CN208249907U - A kind of equipment preparing active carbon from coal for microwave heating auxiliary one step activation of vapor - Google Patents

A kind of equipment preparing active carbon from coal for microwave heating auxiliary one step activation of vapor Download PDF

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Publication number
CN208249907U
CN208249907U CN201820756251.6U CN201820756251U CN208249907U CN 208249907 U CN208249907 U CN 208249907U CN 201820756251 U CN201820756251 U CN 201820756251U CN 208249907 U CN208249907 U CN 208249907U
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China
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microwave
coal
vapor
active carbon
reaction tube
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Expired - Fee Related
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CN201820756251.6U
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Chinese (zh)
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朱玉雯
韩广程
高婷婷
刘汉桥
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Tianjin Chengjian University
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Tianjin Chengjian University
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Abstract

The utility model discloses a kind of equipment for preparing active carbon from coal for microwave heating auxiliary one step activation of vapor, including microwave generating unit, steam generating unit, reaction member and control unit, the microwave generating unit and steam generating unit is connect with reaction member respectively, and is controlled by control unit.The utility model uses microwave radiation method to prepare active carbon for low-order coal and provides thermal energy, can be realized and is rapidly heated, and by controlling microwave power, can regulate and control heating rate;The characteristics of microwave body formula, selectivity heating, so that mixed powder is heated evenly;It will increase the defect of carbon structure by microwave irradiation, increase reaction active site, to promote the reaction rate of vapor and carbon structure;The increase of carbon structure defect can also promote the generation of activated carbon surface functional group, and intensity and time by adjusting microwave irradiation can control oxygen-containing functional group quantity;And device structure is simple and convenient to operate, active carbon preparation efficiency is high.

