CN109437191A - A kind of " press pump " coupling microwaves quickly prepare the apparatus and method of high yield active carbon - Google Patents
A kind of " press pump " coupling microwaves quickly prepare the apparatus and method of high yield active carbon Download PDFInfo
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- CN109437191A CN109437191A CN201811462642.8A CN201811462642A CN109437191A CN 109437191 A CN109437191 A CN 109437191A CN 201811462642 A CN201811462642 A CN 201811462642A CN 109437191 A CN109437191 A CN 109437191A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/39—Apparatus for the preparation thereof
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Abstract
The invention belongs to carbon material preparation technical field, a kind of " press pump " coupling microwaves quickly prepare the apparatus and method of high yield active carbon.Device includes program mode controller, feeder unit, reacting furnace, pump unit, microwave heating unit, produce an unexpected winner unit and pyrolysis gas processing unit.The present invention causes raw molecule friction and collision to reduce reaction activity using microwave, greatly shortens processing operation time.The residence time of the pressure extending volatile matter of " press pump ", it is promoted to be deposited on half carbon surface and improve solid-state charcoal yield；Pressurization also promotes tar itself polycondensation reaction, is greatly lowered or avoids the generation of tar.Furthermore, microwave heating is conducive to generate pyrolysis gas inside raw material, pyrolysis gas molecule is trapped in inside raw molecule under pressurization, play the role of " self-template in situ ", and omnidirectional freedom " shuttle " significantly promotes the aperture of active carbon to develop inside raw material, instantaneously " puffed rice " effect is conducive to the secondary pore-creating of pyrolysis gas, improves carbon material specific surface area.
Description
Technical field
The present invention relates to the apparatus and method that one kind " press pump " coupling microwaves quickly prepare high yield active carbon, have heating
Speed is fast, active carbon yield is high, nearly zero tar emission and the characteristics of continuous production, belongs to carbon material preparation technical field.
Background technique
Active carbon is widely used in absorption, catalysis, storage due to its aperture structure abundant and good chemical stability
The fields such as energy, hydrogen storage, decoloration.Currently, common active charcoal preparing process furnace body includes: stationary furnace, fluidized bed, rotary furnace and drum
Steep bed etc..Sargassum horneri is prepared as Chinese patent literature CN108298535A discloses a kind of rotary atmosphere furnace physical activation method of utilization
The method of base mesopore activated carbon；Chinese patent literature CN108821282A discloses a kind of modified Sha of utilization Muffle furnace preparation shrimp chaff
The method of the careless nitrogenous active carbon of Ke Jigao；Chinese patent literature CN108249435A discloses a kind of various closed stoves of utilization
Body, the method for preparing petroleum coke base mesopore activated carbon including batch-type furnace, vacuum drying oven, rotary furnace, roller furnace, pusher furnace, tube furnace.
These furnace bodies are all made of traditional resistance partition heating method, and heat is internally gradually transmitted from material surface, therefore there are energy
Measure heat and mass transfer characteristic is poor, heat consume greatly, temperature distributing disproportionation (high outside and low outside) and technique the problems such as time-consuming.
Microwave activation pyrolysis is one of the effective way to solve the above problems.Microwave can be directly entered inside raw material and raw material
Molecular action causes internal friction by chemical bond polarization and molecular rearrangement, to be thermal energy by electromagnetic energy, has whole
It is evenly heated, the features such as temperature gradient is small, heating speed is fast.Chinese patent literature CN106241805A discloses a kind of using micro-
Wave heating activation coupling carbon dioxide catalysis prepares black liquid crude extract-lignosulfonates matrix activated carbon method；In
State patent document CN106608622A discloses preprocessed, microwave carbonization, crushing, dipping, activation, eventually a series of works such as processing
The method that skill process prepares superhigh specific surface area Chinese hemp stalk active carbon.Though these traditional microwave heatings solve resistance and add
Hot mass transfer speed is slow and technique the problem of time-consuming, but can generate a large amount of tar in the charing of practical microwave or activation process.
On the one hand the generation of tar is easy blocking pipeline or attaches to furnace body surface, influence pipeline air exhaust water or furnace body heat transfer；On the other hand
Since biomass pyrolysis product is three kinds of forms of gas, liquid, solid, a large amount of generate of tar also reduces obtaining for solid product active carbon
Rate seriously constrains the large-scale promotion of microwave activation industrially.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides one kind " press pump " coupling microwaves and quickly prepares high yield active carbon
Apparatus and method.
