CN108722357A - SO in a kind of efficient absorption flue gas2Modified activated carbon preparation method - Google Patents

SO in a kind of efficient absorption flue gas2Modified activated carbon preparation method Download PDF

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CN108722357A
CN108722357A CN201810614927.2A CN201810614927A CN108722357A CN 108722357 A CN108722357 A CN 108722357A CN 201810614927 A CN201810614927 A CN 201810614927A CN 108722357 A CN108722357 A CN 108722357A
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activated carbon
modified
temperature
preparation
flue gas
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张卫东
刘猛
杨鸣航
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Jiangsu New Gold Environmental Protection Polytron Technologies Inc
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/30—Sulfur compounds
    • B01D2257/302—Sulfur oxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2258/00—Sources of waste gases
    • B01D2258/02—Other waste gases
    • B01D2258/0283—Flue gases

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention discloses SO in a kind of efficient absorption flue gas2Modified activated carbon preparation method, business column activated carbon is rinsed with deionized water, after removing surface dirt, places it in dry in drying box and takes out the activated carbon of preparation, in setting N2Temperature programming is carried out under conditions of being continually fed into, the activated carbon of preparation is taken out, and is placed in tube furnace and is carried out high temperature NH3It is modified, by activated carbon modified activated carbon in high NH3It is cooling under conditions of flow, until room temperature, obtains required sample.The effects that present invention is by the volatilization of organic matter, realizes the expanding treatment of activated carbon, greatly improves activated carbon pore structure, increases mesoporous quantity, improves activated carbon adsorption capacity；The present invention takes " 900-1100 DEG C of 300 DEG C → ammonia of nitrogen temperature heating → stop modified 2-3h → ammonia cooling " pattern, it realizes and forms the relatively strong heat-staple nitrogen-containing functional group such as N-6, N-5 and quaternary nitrogen type (N-Q) in activated carbon surface, improve active carbon high-temp stability and adsorption activity.