Description

It is a kind of to prepare active carbon from coal for microwave heating auxiliary one step activation of vapor Equipment
Technical field
The utility model belongs to active carbon preparation technical field, and in particular to one kind assists vapor one for microwave heating The equipment that step activation prepares active carbon from coal.
Background technique
Preparing active carbon from coal mainly uses gas activation at present, a large amount of without addition compared with chemical activation method Chemicals, not only production cost is low, and avoids equipment corrosion and environmental pollution.Gas activation is by feed coal through charcoal After change process, priming reaction is carried out with carbonized material at a certain temperature using activated gas, ultimately forms flourishing pore structure, And there is certain surface chemistry.Carbonization process usually carries out under 600~750 DEG C of inert atmospheres, decomposes random in coal Then carbon and strengthen microstructure carbon, to improve the intensity of active carbon;Priming reaction process is usually carried out at 750~950 DEG C, is used Activated gas be often certain density vapor, CO2, low concentration O2Or its mixed gas etc., pass through the oxygen of gas and carbon content in coal structure Change reaction, ultimately generates the active carbon with abundant pore structure and surface functional group.
The charing of active carbon preparation and priming reaction process are required to a large amount of thermal energy, conventional heating (hot fume purging etc.) item Under part, material particles are the heating process of ecto-entad, and heating rate is lower, and heating time is long, and material is easy uneven heating It is even.Activated gas vapor, CO2Etc. being weak oxide gas, activation time lower with the reaction rate of carbon content in coal structure It is long, and generate the surface functional group limited amount of activated coke, can not enhancement activated carbon absorption and catalytic performance.In addition, when long Between ecto-entad activation process, also will cause the serious surface of active carbon particle and burn and lose, to reduce the charcoal rate that obtain, improve preparation Cost.
In contrast, the advantage that microwave heating has body formula, selectively heats, is non-contact thermal, there is heating speed Rate is high, particles by heat is uniform, being capable of quick start and the characteristics of stop.The crystallite carbon structure and inorganic ash content being distributed in feed coal Etc. good wave-sucking performance is all had, being conducive to microwave electromagnetic can be to the conversion of thermal energy, therefore coal activated carbon process has benefit With the condition of microwave heating.In addition, microwave heating process can cause the defect sturcture of carbon, activated carbon surface functional group can be promoted Generation.
But there are no can be used for microwave heating auxiliary one step activation of vapor to prepare setting for active carbon from coal on the market It is standby.
Utility model content
The purpose of the utility model is to overcome the deficiencies in the prior art, provide a kind of for microwave heating auxiliary vapor The equipment that one step activation prepares active carbon from coal prepares active carbon from coal by the way that microwave heating combination steam activation is compound, promotees Intake steam and carbon structure reaction rate and promote the generation of activated carbon surface functional group, and structure be simple and convenient to operate, Active carbon preparation efficiency is high.
The utility model is achieved through the following technical solutions:
List occurs for a kind of equipment for preparing active carbon from coal for microwave heating auxiliary one step activation of vapor, including microwave Member, steam generating unit, reaction member and control unit, the microwave generating unit and steam generating unit respectively with react Unit connection, and controlled by control unit;
The microwave generating unit includes microwave generator and microwave transmission pipe, and microwave transmission pipe one end and microwave occur Device connection, the other end are connect with the reaction member;
The steam generating unit includes that mixed gas tank, steam evaporator, peristaltic pump and protection gas tank, the water steam Gas generator is with wriggling series connection of pumps, and common access in parallel with protection gas tank mixes gas tank, and the mixed gas tank and reaction member connect It connects;
The reaction member includes reaction tube, temperature indicator, thermocouple, tripod and support rod, reaction tube and institute The microwave transmission pipe stated is perpendicular, and top is provided with the temperature indicator, and the thermocouple is vertically arranged in reaction It is connect in pipe and with the temperature indicator, below the thermocouple, is equipped with tripod and support rod, crucible inside reaction tube Frame bottom surface is horizontal, by support rod support;
The control unit includes controller and control panel.
In the above-mentioned technical solutions, the microwave generator is also connected with constant temperature water tank.
In the above-mentioned technical solutions, it is offered on the tube wall of the microwave transmission pipe convenient for observing state in the reaction tube Peep hole.
In the above-mentioned technical solutions, the peep hole rectangular array is arranged in microwave transmission pipe and intersects with reaction tube Place, and the same horizontal position is in the bottom of tripod in reaction tube.
In the above-mentioned technical solutions, vent gas treatment bottle is also connected on the reaction tube.
In the above-mentioned technical solutions, between the steam evaporator and mixed gas tank, between mixed gas tank and reaction tube The outer wrap round heat tracing band of gas piping.
In the above-mentioned technical solutions, the reaction tube is transparent quartz ampoule, and reaction tube upper and lower ends are movably connected with There are end cap and pedestal.
In the above-mentioned technical solutions, silicone gasket is provided in the end cap and pedestal.
It in the above-mentioned technical solutions, is inert protective gas, specially nitrogen, helium or argon in the protection gas tank Gas.
In the above-mentioned technical solutions, the control unit further includes power meter.