Technical solution of the present invention:
A kind of " press pump " coupling microwaves quickly prepare the device of high yield active carbon, including program mode controller 1, give material list
Member 2, reacting furnace 3, " press pump " unit 4, microwave heating unit 5, produce an unexpected winner unit 6 and pyrolysis gas processing unit 7；
The feeder unit 2 is equipped with storage bin 8 and feeder 9, and the two is connected, the charging of feeder 9 and reacting furnace 3
Valve 10 is connected；
The reacting furnace 3 is equipped with inlet valve 10, intake valve 11, safety valve 12, circumferentially rotates device 13, temperature element
14, load cell 15 and pulsed discharge device 16；Inlet valve 10 and intake valve 11 are located at the arrival end of reacting furnace 3, safety valve
12 are located inside reacting furnace 3；The output signal linker formula controller 1 of temperature element 14 and load cell 15；It circumferentially rotates
Device 13 is located at the outlet end of reacting furnace 3, passes through 24 phase of hot product inlet valve of pulsed discharge device 16 and the unit 6 that produces an unexpected winner
Even；
Described " press pump " unit 4 is equipped with air accumulator 17, pressure and flow controller 18 and pressurizing device 19；On air accumulator 17
Equipped with pressure and flow controller 18, it is connected by pressurizing device 19 with the intake valve 11 of reacting furnace 3；
The microwave heating unit 5 is equipped with microwave generator 20, timing-power control member 21, overheat protector 22
With closed shield layer 23, microwave generator 20 is arranged in 3 inner wall of reacting furnace, is protected by overheat protector 22；Periodically-function
Rate control element 21 is fixed on 5 outer wall of reacting furnace；Periodically-power control member 21, overheat protector 22 and program mode controller 1
It is connected；
The unit 6 that produces an unexpected winner is equipped with hot product inlet valve 24, product collecting pit 25, protection gas unit 26, discharge valve 27
With pyrolysis gas exhaust valve 28, the main body for the unit 6 that produces an unexpected winner is product collecting pit 25, and arrival end is equipped with hot product inlet valve 24,
Outlet end is equipped with the pyrolysis gas exhaust valve 28 being connected with pyrolysis gas processing unit 7；Discharge valve 27 is arranged at 25 bottom of product collecting pit
Portion；Protection gas unit 26 provides protection gas for the unit 6 that produces an unexpected winner.
A kind of method that " press pump " coupling microwaves quickly prepare high yield active carbon, steps are as follows:
(1) the feed pressurization stage:
Solid waste biomass in storage bin 8, which is transported to activator by the inlet valve 10 of feeder 9 and reacting furnace 3, reacts
Furnace center；After the completion of charging, the pressure and flow controller 18 for adjusting " press pump " unit 4 arrives certain flow rate, utilizes pressurizing device 19
Reaction under high pressure gas is passed into reacting furnace 3 with the intake valve 11 of reacting furnace 3, i.e. the pressure period；Charging is kept in pressure process
Valve 10 circumferentially rotates device 13 and the closing of pulsed discharge device 16；Regulated and controled instead by load cell 15 and program mode controller 1
Answer 3 mesohigh pressure of furnace to target value；The setting of safety valve 12 is to guarantee that pressure is receivable in burner hearth material in reacting furnace 3
In range, when pressure is more than regulation safety limit in burner hearth, safety valve 12 be would automatically turn on, and overpressure in furnace body is discharged,
Guarantee that safe preparation process carries out；
The solid waste biomass include waste and old wood corner material, agriculture waste stalk, excess sludge of municipal sewage plant,
Aquatic giantreed, Technical furfural slag etc.；
The activator includes KOH, NaOH, Na2CO3、K2CO3、H3PO4、ZnCl2Deng；
The activator and material quality ratio is 0:1~5:1；
The gas-pressurized can be helium, argon gas, nitrogen etc.；
100~the 1000ml/min of pressure process induction air flow ratio；
The pressure period pressure codomain range are as follows: 0.5~20MPa.
