 carbonizing Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000011592 zinc chloride Substances 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- 241000609240 Ambelania acida Species 0.000 description 1
- 235000017060 Arachis glabrata Nutrition 0.000 description 1
- 235000010777 Arachis hypogaea Nutrition 0.000 description 1
- 244000105624 Arachis hypogaea Species 0.000 description 1
- 235000018262 Arachis monticola Nutrition 0.000 description 1
- 241000209128 Bambusa Species 0.000 description 1
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 description 1
- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 240000007049 Juglans regia Species 0.000 description 1
- 235000009496 Juglans regia Nutrition 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003570 air Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000010905 bagasse Substances 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 125000003636 chemical group Chemical group 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 235000010675 chips/crisps Nutrition 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 235000020232 peanut Nutrition 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 235000020234 walnut Nutrition 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
Images
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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- Carbon And Carbon Compounds (AREA)
Abstract
The application discloses device of preparation biomass activated carbon coproduction biomass synthesis gas is activated in physical chemistry coupling, including the nitrogen storage tank, the carbon dioxide storage tank, vapor generating device, integrative reaction unit of carbomorphism activation and gas-liquid product collection device, the inside mixture that contains biomass raw materials and chemical activator of integrative reactor of carbomorphism activation, the inside gas distributor that is provided with of integrative reactor of carbomorphism activation, during biomass raw materials and activator mixture are gone into to the venthole submergence of gas distributor, the gas inlet that the gas that activates by integrative reactor top of carbomorphism gets into gas distributor, gas product gas outlet and gas-liquid product collection device are by the tube coupling. The setting of this application gas distributor improves the contact state of activator and biomass feedstock in the reactor, and the tongue shape water conservancy diversion hole that the active gas passes through gas distributor escapes from the alkali metal salt of molten state with the form of tympanic bulla, plays the stirring effect, strengthens the contact between activator and the carbomorphism material and heat transfer and mass transfer effect.
Description
Technical Field
The utility model relates to the technical field of biomass utilization, in particular to a device for preparing biomass activated carbon coproduction synthesis gas by physical and chemical coupling activation.
Background
The biomass energy is used as the fourth most energy in the world, and has important significance for maintaining the energy structure and safety of human society. Currently, the average biomass energy utilization rate is less than 40%, and most biomass energy is released in a combustion mode, so that how to realize high-efficiency and high-value utilization of biomass energy becomes one of important topics of current research. The preparation of biomass activated carbon and synthesis gas is an important way for realizing high-value utilization of biomass resources.
The activated carbon has the characteristics of developed pore structure, larger specific surface area, abundant surface chemical groups, stronger specific adsorption capacity and the like, and is widely applied to the fields of petrochemical industry, food, medicine, metallurgy, environmental management, energy storage and the like. The common preparation method of the activated carbon comprises the following steps: physical activation, chemical activation, and physical-chemical coupling activation. The commonly used activated gas of the physical activation method is water vapor, carbon dioxide, air, flue gas and the like, the activation process is simple, the environmental pollution is small, but the activation time is long, the temperature is high, and the energy consumption is large. The activating agents commonly used in the chemical activation method comprise potassium hydroxide, phosphoric acid, zinc chloride, potassium carbonate and the like, the activation temperature is low, the activation time is short, the yield of the activated carbon is high, the specific surface area is large, but most of chemical activating agents have corrosion behavior on equipment and are not environment-friendly. The biomass synthesis gas can be used as chemical raw material or fuel, and the main component of the biomass synthesis gas is H2And CO, typically to produce synthesis gas by pyrolysis of the gasified biomass. Pyrolysis is the decomposition reaction of organic matter in biomass under the action of heat to produce gas. Gasification uses air, steam and the like as gasifying agents, and biomass is converted into synthesis gas through thermochemical reaction under high temperature conditions. The preparation technology of the synthesis gas has the difficulties of low grade of gas products, tar removal and the like.