Description

SO in a kind of efficient absorption flue gas2Modified activated carbon preparation method
Technical field
The present invention relates to SO in a kind of efficient absorption flue gas2Modified activated carbon preparation method, and in particular to one kind with height The preparation method of warm reaming and the high temperature modified column-shaped active carbon obtained of ammonia, prepares and contains with abundant meso-hole structure and surface The high-efficiency desulfurization column-shaped active carbon of nitrogen functional group, large capacity for generating electricity, in the industry-by-industries desulphurization plant such as steel, chemical industry, High activity SO2Absorption activated carbon.
Background technology
Activated carbon is that a kind of specific surface area is high, pore structure is flourishing and the adjustable porous carbonaceous material of surface chemical property, It is widely used to the various fields such as absorption, catalysis and electrochemistry.The performance of activated carbon depends on its pore structure and by miscellaneous original The surface chemical property that sub (such as oxygen, nitrogen, p and s) significantly affect, i.e. surface functional group.In these hetero atoms, research is most To be widely oxygen and nitrogen, they are respectively formed oxygen-containing and nitrogen-containing functional group in carbon surface.Due to the nitrogenous function of activated carbon surface Therefore the absorption, catalysis and chemical property that group can significantly improve activated carbon improve the pore structure of activated carbon and nitrogenous official The research that can be rolled into a ball causes extensive concern and payes attention to.
In the method that high-temperature technology carries out reaming to activated carbon, it is used not only in sulfur removal technology, in existing denitration, removes Also in extensive use in the link of mercury, studies carefully its preferable reaming effect, the pore structure of activated carbon can be obviously improved, improve it Porosity and mesopore volume have the function that improve activated carbon adsorption capacity.
The ammonia modification of activated carbon is the most popular method that carbon surface introduces nitrogen-containing functional group.The activated carbon of pre-oxidation is not Ammonia modification is carried out under same ammonia treatment temperature, can introduce amide, lactams and acid imide and pyridine, pyrrole in carbon surface It coughs up and greatly improves activated carbon adsorption SO with nitrogen-containing functional groups such as quaternary nitrogen types2The rate of adsorption.At high temperature modified temperature, work as ammonia When treatment temperature reaches 800 DEG C or more, the nitrogen-containing group of carbon surface is mainly derived from ammonia and the carbon atom of carbon surface is directly tied Close formed N-6, N-5 and quaternary nitrogen type (N-Q) nitrogen-containing functional group, than under middle low temperature environment (800 DEG C or less) formed amides, The nitrogen-containing groups such as the nitrogen oxygen type such as acid imide and lactams (N-X) have more thermal stability and desulphurizing activated.
In the patent of invention application No. is CN201610655211.8, " a kind of modified activated carbon and preparation side are disclosed Method and its application ", preparation method is as follows：A kind of graphitization activated carbon is through HNO3After processing, high temperature is carried out under ammonia atmosphere Heat treatment, obtains the high absorbent charcoal carrier of mesoporous rate, has larger void content, higher mesoporous rate (>=97%) conductive Property it is good the features such as, be used for ammonia synthesis catalyst carrier when, the dispersion degree of noble ruthenium can be significantly improved, improve the anti-first of catalyst Alkanisation ability, thermal stability and activity.In the patent of invention application No. is CN201210381226.1, one kind " one is disclosed The modified absorbent charcoal material and preparation method thereof of kind ", preparation method is as follows：Using activated carbon as raw material, activated carbon is placed in and is added In hot stove, it is first passed through nitrogen, ammonia is passed through after raising the temperature to 600-900 DEG C, activated carbon reacts 10- in ammonia 120min is to get modified absorbent charcoal material.Modified absorbent charcoal material has perchlorate ion in water very high adsorptivity Can, the ability of perchlorate in raw material activated carbon adsorption water can be improved to nearly 9 times, and there is high mechanical strength, use life The feature that period is long, use cost is low.Above-mentioned patent is mainly used in adsorbing the application of water pollutant, and present invention proposition is adopted First carry out nitrogen high temperature reaming with business column-shaped active carbon, improve it is mesoporous hastily after carry out the high temperature modified abundant surface of ammonia again and contain Nitrogen functional group, to increase substantially activated carbon to SO2Adsorption efficiency.
The present invention proposes that business column-shaped active carbon first carries out 900-1100 DEG C of nitrogen atmosphere high-temperature process, the hole of activated carbon Gap structure be improved significantly, porosity and mesoporous rate increase, and activated carbon adsorptive capacity is greatly enhanced.Secondly, reaming Activated carbon afterwards passes through high temperature modification of the ammonia at 900-1100 DEG C, and surface nitrogen-containing functional group obviously increases, thermal stability And activity significantly increases, and realizes SO2Large capacity adsorbing and removing.
Invention content
The present invention is directed to that existing activated carbon adsorption volume is small, desulphurizing activated not high, surface nitrogen-containing functional group thermal stability The defects of poor, devises and a set of have high absorption volume, high thermal stability, high adsorption activity and be easily industrialized system Preparation process, and modified activated carbon has been obtained to the SO in flue gas under practical flue gas condition2Suction-operated.
SO in a kind of efficient absorption flue gas2Modified activated carbon preparation method, include the following steps：
(1) business column activated carbon deionized water is rinsed 30-40 times, after removing surface dirt, places it in drying 105 DEG C of dry 12-24h in case；
(2) activated carbon for preparing step (1) takes out, in setting N2Temperature programming is carried out under conditions of being continually fed into, with The heating rate of 10-20 DEG C/min is set in 900-1100 DEG C of temperature range and calcines 2.5-4h, further expands Carriers Active Carbon surface pore structure improves mesoporous rate, realizes reaming；
(3) activated carbon for preparing step (2) takes out, and is placed in tube furnace and carries out high temperature NH3It is modified, it weighs first certain The activated carbon of amount is in tube furnace, first in N2300 DEG C are warming up to certain heating rate under atmosphere, is then switched to NH3Atmosphere Under, it is continuously heating to 900-1100 DEG C, carries out high temperature modified, modification time 2-3h at this temperature；
(4) by the activated carbon modified activated carbon in step (3) in high NH3It is cooling under conditions of flow, until room temperature, obtains Required sample.