(2) microwave activation stage:
After completing pressurized operation in reacting furnace 3, starting circumferentially rotates device 13 and 5 microwave of microwave heating unit occurs
Device 20 jointly controls activation power and activation time by timing-power control member 21 and program mode controller 1；Pass through survey
Activation temperature in warm 14 real-time testing reacting furnace 3 of element, when temperature is more than temperature limit in reacting furnace 3, overheat protector 22
It will start and block microwave heating, automatically to ensure that microwave activation stage carries out safely；The effect of closed shield layer 23 is isolation
Microwave radiation and external environment guarantee operator's safety；In entire microwave activation stage pulsed discharge device 16 and produce an unexpected winner
The hot product inlet valve 24 of unit 6 remains turned-off；
The microwave heating can be using single-stage heating or multistage more gradient-heateds；
The microwave heating time is 300s~1200s；
The microwave heating power is 400W~900W；
(3) it produces an unexpected winner the stage:
It is acted on using protection gas unit 26 so that product collecting pit 25 is filled with certain density inert gas shielding gas, gas
Body pressure will be far below air pressure in reacting furnace 3；After the completion of microwave activation stage, pass through pulsed discharge device 16 and hot product
Inlet valve 24 quick-fried is sprayed onto product collecting pit 25, hot product instantaneous temperature reduction, hot product under atmosphere of inert gases for thermal material is instantaneous
Second reaming is played the role of in intramolecular gas abrupt release.The stage holding discharge valve 27 that produces an unexpected winner is closed until product is cooled to
Room temperature, discharging obtain ultimate absorbent charcoal material.
The inertia protection gas can be helium, argon gas, nitrogen etc.；
Inertia protection atmospheric pressure is 0~1Mpa in the product collecting pit 25.
Compared with prior art, beneficial effects of the present invention:
(1) raw material is heated evenly: the polar molecule in raw material is turned under the radiation of microwave by original random distribution state
Become arranging according to the polarity orientation of electric field, dipole and alternating electric field on dipole direction and direction of an electric field there are phase difference,
It is intermolecular to rub and collide to hinder this variation to generate, therefore it is uniform to outside inside raw material to utilize microwave activation to have
Heated advantage；
(2) shortening of process time: microwave causes raw molecule to shake, and closes on molecule or atom collides, collision
Cause to stir and move, change kinetics, reduce reaction activity, under same material condition, is heated with traditional resistor
It compares, is substantially shorter processing operation time；
(3) raising of product yield: the pressurization of " press pump " can reduce volatile matter diffusion rate, extend volatile matter in coke hole
Residence time in diameter promotes volatile matter and forms carbon black, is deposited on half carbon surface and improves solid-state charcoal yield." press pump " simultaneously
Pressurization can also promote the polycondensation reaction of tar itself, be greatly lowered or avoid the generation of tar, final to improve product living
The yield and degree of graphitization of property charcoal；
(4) raising of specific surface area: microwave heating is conducive to generate pyrolysis gas inside raw material, pyrolysis gas under pressurization
Body molecule is trapped in inside raw molecule, plays the role of " self-template in situ ", is pyrolyzed under second level and multi-mode microwave heat effect
Gas molecule omnidirectional freedom " shuttle " inside raw material can significantly promote the aperture of active carbon to develop.When pressure in reactor
When being increased to certain numerical value, reactor is instantaneously opened, gas expands rapidly in reactor, and pressure instantaneously reduces, so that raw material point
Pressure difference becomes larger inside and outside son, causes the pyrolysis gas in raw material sharply to expand, instantaneously pops, and punctures raw material inherent structure, secondary to make
Carbon material specific surface area, i.e. " puffed rice " effect are improved in hole.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of apparatus of the present invention.
In figure: 1 program mode controller；2 feeder units；3 reacting furnaces；4 " press pump " units；5 microwave heating units；6 produce an unexpected winner
Unit；7 pyrolysis gas processing units；8 storage bins；9 feeders；10 inlet valves；11 intake valves；12 safety valves；13 circumferentially rotate dress
It sets；14 temperature elements；15 load cells；16 pulsed discharge devices；17 air accumulators；18 pressure and flow controllers；19 pressurization dresses
It sets；20 microwave generators；21 timing-power control members；22 overheat protectors；23 closed shield layers；24 hot product inlet valves；
25 product collecting pits；26 protection gas units；27 discharge valves；28 pyrolysis gas exhaust valves.