Chinese patent (publication No. CN102417179A) discloses that peanut shells are used as biomass raw materials, potassium hydroxide and sodium hydroxide are used as activating agents to prepare a biomass with a specific surface area of 990-1277 m2The Chinese patent CN201711481483.1 discloses a preparation method of activated carbon with controllable specific surface area for a super capacitor, which comprises the steps of carbonizing raw materials at 700 ℃ for 23-25 hours, and then activating the raw materials at 1180-1250 ℃ for 11-13 hours by using water vapor as an activating agent to prepare the activated carbon with the specific surface area of 2000-2200 m2Per g of super activated carbon. Chinese patent (CN201811203217.7) discloses a 'downdraft straw carbonized carbon gas co-production device and a production method thereof', wherein the feeding amount of chip straw raw materials is 1.1t/h, the carbon yield is 308kg/h, and the biomass gas yield is 1764Nm3H is used as the reference value. Chinese patent (CN201410571477.5) discloses a carbon and gas co-production treatment method of garbage and production line equipment thereof, combustible gas generated in the production process is used for tail gas treatment, and the generated garbage carbon is used as power generation fuel.
SUMMERY OF THE UTILITY MODEL
Aiming at the problems of low multi-stage utilization rate of biomass, environmental-friendliness in the production process and the like in the existing biomass utilization technology, the utility model aims to provide a device for preparing biomass activated carbon through physical and chemical coupling activation in a co-production mode, when the device is used for preparing the biomass activated carbon, the corrosion of a chemical activating agent to equipment can be reduced, the contact of a biomass raw material with activated gas and the chemical activating agent is effectively increased, the pore size distribution and the specific surface area of an activated carbon product and the composition of the gas product can be adjusted by changing the types and the proportions of the activated gas and the chemical activating agent, and the efficient and high-value utilization of the biomass raw material is realized through carbon and gas co-production. The addition of the related catalyst can reduce the generation of tar so as to improve the quality of the activated carbon and the synthesis gas.
The device for preparing the biomass activated carbon coproduction synthesis gas by physical and chemical coupling activation is characterized by comprising a nitrogen storage tank, a carbon dioxide storage tank, a water vapor generating device, a carbonization-activation integrated device and a gas product collecting device; the carbonization-activation integrated reaction device comprises an electric heating furnace, a carbonization-activation integrated reactor and a thermocouple, a biomass raw material and activator mixture is contained in the carbonization-activation integrated reactor, a gas inlet, a thermocouple jack and a gas product outlet are arranged at the top of the carbonization-activation integrated reactor, the temperature measuring end of the thermocouple penetrates through the thermocouple jack and extends into the carbonization-activation integrated reactor to measure the temperature, a gas distributor is arranged in the carbonization-activation integrated reactor, a gas outlet of the gas distributor is immersed in the biomass raw material and activator mixture, activated gas enters the gas distributor from the gas inlet at the top of the carbonization-activation integrated reactor, and the gas product outlet is connected with a gas product collecting device through a pipeline;
wherein, gas distributor includes intake pipe, gaseous surge chamber and a plurality of square branch pipe, the intake pipe sets up the top at gaseous surge chamber, and a plurality of square branch pipes evenly set up in the bottom of gaseous surge chamber, and the upper end of intake pipe is connected with the gaseous air inlet at the integrative reactor top of carbomorphism activation, and the lower extreme of square branch pipe evenly sets up a plurality of gaseous tongue shape water conservancy diversion holes, and the opening upper end outside in tongue shape water conservancy diversion hole is provided with the tongue piece of downward sloping, and the tongue piece is 15~25 with the contained angle on square branch pipe surface.
Further, gaseous surge chamber includes cylindrical cavity and sets up in the annular chamber of cylindrical cavity outside, through 3 at least pipeline cavity intercommunications between cylindrical cavity and the annular chamber, the intake pipe sets up at the cylindrical cavity top of gaseous surge chamber, and cylindrical cavity bottom and annular chamber bottom all evenly set up a plurality of square branch pipes.