A kind of equipment preparing active carbon from coal for microwave heating auxiliary one step activation of vapor of the utility model exists In use, the reaction utensil for being contained with iron and coal dust mixed powder is placed on the tripod in reaction tube, control microwave occurs single Member and steam generating unit, which are opened, carries out microwave irradiation and steam activation to mixed powder, and the tail gas generated in reaction process is logical It is discharged after crossing the processing of vent gas treatment bottle.
It the advantages of the utility model and has the beneficial effect that
(1) the utility model uses microwave radiation method to prepare active carbon for low-order coal and provides thermal energy, naturally divides using in coal The crystallite carbon structure and inorganic ash content of cloth can be realized and are rapidly heated as wave absorbing agent, by controlling microwave power, can regulate and control Heating rate;It the characteristics of microwave body formula, selectivity heating, is heated simultaneously so that each particle and particle in mixed powder are inside and outside, Powder is heated evenly.
(2) the utility model will increase the defect of carbon structure by microwave irradiation, increase reaction active site, to promote water The reaction rate of steam and carbon structure;The increase of carbon structure defect can also promote the generation of activated carbon surface functional group, and lead to The intensity and time for overregulating microwave irradiation can control oxygen-containing functional group quantity.
(3) a kind of equipment for preparing active carbon from coal for microwave heating auxiliary one step activation of vapor of the utility model Structure is simple and convenient to operate, active carbon preparation efficiency is high.
Detailed description of the invention
Fig. 1 is a kind of equipment for preparing active carbon from coal for microwave heating auxiliary one step activation of vapor of the utility model Structural schematic diagram.
Fig. 2 is the cross-sectional view of reaction tube in Fig. 1 (6) part.
Wherein:
1: constant temperature water tank, 2: microwave generator, 3: controller, 4: control panel, 5: power meter, 6: reaction tube, 7: observation Hole, 8: temperature indicator, 9: heating tape, 10: mixed gas tank, 11: steam evaporator, 12: peristaltic pump, 13: protection gas tank, 14: Vent gas treatment bottle, 15: microwave transmission pipe, 16: thermocouple, 17: tripod, 18: support rod.
It for those of ordinary skill in the art, without creative efforts, can be according to above attached Figure obtains other relevant drawings.
Specific embodiment
The utility model is described in further detail with specific embodiment with reference to the accompanying drawing.It should be understood that Following embodiments be it is illustrative, be not restrictive, the protection scope of the utility model cannot be limited with following embodiments.
Embodiment one
In conjunction with shown in attached drawing 1-2, one kind of the utility model prepares coal for microwave heating auxiliary one step activation of vapor The equipment of matrix activated carbon, including the microwave generating unit being made of microwave generator 2 and microwave transmission pipe 15, by mixed gas tank 10, Steam evaporator 11, peristaltic pump 12 and protection gas tank 13 form steam generating unit, by reaction tube 6, temperature indicator 8, The reaction member and be made of controller 3, power meter 5 and control panel 4 that thermocouple 16, tripod 17 and support rod 18 form Control unit;The microwave generating unit and steam generating unit is connect with reaction member respectively, and passes through control Unit control;
The microwave transmission pipe 15 is horizontally disposed, connect with one end of microwave generator 2, microwave generator 2 it is another End be connected with constant temperature water tank 1, the constant temperature water tank 1 be used for microwave generator 2 cooling, the other end of microwave transmission pipe 15 with react The reaction tube 6 of unit connects, and microwave transmission pipe 15 is mutually perpendicular to reaction tube 6, and reaction tube 6 is transparent quartz ampoule, top It is provided with temperature indicator 8, inner vertical is provided with thermocouple 16, which connect with temperature indicator 8, in thermocouple The reaction tube 6 of 16 lower sections is internally provided with tripod 17 and support rod 18, and the bottom surface of tripod 17 is horizontal, by holding with support rod 18 Support, above-mentioned support rod 18 are vertically arranged;On the tube wall of the microwave transmission pipe 15 of microwave transmission pipe 15 Yu 6 intersection of reaction tube Offer 7 rectangular array of the peep hole arrangement convenient for observing the peep hole 7 of state in the reaction tube 6, and with reaction tube 6 The bottom of interior tripod 17 is in the same horizontal position, is also connected with vent gas treatment bottle 14 on reaction tube 6.
The steam evaporator 11 is connected with peristaltic pump 12, and common access in parallel with protection gas tank 13 mixes gas tank 10, which connect with the top of reaction tube 6, wherein between steam evaporator 11 and mixed gas tank 10, mix gas tank 10 and The outer wrap round heat tracing band 9 of gas piping between reaction tube 6, interior protection gas tank 13 is inert protective gas, specially nitrogen.
Embodiment two
On the basis of the above embodiment 1, further, 6 upper and lower ends of reaction tube have been movably connected with End cap and pedestal are provided with silicone gasket in end cap and pedestal, are equivalent on the top of reaction tube 6 and bottom end setting silica gel Washer can play the role of the sealed environment for protecting reaction tube 6 to be can guarantee in reaction tube 6 again.
A kind of equipment preparing active carbon from coal for microwave heating auxiliary one step activation of vapor of the utility model exists In use, the reaction utensil for being contained with ferrum-based catalyst and coal dust mixed powder is placed on the tripod 17 in reaction tube 6, control Microwave generating unit and steam generating unit, which are opened, carries out microwave irradiation and steam activation to mixed powder, produces in reaction process Raw tail gas is discharged after being handled by vent gas treatment bottle 14.
Embodiment three
On the basis of above-described embodiment two, active carbon from coal is prepared using the utility model, it is (i.e. low using low-order coal The coal of degree of metamorphism) in the eastern coal of standard, it is as shown in the table as coal dust raw material:
Using Micromeritics company ASAP2020 surface area and pore structure study instrument, the hole of sample is held and is divided Analysis: being put into de-aeration stage for test sample first, deaerates 8h, is then analyzed, with high-purity N in 473K under vacuum condition2To inhale Attached matter measures relative pressure (P/P at liquid nitrogen temperature (77.3K)0)10-7Absorption, desorption isotherm in~1 range;By opposite Liquid nitrogen adsorptive value calculates liquid nitrogen volume as total pore volume, using DR equation calculation Micropore volume, mesopore volume when pressure is 0.98 Micropore volume is subtracted for total pore volume.
It is tested by temperature programmed desorption (TPD), the quantity-of test activated carbon surface oxygen-containing functional group uses program liter Warm detachment assays system mainly includes temperature programmed control tubular heater, heat tracing carrying pipe and portable fourier-transform infrared light Spectrometer (Gasment-DX4000 type).Portable Fourier transformation infrared spectrometer can measure gas component change with on-line continuous Change.2.0g sample is weighed, is laid in horizontal pipe furnace, heat temperature raising.Escaping gas is by high-purity N2(1L/min) is carried, warp Conduit with heating tape is continually fed into portable Fourier transformation infrared spectrometer and measures gas concentration (CO, CO2And H2O)。 Tube furnace initial temperature is set as 110 DEG C, stops 20min drying and dehydrating, is then warming up to 1000 DEG C with 8 DEG C/min.Temperature-rise period In, oxygen-containing functional group is thermally decomposed, with CO or CO2Form evolution.It is measured by portable Fourier transformation infrared spectrometer CO and CO2Lasting evolution concentration, then it is integrated calculate 110 DEG C~1000 DEG C heating process be precipitated CO and CO2Total amount Correspondence obtains the total amount of the oxygen-containing functional groups such as phenolic hydroxyl group, carboxyl, lactone group, ether, carbonyl, quinonyl, pyranone and chromene.
Use six hydration FeCl3It is added in raw coal coal dust, is uniformly mixed using ball-milling method, drum's speed of rotation is 1500rad/min, Ball-milling Time 100min, obtains coal dust intermixture.Under conditions of microwave irradiation, to coal dust intermixture into Row steam activation, microwave output power 450W, vapor volumetric concentration (percentage by volume) are 50%, other gases are nitrogen The flow that gas, every 10g mixture institute water flowing steam and nitrogen mix gas is 400mL/min, activation time 60min.After activating Mixture remove Fe element, concentration of hydrochloric acid 1mol/L with salt acid soak, hydrochloric acid dosage needed for every 10g mixture is 120mL, Soaking time is 2h, then with deionized water wash products up to no chloride test goes out.By the active carbon after washing at 80 DEG C Drying obtains the active carbon from coal of structural strength height, hole prosperity after dry.Wherein adjustment ferro element accounts for quality of pc ratio and is 4%, 6%, 8% and 10%, the active carbon of different ferro element additive amounts is prepared respectively, pore volume adds with ferro element in investigation The relationship of dosage.For the intensity for increasing active carbon, a small amount of ferrum-based catalyst is adulterated into low-order coal, since ferrum-based catalyst has Good wave-sucking performance can generate localized hyperthermia at 1000 DEG C or more, and have the function of catalyzed graphitization, therefore can The intensity that a large amount of class graphite microcrystalline structures improve active carbon is formed around Fe can by controlling the content of Fe base catalyst The content of class graphite microcrystal is adjusted, microstructure is the class graphite microcrystal group of shortrange order, and class graphite microcrystalline structure can be improved The intensity of active carbon;Fe is removed after pickling simultaneously, forms apparent central hole structure, Fe base catalyst not only has catalytic graphite The effect of change also has the function of mesoporous template, by adjusting the content of Fe base catalyst, can regulate and control central hole structure, make It obtains mesopore volume and is not less than 0.25cm3/ g-only changes the mass ratio that Fe element accounts for coal dust, when mass ratio is increased to from 3% 10%, mesopore volume is from 0.25cm3/ g increases to 0.40cm3/g。
The utility model uses microwave radiation method to prepare active carbon for low-order coal and provides thermal energy, utilizes natural distributed in coal Crystallite carbon structure and inorganic ash content can be realized and are rapidly heated as wave absorbing agent, by controlling microwave power, can regulate and control heating Rate;It the characteristics of microwave body formula, selectivity heating, is heated simultaneously so that each particle and particle in mixed powder are inside and outside, powder It is heated evenly;It will increase the defect of carbon structure by microwave irradiation, increase reaction active site, to promote vapor and carbon structure Reaction rate;The increase of carbon structure defect can also promote the generation of activated carbon surface functional group, and by adjusting microwave spoke According to intensity and time can control oxygen-containing functional group quantity;And device structure is simple and convenient to operate, active carbon preparation efficiency It is high.
The spatially relative terms such as "upper", "lower", "left", "right" have been used in embodiment for ease of explanation, have been used for Relationship of the elements or features relative to another elements or features shown in explanatory diagram.It should be understood that in addition to figure Shown in except orientation, spatial terminology is intended to include the different direction of device in use or operation.For example, if in figure Device be squeezed, the element for being stated as being located at other elements or feature "lower" will be located into other elements or feature "upper". Therefore, exemplary term "lower" may include both upper and lower orientation.Device, which can be positioned in other ways, (to be rotated by 90 ° or position In other orientation), it can be interpreted accordingly used herein of the opposite explanation in space.
Illustrative description has been done to the utility model above, it should explanation, in the core for not departing from the utility model In the case where the heart, it is any it is simple deformation, modification or other skilled in the art can not spend creative work etc. The protection scope of the utility model is each fallen with replacement.