Specific embodiment
Below in conjunction with technical solution and the attached drawing specific embodiment that the present invention will be described in detail, but be not limited to the present embodiment.
For those of ordinary skill in the art, without departing from the technical principles of the invention, its other party can also be used
Formula makes replacement, these replacements also should be regarded as protection scope of the present invention.
Embodiment 1
It opens feeder 9 and inlet valve 10 and 500g stalk powder and 500g NaOH activator granulate is transported to reacting furnace 3
Center.After the completion of charging, feeder 9 and inlet valve 10 are closed.Open air accumulator 17, adjust pressure and flow controller 18 to
1000mL/min opens intake valve 11 and nitrogen is passed into reacting furnace 3, until program mode controller shows height in reacting furnace 3
Press pressure to 5MPa.Close air accumulator 17, pressure and flow controller 18 and intake valve 11.Starting circumferentially rotates device 13, and same
Multistage more gradient-heated sides are arranged by timing-power control member 21 and program mode controller 1 in Shi Kaiqi microwave generator 20
Formula, design parameter are as follows: heating 300s with 400W power, then increased wattage maintains 600s to 800W.Microwave priming reaction is completed
First five minute, opening protection gas unit 26 makes product collecting pit 25 filled with nitrogen, gas pressure 0.101Mpa.Microwave activation
After the reaction was completed, it closes and circumferentially rotates device 13 and microwave generator 20.Unbalanced pulse formula discharge device 16, hot product inlet valve
24 and pyrolysis gas exhaust valve 28, by thermal material it is instantaneous it is quick-fried be sprayed onto product collecting pit 25 while reacting furnace in high pressure gas and pyrolysis
Reaction gas is discharged into pyrolysis gas processing unit 7 by pyrolysis gas exhaust valve 28 and carries out subsequent processing and resource utilization.To solid
After product is cooled to room temperature, opens 27 discharging of discharge valve and obtain ultimate activated carbon product.
Claims (6)
1. the device that a kind of " press pump " coupling microwaves quickly prepare high yield active carbon, which is characterized in that described " press pump " coupling
Close microwave quickly prepare high yield active carbon device include program mode controller (1), feeder unit (2), reacting furnace (3), " pressure
Pump " unit (4), microwave heating unit (5), the unit that produces an unexpected winner (6) and pyrolysis gas processing unit (7)；
The feeder unit (2) is equipped with storage bin (8) and feeder (9), and the two is connected, feeder (9) and reacting furnace (3)
Inlet valve (10) be connected；
The reacting furnace (3) is equipped with inlet valve (10), intake valve (11), safety valve (12), circumferentially rotates device (13), thermometric
Element (14), load cell (15) and pulsed discharge device (16)；Inlet valve (10) and intake valve (11) are located at reacting furnace (3)
Arrival end, it is internal that safety valve (12) is located at reacting furnace (3)；Temperature element (14) is connected with the output signal of load cell (15)
Program mode controller (1)；The outlet end that device (13) is located at reacting furnace (3) is circumferentially rotated, pulsed discharge device is passed through
(16) it is connected with the hot product inlet valve (24) of the unit that produces an unexpected winner (6)；
It is described " press pump " unit (4) is equipped with air accumulator (17), pressure and flow controller (18) and pressurizing device (19)；Air accumulator
(17) pressure and flow controller (18) are equipped with, are connected by pressurizing device (19) with the intake valve (11) of reacting furnace (3)；
The microwave heating unit (5) is equipped with microwave generator (20), timing-power control member (21), overheat protector
(22) it is carried out in reacting furnace (3) inner wall by overheat protector (22) with closed shield layer (23), microwave generator (20) setting
Protection；Periodically-power control member (21) is fixed on 5 outer wall of reacting furnace；Periodically-power control member (21), overheat protector
(22) it is connected with program mode controller (1)；
The unit that produces an unexpected winner (6) is equipped with hot product inlet valve (24), product collecting pit (25), protection gas unit (26), discharging
Valve (27) and pyrolysis gas exhaust valve (28), the main body of the unit that produces an unexpected winner (6) are product collecting pit (25), and arrival end is equipped with hot product
Inlet valve (24), outlet end are equipped with the pyrolysis gas exhaust valve (28) being connected with pyrolysis gas processing unit (7)；Discharge valve (27) is set
It sets in product collecting pit (25) bottom；Protection gas unit (26) is unit (6) offer protection gas that produces an unexpected winner.