The device for preparing the biomass activated carbon coproduction synthesis gas through physical and chemical coupling activation is characterized in that the water vapor generating device comprises a water storage tank, a water pump, a gasification chamber heating furnace and a heating belt, wherein the gasification chamber heating furnace is used for heating and warming the gasification chamber, the gasification chamber is provided with a liquid inlet, a gas inlet and a gas outlet, gas outlets of the nitrogen storage tank and the carbon dioxide storage tank are connected with the gas inlet of the gasification chamber through pipelines, the water pump is used for conveying water in the water storage tank into the gasification chamber, and the gas outlet of the gasification chamber is connected with a gas inlet at the top of the carbonization and activation integrated reactor through a pipeline; wherein, the heating belt is coated on the pipeline between the gas outlet of the gasification chamber and the gas inlet of the carbonization-activation integrated reactor.
The device for preparing the biomass activated carbon coproduction synthesis gas by virtue of carbonization-activation coupling is characterized in that the gas-liquid product collecting device comprises a condenser, a liquid storage tank, a low-temperature circulating cooling pump, a gas washing tank and a gas collecting tank; a gas product gas outlet at the top of the carbonization-activation integrated reactor is connected with a gas inlet at the bottom of the condenser through a pipeline, gas discharged from the gas outlet at the top of the condenser is introduced into a gas washing tank through the pipeline, and a gas outlet of the gas washing tank is connected with a gas collecting groove through the pipeline; a condensing jacket is arranged outside the condenser, and an inlet and an outlet of the condensing jacket are respectively connected with an outlet and an inlet of the low-temperature circulating cooling pump through pipelines to form a condensed fluid loop; the liquid formed by condensation in the condenser is collected in a liquid storage tank.
The beneficial effects obtained by the utility model are as follows:
1. the biomass activated carbon is prepared by a physical-chemical coupling activation method, so that the activation temperature is reduced, the activation time is shortened, and the production cost is reduced. The specific surface area, the pore volume and the pore size distribution of the activated carbon are regulated and controlled by changing the type of the activated gas, the type and the proportion of the catalyst and the alkali metal salt.
2. The alkali metal salt added with the catalyst is used as a heat medium and an activating agent, and metal ions in the molten alkali metal salt permeate into biomass particles in the activation process, so that the heat and mass transfer rate in the biomass is increased, the activation time is obviously shortened, and the activation temperature is reduced. The catalyst can change the pyrolysis gasification process of the biomass raw material, can effectively reduce the generation of byproduct tar, and is beneficial to improving the quality of the activated carbon and the synthesis gas.
3. The arrangement of the gas distributor improves the contact state of the activating agent and the biomass raw material in the reactor and increases the contact probability of the activating agent and the carbonized material. The activating gas escapes from the alkali metal salt in a molten state in a bubbling mode through the tongue-shaped diversion holes which are formed downwards, so that the stirring effect is achieved, and the contact between the activating agent and the carbonized material and the heat transfer and mass transfer effects are enhanced.
4. The biomass activated carbon and the synthesis gas are co-produced through preparation, so that the multi-stage utilization of biomass resources and the diversification and high-valued of biomass products are realized, and the method has important significance for assisting in realizing the aims of carbon peak reaching and carbon neutralization.
Drawings
FIG. 1 is a schematic structural diagram of a production apparatus for preparing biomass activated carbon according to the present invention;
FIG. 2 is a cross-sectional view of a carbonization-activation integrated reactor of the present invention;
FIG. 3 is a front view of the gas distributor of the present invention;
FIG. 4 is a top view of a gas distributor of the present invention;
in fig. 1: 1-a nitrogen storage tank; 2-a carbon dioxide storage tank; 3-a pressure reducing valve; 4-a flow meter; 5-a water storage tank; 6, a water pump; 7-a gasification chamber; 8-a gasification chamber furnace; 9-heating a belt; 10-an electric heating furnace; 11-carbonization-activation integrated reactor; 12-a gas distributor; 13-a thermocouple; 14-a condenser; 15-a liquid storage tank; 16-a cryogenic circulating cooling pump; 17-a scrubber tank; 18-a gas collecting tank;
in fig. 2: 1101-gas inlet; 1102-thermocouple insertion holes; 1103-gas product outlet.