Further, in the method for the present invention, the business column-shaped active carbon used in the step (1), diameter in 4-6mm, Length is more than 750m in 5-10mm, specific surface area2/ g, ash content are less than 8%, and intensity is more than 98%.
Further, in the method for the present invention, N is injected in the step (2)2The flow velocity of gas remains at 70-80mL/ Min, calcining furnace temperature are maintained at 900-1100 DEG C, reaction time 2.5-4h.
Further, in the method for the present invention, for modified NH in the step (3)3Purity is 99.99%.
Further, in the method for the present invention, N in the step (3)2Flow velocity in 70-80mL/min, 10 DEG C of heating rate/ Min, NH3Flow velocity is 1-2ml/min, modification time 2-3h.
Further, in the method for the present invention, by NH after the completion of being modified in the step (4)3Flow is improved from 1-2ml/min It to 60ml/min, is continually fed into, until being cooled to room temperature.
Compared with prior art, the present invention has the advantages that：
(1) present invention takes high temperature reaming under 900-1100 DEG C of nitrogen atmosphere, real the effects that by the volatilization of organic matter The expanding treatment of existing activated carbon, greatly improves activated carbon pore structure, increases mesoporous quantity, improves activated carbon adsorption capacity；
(2) present invention takes " 900-1100 DEG C of 300 DEG C → ammonia of nitrogen temperature heating → stop modified 2-3h → ammonia drop Temperature " pattern is realized and forms the relatively strong heat-staple nitrogen-containing functional group such as N-6, N-5 and quaternary nitrogen type (N-Q) in activated carbon surface, improves Active carbon high-temp stability and adsorption activity.
Description of the drawings：
The preparation technology flow chart of the high effective and modified desulphurized aetivated carbon in the positions Fig. 1
Specific implementation mode：
Example 1：
(1) business column-shaped active carbon, diameter 4mm, length 5mm, specific surface area 800m are selected3/ g, intensity 98.5%, ash content 8%；
(2) business column activated carbon is carried out deionized water to rinse 30 times, after clean dry, is placed it in drying box 105 DEG C of dryings, drying time 12h；
(3) activated carbon for preparing step (2) takes out, in setting N2The condition being continually fed into 75mL/min air velocities Lower carry out temperature programming is set in 900 DEG C of temperature ranges with the heating rate of 15 DEG C/min and is calcined 2.5h, is further expanded Carriers Active carbon surface pore structure realizes reaming；
(4) activated carbon for preparing step (3) takes out, and is placed in tube furnace and carries out high temperature NH3It is modified, it weighs first certain The activated carbon of amount is in tube furnace, first in N2It is continually fed into down the heating rate liter with 10 DEG C/min with 75mL/min air velocities Temperature is then switched to NH to 300 DEG C3Under atmosphere, NH is kept3Air-flow is continuously heating to 900 DEG C under the conditions of being 2ml/min, warm herein Degree is lower to carry out high temperature modified, modification time 3h.
(5) by NH after the completion of the activated carbon in step (4) being modified3Flow is improved to 60ml/min, is continually fed into, until It is cooled to room temperature, obtains required sample.
Product activated carbon 15g is taken, desulfurization adsorption test is carried out on fixed bed device.Flue gas composition：Air speed 2374h-1, SO2:1000ppm,O2:10%, remaining is N2, general gas flow 2L/min, reaction show SO2Adsorption efficiency reaches 95%, when continuing Between 4.5h.Its surface pore structure is analyzed by BET, finds SBETReach 954m2/ g, VmesReach 0.025cm3/ g, and surface contains Nitrogen functional group's content is 0.81mmol/g.Example 2：
(1) business column-shaped active carbon, diameter 5mm, length 5mm, specific surface area 850m are selected3/ g, intensity
99%, ash content 7.5%；
(2) business column activated carbon is carried out deionized water to rinse 30 times, after clean dry, is placed it in drying box 105 DEG C of dryings, drying time 12h；
(3) activated carbon for preparing step (2) takes out, in setting N2The condition being continually fed into 75mL/min air velocities Lower carry out temperature programming is set in 1000 DEG C of temperature ranges with the heating rate of 10 DEG C/min and is calcined 3h, is further expanded and is carried Body activated carbon surface pore structure realizes reaming；
(4) activated carbon for preparing step (3) takes out, and is placed in quartz capsule pipe-type stove and carries out high temperature NH3It is modified, claim first Take a certain amount of activated carbon in tube furnace, first in N2It is continually fed into down with the heating of 10 DEG C/min with 75mL/min air velocities Rate is warming up to 300 DEG C, is then switched to NH3Under atmosphere, NH is kept3Air-flow is continuously heating to 1000 under the conditions of being 1.5ml/min DEG C, high temperature modified, modification time 3h is carried out at this temperature.
(5) by NH after the completion of the activated carbon in step (4) being modified3Flow is improved to 60ml/min, is continually fed into, until It is cooled to room temperature, obtains required sample.
Product activated carbon 15g is taken, desulfurization adsorption test is carried out on fixed bed device.Flue gas composition：Air speed 2374h-1, SO2:1000ppm,O2:10%, remaining is N2, general gas flow 2L/min, verification experimental verification SO2Adsorption efficiency reaches 97.06%, holds Continuous time 5h.Its surface pore structure is analyzed by BET, finds SBETReach 1025m2/ g, VmesReach 0.032cm3/ g, and table Face nitrogen-containing functional group content is 0.86mmol/g.Example 3：
(1) business column-shaped active carbon, diameter 6mm, length 5mm, specific surface area 900m are selected3/ g, intensity 99%, ash content 7.5%；
(2) business column activated carbon is carried out deionized water to rinse 30 times, after clean dry, is placed it in drying box 105 DEG C of dryings, drying time is for 24 hours；
(3) activated carbon for preparing step (2) takes out, in setting N2The condition being continually fed into 75mL/min air velocities Lower carry out temperature programming is set in 1100 DEG C of temperature ranges with the heating rate of 20 DEG C/min and is calcined 4h, is further expanded and is carried Body activated carbon surface pore structure realizes reaming；
(4) activated carbon for preparing step (3) takes out, and is placed in quartz capsule pipe-type stove and carries out high temperature NH3It is modified, claim first Take a certain amount of activated carbon in tube furnace, first in N2It is continually fed into down with the heating of 10 DEG C/min with 75mL/min air velocities Rate is warming up to 300 DEG C, is then switched to NH3Under atmosphere, NH is kept3Air-flow is continuously heating to 1100 under the conditions of being 1ml/min DEG C, high temperature modified, modification time 3h is carried out at this temperature.
(5) by NH after the completion of the activated carbon in step (4) being modified3Flow is improved to 60ml/min, is continually fed into, until It is cooled to room temperature, obtains required sample.
Product activated carbon 15g is taken, desulfurization adsorption test is carried out on fixed bed device.Flue gas composition：Air speed 2374h-1, SO2:1000ppm,O2:10%, remaining is N2, general gas flow 2L/min, verification experimental verification SO2Adsorption efficiency reaches 99.13%, holds Continuous time 6h.Its surface pore structure is analyzed by BET, finds SBETReach 1056m2/ g, VmesReach 0.036cm3/ g, and table Face nitrogen-containing functional group content is 0.94mmol/g.

