CN107983308A - A kind of porous carbon adsorbent for removing mercury and preparation method thereof - Google Patents
A kind of porous carbon adsorbent for removing mercury and preparation method thereof Download PDFInfo
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- CN107983308A CN107983308A CN201711308586.8A CN201711308586A CN107983308A CN 107983308 A CN107983308 A CN 107983308A CN 201711308586 A CN201711308586 A CN 201711308586A CN 107983308 A CN107983308 A CN 107983308A
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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
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- 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
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
- C10B53/02—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of cellulose-containing material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/102—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/60—Heavy metals or heavy metal compounds
- B01D2257/602—Mercury or mercury compounds
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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
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Abstract
The invention discloses a kind of porous carbon adsorbent for removing mercury and preparation method thereof, belongs to gas mercury control technology field, porous carbon adsorbent has big specific surface area, flourishing pore structure and abundant Adsorption, beneficial to the efficient removal for realizing mercury.The preparation method of the adsorbent is mainly as follows：Biomass solution agitating and heating is obtained into biomass gel, charing presoma is obtained by freeze-drying, presoma is carbonized under an inert atmosphere, uses CO2Presoma is activated, using H2S is modified material, obtains porous carbon adsorbent.The preparation method is simple and reliable, of low cost without using severe corrosive activating agent, is easy to industrial applications.Therefore, which is a kind of demercuration material with prospects for commercial application.
Description
Technical field
The invention belongs to flue gas pollutant control field, more particularly, to a kind of porous carbon adsorbent for removing mercury and
Its preparation method.
Background technology
Mercury is a kind of poisonous heavy metal, it particularly merits attention the harm that human body and environment are brought.At present, Hen Duoling
Domain can all be related to the discharge of mercury, especially in terms of coal-burning power plant.
Mercury in coal-fired flue-gas includes Elemental Mercury (Hg0), oxidation state mercury (Hg2+) and particle mercury (Hgp)。Hg2+It is soluble in
Water, can be by existing wet desulphurization device efficient removal, HgpIt can be removed by existing dust-extraction unit.But Hg0Since volatility is high,
The reasons such as water-soluble low and chemical inertness, it is difficult to be removed by existing air pollution control devices.Therefore, Hg0Capture be combustion
One of coal-fired plant's mercury control ultimate challenge.Coal-burning power plant's mercury control technology mainly includes oxidation and sorbent injection etc.
Technology.Oxidation technology can make Hg0It is converted into Hg2+, then effectively removed by wet desulphurization equipment.However, the reality of oxidation technology
Matter is to be transferred to mercury in desulfuration solution or desulfurated plaster from flue gas, is not tackled the problem at its root, it is easy to cause
Secondary pollution.Current most promising technology is sorbent injection method, and most common adsorbent is activated carbon, the type adsorbent
It is primarily present problems with：1) activated carbon is low to the adsorption efficiency of mercury；2) need to spray substantial amounts of activated carbon and can be only achieved accordingly
Discharge standard, therefore activated carbon spraying technique cost is higher.
The content of the invention
For the disadvantages described above or Improvement requirement of the prior art, the present invention provides a kind of porous carbon adsorbent for removing mercury
And preparation method thereof, when thus solving to go the removal of mercury using acticarbon at present the existing adsorption efficiency to mercury it is low and into
This higher technical problem.
To achieve the above object, one side according to the invention, there is provided a kind of porous carbon adsorbent for removing mercury
Preparation method, including：
Biomass solution is obtained as carbon source using biomass, being stirred heating to the biomass solution obtains biology
Matter gel；
Charing presoma is obtained by freeze-drying to the biomass gel；
The charing presoma is carbonized under an inert atmosphere；
Use CO2Reaming is carried out to the charing presoma after charing to activate to obtain porous carbon material；
The porous carbon material is ground, then using H2S is modified the porous carbon materials after grinding,
Obtain porous carbon adsorbent.
Preferably, the biomass solution concentration is 10%~30%, to realize more preferable pore-creating character.
Preferably, the biomass gel stirs 20min~50min for the biomass solution in 90 DEG C, and in mould
The shaping biomass gel that middle shaping 4h~8h is obtained, in order to which hydrone is well into biomass molecule gap, is realized more preferable
Pore-size distribution.