In fig. 3 and 4: 1201-intake pipe; 1202-gas buffer chamber; 1203-square manifold; 1204-tongue deflector hole.
Detailed Description
The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the utility model.
Example (b): compare FIGS. 1 to 4
A process for preparing biomass activated carbon and coproducing synthesis gas by physical and chemical coupling activation comprises the following steps:
and washing the crushed biomass raw material with water to remove impurities, and drying for later use. Uniformly mixing the treated biomass raw material with a chemical activating agent, putting the mixture into a carbonization and activation integrated reactor, and carbonizing the material in a nitrogen atmosphere. And after carbonization, keeping the temperature in the carbonization-activation integrated reactor at the activation temperature, and introducing activated gas to activate the raw material. And cooling to room temperature after activation is finished, taking out a product from an activating agent to obtain crude activated carbon, washing the crude activated carbon with water, dissolving most of the activating agent on the surface of the crude activated carbon in water, washing with 1mol/L hydrochloric acid solution to remove redundant activating agent and ash, washing with deionized water to be neutral, and drying to obtain a finished product.
The biomass raw material is any one or the combination of two of agricultural wastes and forestry wastes; the agricultural waste is at least one of crop straws, bagasse and rice husks, and the forestry waste is at least one of wood chips, bamboos, walnut shells and coconut shells; the activating gas is one or two mixed gases of water vapor and carbon dioxide.
The alkali metal salt is prepared from the following components in a mass ratio of 30-35: 30-35: and 32-38 of ternary mixed salt of lithium carbonate, sodium carbonate and potassium carbonate, wherein the ternary mixed salt is in a molten state in the process of preparing the activated carbon coproduction synthesis gas. The catalyst is Fe2O3、Fe3O4、FeCl3、TiO2、Co2O3、CoCl2、Cr2O3、MgO、ZnCl2The mass ratio of the catalyst to the alkali metal salt is 0.02-0.1: 1, preferably 0.02-0.06: 1.
The mass ratio of the biomass raw material to the chemical activating agent is 0.5-2: 20, preferably 1: 20.
The nitrogen flow rate is 0.1 to 1L/min, preferably 0.3 to 0.5L/min.
The temperature is 500-900 deg.C, and the activated gas is preferably 650-850 deg.C.
The time for the physicochemical coupling activation is 0.5 to 5 hours, preferably 1 to 1.5 hours.
The mass ratio of the introduced activated gas to the biomass raw material is 0.5-2: 1, preferably 0.8-1.2: 1.
A device for preparing biomass activated carbon coproduction synthesis gas by physical and chemical coupling activation comprises a nitrogen storage tank 1, a carbon dioxide storage tank 2, a water vapor generation device, a carbonization and activation integrated device and a gas-liquid product collection device; the integrated carbonization-activation device comprises an electric heating furnace 10, an integrated carbonization-activation reactor 11 and a thermocouple 13, a biomass raw material and an activating agent mixture are contained inside the integrated carbonization-activation reactor 11, a gas inlet 1101, a thermocouple jack 1102 and a gas product gas outlet 1103 are arranged at the top of the integrated carbonization-activation reactor 11, the temperature measuring end of the thermocouple 13 penetrates through the thermocouple jack 1201 to extend into the integrated carbonization-activation reactor 11 for measuring the temperature, a gas distributor 12 is arranged inside the integrated carbonization-activation reactor 11, the gas outlet of the gas distributor 12 is immersed into the biomass raw material and the activating agent mixture, activated gas enters the gas distributor 12 from the gas inlet 1101 at the top of the integrated carbonization-activation reactor, and the gas product gas outlet 1103 is connected with a gas-liquid product collecting device through a pipeline.