Claims (6)

1. SO in a kind of efficient absorption flue gas2Modified activated carbon preparation method, it is characterised in that the method includes the steps of：
Business column activated carbon deionized water is rinsed 30-40 times, after removing surface dirt, is placed it in 105 in drying box DEG C dry 12-24h；
Activated carbon prepared by step (1) takes out, in setting N2Temperature programming is carried out under conditions of being continually fed into, with 10-20 DEG C/ The heating rate of min is set in 900-1100 DEG C of temperature range and calcines 2.5-4h；
Activated carbon prepared by step (2) takes out, and is placed in tube furnace and carries out high temperature NH3It is modified, a certain amount of activity is weighed first Charcoal is in tube furnace, first in N2300 DEG C are warming up to certain heating rate under atmosphere, is then switched to NH3Under atmosphere, continue It is warming up to 900-1100 DEG C, carries out high temperature modified, modification time 2-3h at this temperature；
By the activated carbon modified activated carbon in step (3) in high NH3It is cooling under conditions of flow, until room temperature, obtains required sample Product.
2. SO in a kind of efficient absorption flue gas according to claim 12Modified activated carbon preparation method, it is characterised in that： In step a, the business column-shaped active carbon of selection, diameter is more than 750m in 4-6mm, length in 5-10mm, specific surface area2/ g, ash Divide and be less than 8%, intensity is more than 98%.
3. SO in a kind of efficient absorption flue gas according to claim 12Modified activated carbon preparation method, it is characterised in that： In step b, N is injected2The flow velocity of gas remains at 70-80mL/min, and calcining furnace temperature is maintained at 900-1100 DEG C, calcining Time maintains 2.5-4h.
4. SO in a kind of efficient absorption flue gas according to claim 12Modified activated carbon preparation method, it is characterised in that： In step c, for modified NH3Purity is 99.99%.
5. SO in a kind of efficient absorption flue gas according to claim 12Modified activated carbon preparation method, it is characterised in that： In step c, N2Flow velocity is in 70-80mL/min, heating rate 10 DEG C/min, NH3Flow velocity is 1-2ml/min, modification time 2-3h.
6. according to claim 1 a kind of for adsorbing SO in flue gas2Modified activated carbon preparation method, it is characterised in that： In step d, by NH after the completion of being modified3Flow is improved from 1-2ml/min to 60ml/min, is continually fed into, until being cooled to room temperature.
CN201810614927.2A 2018-06-14 2018-06-14 SO in a kind of efficient absorption flue gas2Modified activated carbon preparation method Pending CN108722357A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111821945A (en) * 2020-07-07 2020-10-27 美埃(中国)环境科技股份有限公司 Active carbon modification method for removing sulfur dioxide and hydrogen sulfide gas in air
CN112575575A (en) * 2020-07-21 2021-03-30 苏州远浩新纺织科技有限公司 Hole expanding method for activated carbon fiber

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111821945A (en) * 2020-07-07 2020-10-27 美埃(中国)环境科技股份有限公司 Active carbon modification method for removing sulfur dioxide and hydrogen sulfide gas in air
CN112575575A (en) * 2020-07-21 2021-03-30 苏州远浩新纺织科技有限公司 Hole expanding method for activated carbon fiber
WO2022016663A1 (en) * 2020-07-21 2022-01-27 苏州远浩新纺织科技有限公司 Reaming method for activated carbon fiber

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