Preferably, the charing presoma is to be freeze-dried 60h~84h in -52 DEG C by the shaping biomass gel to obtain
Arrive, in order to fully remove moisture removal.
Preferably, it is described that the charing presoma is carbonized under an inert atmosphere, including：
Using nitrogen atmosphere, with 3 DEG C/min~8 DEG C/min, from room temperature to 600 DEG C, and 0.5h is carbonized at 600 DEG C
~2h, in order to retain the aperture response of charing presoma.
Preferably, the gas flow rate of the nitrogen is 50mL/min~200mL/min, to reduce the disturbance to carbonization process.
Preferably, it is described to use CO2Reaming is carried out to the charing presoma after charing to activate to obtain porous carbon material, is wrapped
Include：
CO is used under the conditions of 900 DEG C2Reaming activation 2h~4h is carried out to the charing presoma after charing and obtains porous charcoal
Material, to realize the specific surface area of the yield of higher and bigger.
Preferably, the CO2Gas flow rate be 50mL/min~200mL/min, to reduce disturbance to activation process.
Preferably, it is described to use H2S is modified the porous carbon materials after grinding, and obtains porous carbon adsorbent,
Including：
With the H of 200ppm~600ppm2S handles porous carbon materials 1h~3h after grinding at room temperature, obtains more
Hole carbon adsorbent, to realize more preferably active bit distribution.
It is another aspect of this invention to provide that provide a kind of the more of removing mercury prepared such as above-mentioned any one the method
Hole carbon adsorbent.
In general, by the contemplated above technical scheme of the present invention compared with prior art, it can obtain down and show
Beneficial effect：
(1) adsorbent provided by the invention uses biomass as charcoal source, it is of low cost, easy to use, its heat endurance is good,
Demercuration efficiency is high, adsorption capacity is big, can effectively remove the Elemental Mercury in coal-fired flue-gas.
(2) sorbent preparation method of the invention, operating method is simple, energy consumption is low, with short production cycle, it can be achieved that adsorbent
Extensive generation.
(3) mercury absorbent of the invention uses H2S is loaded, it can be achieved that H2The joint removing of this polluted gas of S.
Brief description of the drawings
Fig. 1 is a kind of demercuration efficiency schematic diagram of porous carbon adsorbent provided in an embodiment of the present invention.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, it is right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in each embodiment of invention described below
Not forming conflict each other can be mutually combined.
The present invention provides a kind of porous carbon adsorbent for removing mercury and preparation method thereof, biomass is used as charcoal source, it is first
First agitating and heating obtains biomass gel, charing presoma is obtained by freeze-drying, then under an inert atmosphere to presoma
Carbonized, using CO2Activated under the high temperature conditions, finally, using H2S is modified material, obtains porous charcoal absorption
Agent.It can effectively adsorb Hg in coal-fired flue-gas0, it uses cheap biomass as charcoal source, with reference to frozen drying, high temperature CO2Expand
Hole and H2S is loaded, and has the advantages that of low cost, structural behaviour is good, demercuration efficiency is high, adsorption capacity is big.Step is as follows：
(1) biomass solution is obtained as carbon source using biomass, being stirred heating to biomass solution obtains biology
Matter gel；
In one preferred embodiment, biomass can be dissolved and obtains biomass solution concentration in deionized water
For 10%~30%.
In embodiments of the present invention, biomass solution concentration can also be 15%~25%.
In one preferred embodiment, biomass gel stirs 20min~50min for biomass solution in 90 DEG C,
And in a mold, the shaping biomass gel that 4h~8h is obtained is molded at room temperature.
Biomass in embodiments of the present invention can be starch, lignin or sucrose.
(2) charing presoma is obtained by freeze-drying to biomass gel；
In one preferred embodiment, it is to be freeze-dried 60h in -52 DEG C by shaping biomass gel to carbonize presoma
~84h is obtained.
(3) charing presoma is carbonized under an inert atmosphere；
In one preferred embodiment, charing presoma is carbonized under an inert atmosphere, including：
Using nitrogen atmosphere, with 3 DEG C/min~8 DEG C/min, from room temperature to 600 DEG C, and 0.5h is carbonized at 600 DEG C
~2h, it is preferable that the gas flow rate of nitrogen is 50mL/min~200mL/min.