The gas distributor 12 comprises a gas inlet pipe 1201, a gas buffer chamber 1202 and a plurality of square branch pipes 1203, the gas inlet pipe 1201 is arranged at the top of the gas buffer chamber 1202, the square branch pipes 1203 are uniformly arranged at the bottom of the gas buffer chamber 1202, the upper end of the gas inlet pipe 1201 is connected with a gas inlet 1101 at the top of the carbonization-activation integrated reactor 11, a plurality of uniform tongue-shaped guide holes 1204 are formed in the lower end of the square branch pipe 1203, a tongue piece which is inclined downwards is arranged on the outer side of the upper end of an opening of the tongue-shaped guide hole 1204, and the included angle between the tongue piece and the surface of the square branch pipe 1203 is 15-25 degrees.
The gas buffer chamber 1202 comprises a cylindrical chamber and an annular chamber arranged outside the cylindrical chamber, the cylindrical chamber is communicated with the annular chamber through at least 3 pipeline chambers, the gas inlet pipe 1201 is arranged at the top of the cylindrical chamber of the gas buffer chamber 1202, and a plurality of square branch pipes 1203 are uniformly arranged at the bottom of the cylindrical chamber and the bottom of the annular chamber. In the comparison of fig. 4, the bottom of the cylindrical chamber is provided with 4 square pipe branches 1203, and the bottom of the annular chamber is provided with 6 square pipe branches 1203.
The water vapor generating device comprises a water storage tank 5, a water pump 6, a gasification chamber 7, a gasification chamber heating furnace 8 and a heating belt 9, wherein the gasification chamber heating furnace 8 is used for heating the gasification chamber 7, the gasification chamber 7 is provided with a liquid inlet, a gas inlet and a gas outlet, gas outlets of the nitrogen storage tank 1 and the carbon dioxide storage tank 2 are connected with the gas inlet of the gasification chamber 7 through pipelines, the water pump 6 is used for conveying water in the water storage tank 5 into the gasification chamber 7, and the gas outlet of the gasification chamber 7 is connected with a gas inlet 1101 at the top of the carbonization and activation integrated reactor 11 through a pipeline; wherein, the heating band 9 is coated on the pipeline between the gas outlet of the gasification chamber 7 and the gas inlet 1101. Wherein the temperature of the gasification chamber is 200-400 ℃, preferably 200-250 ℃.
The gas-liquid product collecting device comprises a condenser 14, a liquid storage tank 15, a condensation circulating pump 16, a gas washing tank 17 and a gas collecting tank 18; a gas product gas outlet 1103 at the top of the carbonization-activation integrated reactor 11 is connected with a gas inlet at the bottom of the condenser 14 through a pipeline, gas discharged from a gas outlet at the top of the condenser 14 is introduced into a gas washing tank 17 through a pipeline, and a gas outlet of the gas washing tank 17 is connected with a gas collecting tank 18 through a pipeline; a condensing jacket is arranged on the outer side of the condenser 14, and an inlet and an outlet of the condensing jacket are respectively connected with an outlet and an inlet of a condensing circulating pump 16 through pipelines to form a condensed fluid loop; the liquid formed by condensation in the condenser 14 is collected in a liquid storage tank 15.
In the comparison graph 1, a nitrogen storage tank 1 and a carbon dioxide storage tank 2 are both provided with a pressure reducing valve 3, the gas outlets of the nitrogen storage tank 1 and the carbon dioxide storage tank 2 are respectively connected to a main gas inlet pipe through branch pipes, a flow meter 4 is arranged on the main gas inlet pipe, and the outlet of the main gas inlet pipe is connected with the gas inlet of a gasification chamber 7.
Example 1:
a process for preparing biomass activated carbon and coproducing synthesis gas by physical and chemical coupling activation (by adopting a device shown in figure 1) comprises the following steps:
1) screening 10 g of cedar chips by using a screen of 80-100 meshes as a raw material, washing with water, drying, uniformly mixing with a chemical activating agent, putting into a reactor with the nitrogen flow of 0.3L/min, heating to carbonize, raising the temperature of the reactor from room temperature to 600 ℃ at the heating rate of 10 ℃/min, and keeping the constant temperature for 1.5 h.