Claims (10)

1. a kind of equipment for preparing active carbon from coal for microwave heating auxiliary one step activation of vapor, it is characterised in that: including Microwave generating unit, steam generating unit, reaction member and control unit, the microwave generating unit and steam generating unit It connect with reaction member, and is controlled by control unit respectively;
The microwave generating unit includes microwave generator and microwave transmission pipe, and microwave transmission pipe one end and microwave generator connect It connects, the other end is connect with the reaction member;
The steam generating unit includes mixed gas tank, steam evaporator, peristaltic pump and protection gas tank, the vapor hair Raw device is with wriggling series connection of pumps, and common access in parallel with protection gas tank mixes gas tank, and the mixed gas tank is connect with reaction member;
The reaction member includes reaction tube, temperature indicator, thermocouple, tripod and support rod, reaction tube and described Microwave transmission pipe is perpendicular, and top is provided with the temperature indicator, and the thermocouple is vertically arranged in reaction tube And connect with the temperature indicator, below the thermocouple, tripod and support rod, tripod bottom are equipped with inside reaction tube Face is horizontal, by support rod support;
The control unit includes controller and control panel.
2. the equipment according to claim 1 for preparing active carbon from coal for microwave heating auxiliary one step activation of vapor, It is characterized by: the microwave generator is also connected with constant temperature water tank.
3. the equipment according to claim 1 for preparing active carbon from coal for microwave heating auxiliary one step activation of vapor, It is characterized by: being offered on the tube wall of the microwave transmission pipe convenient for observing the peep hole of state in the reaction tube.
4. the equipment according to claim 3 for preparing active carbon from coal for microwave heating auxiliary one step activation of vapor, It is characterized by: the peep hole rectangular array is arranged in microwave transmission pipe and reaction tube intersection, and in reaction tube The bottom of tripod is in the same horizontal position.
5. the equipment according to claim 1 for preparing active carbon from coal for microwave heating auxiliary one step activation of vapor, It is characterized by: being also connected with vent gas treatment bottle on the reaction tube.
6. the equipment according to claim 1 for preparing active carbon from coal for microwave heating auxiliary one step activation of vapor, It is characterized by: the gas piping between the steam evaporator and mixed gas tank, between mixed gas tank and reaction tube is wound outside Heating tape.
7. the equipment according to claim 1 for preparing active carbon from coal for microwave heating auxiliary one step activation of vapor, It is characterized by: the reaction tube is transparent quartz ampoule, reaction tube upper and lower ends have been movably connected with end cap and pedestal.
8. the equipment according to claim 7 for preparing active carbon from coal for microwave heating auxiliary one step activation of vapor, It is characterized by: being provided with silicone gasket in the end cap and pedestal.
9. the equipment according to claim 1 for preparing active carbon from coal for microwave heating auxiliary one step activation of vapor, It is characterized by: being inert protective gas, specially nitrogen, helium or argon gas in the protection gas tank.
10. the equipment according to claim 1 for preparing active carbon from coal for microwave heating auxiliary one step activation of vapor, It is characterized by: the control unit further includes power meter.
CN201820756251.6U 2018-05-21 2018-05-21 A kind of equipment preparing active carbon from coal for microwave heating auxiliary one step activation of vapor Expired - Fee Related CN208249907U (en)

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CN201820756251.6U CN208249907U (en) 2018-05-21 2018-05-21 A kind of equipment preparing active carbon from coal for microwave heating auxiliary one step activation of vapor

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110980730A (en) * 2019-12-05 2020-04-10 中国科学院广州能源研究所 Method and device for preparing activated carbon by microwave heating and gas activation
CN111533128A (en) * 2020-05-15 2020-08-14 中天超容科技有限公司 Preparation device and preparation method of activated carbon for supercapacitor

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110980730A (en) * 2019-12-05 2020-04-10 中国科学院广州能源研究所 Method and device for preparing activated carbon by microwave heating and gas activation
CN111533128A (en) * 2020-05-15 2020-08-14 中天超容科技有限公司 Preparation device and preparation method of activated carbon for supercapacitor

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