2. a kind of method that " press pump " coupling microwaves quickly prepare high yield active carbon, which is characterized in that steps are as follows:
(1) the feed pressurization stage:
Solid waste biomass in storage bin (8) is transported to activator by the inlet valve (10) of feeder (9) and reacting furnace (3)
Reacting furnace center；After the completion of charging, adjust " press pump " pressure and flow controller (18) of unit (4) arrives certain flow rate, using adding
Reaction under high pressure gas is passed into reacting furnace (3) by the intake valve (11) of pressure device (19) and reacting furnace (3), i.e. the pressure period；Add
Inlet valve (10) are kept during pressure, circumferentially rotate device (13) and pulsed discharge device (16) closing；Pass through load cell
(15) and program mode controller (1) regulates and controls reacting furnace (3) mesohigh pressure to target value；The setting of safety valve (12) is to protect
Demonstrate,prove reacting furnace (3) interior pressure can receive in range in burner hearth material, when pressure is more than regulation safety limit in burner hearth, safety valve
(12) it would automatically turn on, overpressure in furnace body be discharged, guarantee that safe preparation process carries out；
(2) microwave activation stage:
After completing pressurized operation in reacting furnace (3), starting circumferentially rotates device (13) and microwave heating unit (5) microwave hair
Raw device (20), when jointly controlling activation power and activation by timing-power control member (21) and program mode controller (1)
Between；By temperature element (14) real-time testing reacting furnace (3) interior activation temperature, when reacting furnace (3) interior temperature is more than temperature limit
When, overheat protector (22) will start automatically and block microwave heating, to ensure that microwave activation stage carries out safely；Closed shield
The effect of layer (23) is isolation microwave radiation and external environment, guarantees operator's safety；In entire microwave activation stage pulse
The hot product inlet valve (24) of formula discharge device (16) and the unit that produces an unexpected winner (6) remains turned-off；
(3) it produces an unexpected winner the stage:
It is acted on using protection gas unit (26) so that product collecting pit (25) is filled with certain density inert gas shielding gas, gas
Body pressure will be far below reacting furnace (3) interior air pressure；After the completion of microwave activation stage, pass through pulsed discharge device (16) and heat
Product inlet valve (24) by thermal material it is instantaneous it is quick-fried be sprayed onto product collecting pit (25), hot product moment under atmosphere of inert gases drops
Second reaming is played the role of in temperature, the intramolecular gas abrupt release of hot product；Stage holding discharge valve (27) that produces an unexpected winner is closed straight
It is cooled to room temperature to product, discharging obtains ultimate absorbent charcoal material.
3. according to the method described in claim 2, it is characterized in that,
The solid waste biomass includes waste and old wood corner material, agriculture waste stalk, excess sludge of municipal sewage plant, aquatic
Giantreed, Technical furfural slag；
The activator includes KOH, NaOH, Na2CO3、K2CO3、H3PO4、ZnCl2；
The activator and material quality ratio is 0:1~5:1；
The gas-pressurized is helium, argon gas, nitrogen；
100~the 1000ml/min of pressure process induction air flow ratio；
The pressure period pressure codomain range are as follows: 0.5~20MPa.
4. according to the method in claim 2 or 3, which is characterized in that
The microwave heating is heated using single-stage or multistage more gradient-heateds；
The microwave heating time is 300s~1200s；
The microwave heating power is 400W~900W.
5. according to the method in claim 2 or 3, which is characterized in that
The inertia protection gas is the mixing of one or more of helium, argon gas, nitrogen；
The interior inertia protection atmospheric pressure of the product collecting pit (25) is 0~1Mpa.
6. according to the method described in claim 4, it is characterized in that,
The inertia protection gas is the mixing of one or more of helium, argon gas, nitrogen；
The interior inertia protection atmospheric pressure of the product collecting pit (25) is 0~1Mpa.
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| CN201811462642.8A CN109437191A (en) | 2018-12-03 | 2018-12-03 | A kind of " press pump " coupling microwaves quickly prepare the apparatus and method of high yield active carbon |
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Cited By (1)
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| CN112158843A (en) * | 2020-09-08 | 2021-01-01 | 新奥生物质能(天津)有限公司 | Preparation system and preparation method of biomass activated carbon |
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Application publication date: 20190308 |
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