2) After the carbonization treatment is finished, the temperature of the carbonization-activation integrated reactor is raised to 650 ℃ at the heating rate of 10 ℃/min, the introduction of nitrogen is stopped, water vapor with the mass flow of 10 g/h is introduced into the reactor, and the physical-chemical coupling activation treatment is carried out for 0.5 h. Wherein the total amount of the chemical activating agent is 200 g, and the chemical activating agent is formed by mixing a catalyst and an alkali metal salt according to the mass ratio of 0.02: 1. The alkali metal salt is a mixed salt of lithium carbonate, sodium carbonate and potassium carbonate in a mass ratio of 3:3:4, and the catalyst is Fe in a mass ratio of 2:12O3And Co2O3And (3) mixing the catalyst.
3) And after the reaction in the step 2), washing the activated crude activated carbon by using deionized water and 1mol/L hydrochloric acid solution in sequence to remove salt and ash in the activated crude activated carbon, washing the activated crude activated carbon by using deionized water to be neutral, and drying to obtain an activated carbon finished product, wherein the yield of the activated carbon is 11.4%. The BET specific surface area of the activated carbon product is 575.99 m by characterization2The pore volume is 0.3839 mL/g, the average pore diameter is 2.44 nm, and the micropore volume accounts for 74.77%.
Example 2:
a process for preparing biomass activated carbon and coproducing synthesis gas by physical and chemical coupling activation (by adopting a device shown in figure 1) comprises the following steps:
1) screening 10 g of cedar chips by using a 80-100-mesh screen as a raw material, washing with water, drying, uniformly mixing with an activating agent, putting into a carbonization-activation integrated reactor, heating the temperature of the reactor from room temperature to 650 ℃ at a heating rate of 10 ℃/min, and keeping for 0.5 h.
2) Introducing water vapor with the mass flow of 10 g/h into the carbonization-activation integrated reactor at 650 ℃, and carrying out physical-chemical coupling activation treatment for 0.5 h. Wherein the total amount of the activating agent is 200 g, and the activating agent is formed by mixing a catalyst and an alkali metal salt according to the mass ratio of 0.02: 1. The alkali metal salt is prepared from 3:3:4 mass ratio of lithium carbonate, sodium carbonate and carbonic acidPotassium mixed salt, and the catalyst is Fe with the mass ratio of 2:12O3And Co2O3And (3) mixing the catalyst.
3) And 2) after the reaction in the step 2), washing the activated crude activated carbon by using deionized water and 1mol/L hydrochloric acid solution in sequence to remove salt and ash in the activated crude activated carbon, washing the activated crude activated carbon by using deionized water to be neutral, and drying the activated crude activated carbon to obtain an activated carbon finished product, wherein the yield of the activated carbon is 13.1%. The BET specific surface area of the comparative product is 555.16 m by characterization2The pore volume was 0.3024 mL/g, the average pore diameter was 2.56 nm, and the micropore volume was 70.23%.
Example 3:
a process for preparing biomass activated carbon and coproducing synthesis gas by physical and chemical coupling activation (by adopting a device shown in figure 1) comprises the following steps:
1) screening 10 g of China fir sawdust by using a 80-100-mesh screen as a raw material, washing with water, drying, uniformly mixing with an activating agent, and putting into a carbonization-activation integrated reactor with the nitrogen flow of 0.3L/min for heating and carbonization. The reactor temperature was raised from room temperature to 600 ℃ at a ramp rate of 10 ℃/min and then held at constant temperature for 1.5 h.
2) After the carbonization treatment is finished, the temperature of the carbonization-activation integrated reactor is raised to 700 ℃ at the heating rate of 10 ℃/min, the introduction of nitrogen is stopped, water vapor with the mass flow of 10 g/h is introduced into the reactor, and the physical-chemical coupling activation treatment is carried out for 1.5 h. Wherein the total amount of the activating agent is 200 g, and the activating agent is formed by mixing a catalyst and an alkali metal salt according to the mass ratio of 0.1: 1. The alkali metal salt is a mixed salt of lithium carbonate, sodium carbonate and potassium carbonate in a mass ratio of 3:3:4, and the catalyst is Fe in a mass ratio of 2:12O3And Co2O3And (3) mixing the catalyst.