In embodiments of the present invention, presoma carbonization time can also be 0.5h~1.5h.
(4) CO is used2Reaming is carried out to the charing presoma after charing to activate to obtain porous carbon material；
In one preferred embodiment, using CO2Charing presoma progress reaming after charing is activated to obtain more
Hole Carbon Materials, including：
CO is used under the conditions of 900 DEG C2Reaming activation 2h~4h is carried out to the charing presoma after charing and obtains porous charcoal
Material, it is preferable that CO2Gas flow rate be 50mL/min~200mL/min.
For example, 900 DEG C can be raised the temperature in a nitrogen atmosphere, gas is then switched to CO2, at 900 DEG C
2h~4h is activated, then switches to nitrogen, cooled to room temperature, obtains porous carbon material.
In embodiments of the present invention, high temperature CO2Reaming soak time can also be 2.5h~3.5h.
(5) porous carbon material is ground, then using H2S is modified the porous carbon materials after grinding,
Obtain porous carbon adsorbent.
In embodiments of the present invention, after porous carbon material is ground, it can also include what is sieved after grinding with sieve
Step, to obtain the mercury absorbent that particle diameter is less than 150 μm.
In one preferred embodiment, using H2S is modified the porous carbon materials after grinding, and obtains more
Hole carbon adsorbent, including：
With the H of 200ppm~600ppm2S gases, porous carbon materials 1h~3h after processing is ground at room temperature, obtain
To porous carbon adsorbent.
Below in conjunction with drawings and the specific embodiments, the present invention is described in detail.
Embodiment 1
A kind of porous carbon adsorbent of achievable efficient absorption mercury, its preparation method comprise the following steps：
(1) 10g lignin is taken, is dissolved in 100ml deionized waters.
(2) biomass solution is stirred into 20min at 90 DEG C, pours into grinding tool, place 4h at room temperature.
(3) biomass gel prepared by step (2) is transferred to the dry 60h of -52 DEG C of freeze drying box.
(4) by charing presoma prepared by step (3) in 600 DEG C of charing 0.5h of nitrogen atmosphere.
(5) by the CO of the material 50ml/min after charing22h is activated in 900 DEG C of reamings.
(6) Carbon Materials after reaming is activated are ground to 150 μm, then through 200ppm H2S gas modification 1h,
Obtain porous carbon adsorbent PC-1.
Embodiment 2
A kind of porous carbon adsorbent of achievable efficient absorption mercury, its preparation method comprise the following steps：
(1) 10g starch is taken, is dissolved in 100ml deionized waters.
(2) biomass solution is stirred into 20min at 90 DEG C, pours into grinding tool, place 4h at room temperature.
(3) biomass gel prepared by step (2) is transferred to the dry 60h of -52 DEG C of freeze drying box.
(4) by charing presoma prepared by step (3) in 600 DEG C of charing 0.5h of nitrogen atmosphere.
(5) by the CO of the material 200ml/min after charing24h is activated in 900 DEG C of reamings.
(6) Carbon Materials after reaming is activated are ground to 150 μm, then through 200ppm H2S gas modification 1h,
Obtain porous carbon adsorbent PC-2.
Embodiment 3
A kind of porous carbon adsorbent of achievable efficient absorption mercury, its preparation method comprise the following steps：
(1) 10g sucrose is taken, is dissolved in 100ml deionized waters.
(2) biomass solution is stirred into 20min at 90 DEG C, pours into grinding tool, place 4h at room temperature.
(3) biomass gel prepared by step (2) is transferred to the dry 60h of -52 DEG C of freeze drying box.
(4) by charing presoma prepared by step (3) in 600 DEG C of charing 0.5h of nitrogen atmosphere.
(5) by the CO of the material 100ml/min after charing22h is activated in 900 DEG C of reamings.
(6) Carbon Materials after reaming is activated are ground to 150 μm, then through 200ppm H2S gas modification 1h,
Obtain porous carbon adsorbent PC-3.
Embodiment 4
A kind of porous carbon adsorbent of achievable efficient absorption mercury, its preparation method comprise the following steps：
(1) 30g lignin is taken, is dissolved in 100ml deionized waters.