3) After the reaction is finished, washing the activated crude activated carbon by using ionized water and 1mol/L hydrochloric acid solution in sequence to remove salt and ash in the activated crude activated carbon, washing the activated crude activated carbon by using the ionized water to be neutral, and drying the activated crude activated carbon to obtain an activated carbon finished product, wherein the yield of the activated carbon is 9.3%. The BET specific surface area of the activated carbon product is 1049.40 m by characterization2Per g, pore volume0.7535 mL/g, average pore diameter of 2.83 nm, and micropore volume ratio of 69.38%.
Example 4:
a process for preparing biomass activated carbon and coproducing synthesis gas by physical and chemical coupling activation (by adopting a device shown in figure 1) comprises the following steps:
1) screening 10 g of China fir sawdust by using a 80-100-mesh screen as a raw material, washing with water, drying, uniformly mixing with an activating agent, and putting into a carbonization-activation integrated reactor with the nitrogen flow of 0.3L/min for heating and carbonization. The temperature of the carbonization-activation integrated reactor is raised from room temperature to 600 ℃ at the temperature raising rate of 10 ℃/min, and then the temperature is kept constant for 1.5 h.
2) After the carbonization treatment is finished, the temperature of the carbonization-activation integrated reactor is raised to 700 ℃ at the heating rate of 10 ℃/min, the introduction of nitrogen is stopped, water vapor with the mass flow of 10 g/h is introduced into the carbonization-activation integrated reactor, and the physical-chemical coupling activation treatment is carried out for 1.5 h. Wherein the total amount of the activating agent is 200 g, and the activating agent is formed by mixing a catalyst and an alkali metal salt according to the mass ratio of 0.05: 1. The alkali metal salt is a mixed salt of lithium carbonate, sodium carbonate and potassium carbonate in a mass ratio of 3:3:4, and the catalyst is Fe in a mass ratio of 2:12O3And Co2O3And (3) mixing the catalyst.
3) After the reaction is finished, washing the activated crude activated carbon by using ionized water and 1mol/L hydrochloric acid solution in sequence to remove salt and ash in the activated crude activated carbon, washing the activated crude activated carbon by using the ionized water to be neutral, and drying the activated crude activated carbon to obtain an activated carbon finished product, wherein the yield of the activated carbon is 10.1%. The BET specific surface area of the comparative product is 821.08 m by characterization2The pore volume is 0.5222 mL/g, the average pore diameter is 3.03nm, and the micropore volume accounts for 68.31%.
The main components of the synthesis gas collected in examples 1 to 4 are shown in Table 1, and the main component of the synthesis gas is H2、CO、CH4、CO2Four gases, the balance being impurity gases.
The statements in this specification merely set forth a list of implementations of the inventive concepts, and the scope of the present disclosure should not be construed as limited to the particular forms set forth in the examples.
Claims (5)
1. A device for preparing biomass activated carbon and co-producing biomass synthesis gas by physical and chemical coupling activation is characterized by comprising a nitrogen storage tank (1), a carbon dioxide storage tank (2), a water vapor generating device, a carbonization-activation integrated reaction device and a gas-liquid product collecting device; the carbonization-activation integrated reaction device comprises an electric heating furnace (10), a carbonization-activation integrated reactor (11) and a thermocouple (13), a mixture of a biomass raw material and a chemical activating agent is contained in the carbonization-activation integrated reactor (11), a gas inlet (1101), a thermocouple jack (1102) and a gas product gas outlet (1103) are arranged at the top of the carbonization-activation integrated reactor (11), the temperature measuring end of the thermocouple (13) penetrates through the thermocouple jack (1102) to stretch into the reaction product of the carbonization-activation integrated reactor (11) for measuring the temperature, a gas distributor (12) is arranged in the carbonization-activation integrated reactor (11), the gas outlet of the gas distributor (12) is immersed into the mixture of the biomass raw material and the activating agent, and activated gas enters the gas distributor (12) from the gas inlet (1101) at the top of the carbonization-activation integrated reactor (11), the gas product gas outlet (1103) is connected with a gas-liquid product collecting device through a pipeline.
2. The device for preparing biomass activated carbon and co-producing biomass synthesis gas by physical and chemical coupling activation as claimed in claim 1, it is characterized in that the water vapor generating device comprises a water storage tank (5), a water pump (6), a vaporizing chamber (7), a vaporizing chamber heating furnace (8) and a heating belt (9), the gasification chamber heating furnace (8) is used for heating the gasification chamber (7), the gasification chamber (7) is provided with a liquid inlet, a gas inlet and a gas outlet, the gas outlets of the nitrogen storage tank (1) and the carbon dioxide storage tank (2) are connected with a gas inlet of the gasification chamber (7) through pipelines, the water pump (6) is used for conveying water in the water storage tank (5) into the gasification chamber (7), and a gas outlet of the gasification chamber (7) is connected with a gas inlet (1101) at the top of the carbonization-activation integrated reactor (11) through a pipeline; wherein, the pipeline between the gas outlet of the gasification chamber (7) and the gas inlet (1101) is coated with the heating belt (9).
3. The device for preparing the biomass activated carbon and co-producing the biomass synthesis gas by the physical and chemical coupling activation as claimed in claim 1, wherein the gas product collecting device comprises a condenser (14), a liquid storage tank (15), a low-temperature circulating cooling pump (16), a gas washing tank (17) and a gas collecting tank (18); a gas product gas outlet (1103) at the top of the carbonization-activation integrated reactor (11) is connected with a gas inlet at the bottom of a condenser (14) through a pipeline, gas discharged from a gas outlet at the top of the condenser (14) is introduced into a gas washing tank (17) through a pipeline, and a gas outlet of the gas washing tank (17) is connected with a gas collecting tank (18) through a pipeline; a condensing jacket is arranged on the outer side of the condenser (14), and an inlet and an outlet of the condensing jacket are respectively connected with an outlet and an inlet of the low-temperature circulating cooling pump (16) through pipelines to form a condensed fluid loop; the liquid formed by condensation in the condenser (14) is collected in a liquid storage tank (15).
4. The device for preparing the biomass activated carbon and co-producing the biomass syngas through the physical and chemical coupling activation as claimed in claim 1, wherein the gas distributor (12) comprises a gas inlet pipe (1201), a gas buffer chamber (1202) and a plurality of square branch pipes (1203), the gas inlet pipe (1201) is arranged at the top of the gas buffer chamber (1202), the square branch pipes (1203) are uniformly arranged at the bottom of the gas buffer chamber (1202), the upper end of the gas inlet pipe (1201) is connected with a gas inlet (1101) at the top of the carbonization and activation integrated reactor (11), the lower end of each square branch pipe (1203) is uniformly provided with a plurality of tongue-shaped guide holes (1204), the outer side of the upper end of each opening of each tongue-shaped guide hole (1204) is provided with a downward-inclined tongue piece, and the included angle between each tongue piece and the surface of each square branch pipe (1203) is 15-25 °.
5. The device for preparing the biomass activated carbon and co-producing the biomass synthesis gas by the physical and chemical coupling activation as claimed in claim 4, wherein the gas buffer chamber (1202) comprises a cylindrical chamber and an annular chamber arranged outside the cylindrical chamber, the cylindrical chamber is communicated with the annular chamber through at least 3 pipeline chambers, the gas inlet pipe (1201) is arranged at the top of the cylindrical chamber of the gas buffer chamber (1202), and a plurality of square branch pipes (1203) are uniformly arranged at the bottom of the cylindrical chamber and the bottom of the annular chamber.
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| CN113401900B (en) * | 2021-07-21 | 2023-10-24 | 浙江工业大学 | Technology and device for preparing biomass activated carbon and co-producing biomass synthetic gas through physical and chemical coupling activation |
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