(2) biomass solution is stirred into 50min at 90 DEG C, pours into grinding tool, place 8h at room temperature.
(3) biomass gel prepared by step (2) is transferred to the dry 72h of -52 DEG C of freeze drying box.
(4) by charing presoma prepared by step (3) in 600 DEG C of charing 2h of nitrogen atmosphere.
(5) by the CO of the material 50ml/min after charing23h is activated in 900 DEG C of reamings.
(6) Carbon Materials after reaming is activated are ground to 150 μm, then through 600ppm H2S gas modification 3h,
Obtain porous carbon adsorbent PC-4.
Embodiment 5
A kind of porous carbon adsorbent of achievable efficient absorption mercury, its preparation method comprise the following steps：
(1) 20g starch is taken, is dissolved in 100ml deionized waters.
(2) biomass solution is stirred into 30min at 90 DEG C, pours into grinding tool, place 6h at room temperature.
(3) biomass gel prepared by step (2) is transferred to the dry 72h of -52 DEG C of freeze drying box.
(4) by charing presoma prepared by step (3) in 600 DEG C of charing 1h of nitrogen atmosphere.
(5) by the CO of the material 100ml/min after charing23h is activated in 900 DEG C of reamings.
(6) Carbon Materials after reaming is activated are ground to 150 μm, then through 400ppm H2S gas modification 2h,
Obtain porous carbon adsorbent PC-5.
Embodiment 6
A kind of porous carbon adsorbent of achievable efficient absorption mercury, its preparation method comprise the following steps：
(1) 20g sucrose is taken, is dissolved in 100ml deionized waters.
(2) biomass solution is stirred into 30min at 90 DEG C, pours into grinding tool, place 8h at room temperature.
(3) biomass gel prepared by step (2) is transferred to the dry 84h of -52 DEG C of freeze drying box.
(4) by charing presoma prepared by step (3) in 600 DEG C of charing 2h of nitrogen atmosphere.
(5) by the CO of the material 100ml/min after charing23h is activated in 900 DEG C of reamings.
(6) Carbon Materials after reaming is activated are ground to 150 μm, then through 600ppm H2S gas modification 3h,
Obtain porous carbon adsorbent PC-6.
Embodiment 7
A kind of porous carbon adsorbent of achievable efficient absorption mercury, its preparation method comprise the following steps：
(1) 25g starch is taken, is dissolved in 100ml deionized waters.
(2) biomass solution is stirred into 30min at 90 DEG C, pours into grinding tool, place 6h at room temperature.
(3) biomass gel prepared by step (2) is transferred to the dry 72h of -52 DEG C of freeze drying box.
(4) by charing presoma prepared by step (3) in 600 DEG C of charing 1.5h of nitrogen atmosphere.
(5) by the CO of the material 200ml/min after charing23.5h is activated in 900 DEG C of reamings.
(6) Carbon Materials after reaming is activated are ground to 150 μm, then through 600ppm H2S gas modifications
2.5h, obtains porous carbon adsorbent PC-7.
Embodiment 8
A kind of porous carbon adsorbent of achievable efficient absorption mercury, its preparation method comprise the following steps：
(1) 15g starch is taken, is dissolved in 100ml deionized waters.
(2) biomass solution is stirred into 50min at 90 DEG C, pours into grinding tool, place 8h at room temperature.
(3) biomass gel prepared by step (2) is transferred to the dry 60h of -52 DEG C of freeze drying box.
(4) by charing presoma prepared by step (3) in 600 DEG C of charing 1h of nitrogen atmosphere.
(5) by the CO of the material 50ml/min after charing22.5h is activated in 900 DEG C of reamings.
(6) Carbon Materials after reaming is activated are ground to 150 μm, then through 600ppm H2S gas modification 2h,
Obtain porous carbon adsorbent PC-8.
The demercuration performance test methods of above example 1~8 are as described below：
The demercuration performance of adsorbent prepared by the present invention is tested in fixed bed reactors, and adsorbent amount is
0.1g, flue gas flow 1L/min.As shown in Figure 1, the different porous carbon adsorbent mercury absorbent demercuration efficiencies of embodiment 1~8 with
The change curve of temperature.As shown in Figure 1, mercury absorbent of the invention can maintain more than 85% demercuration efficiency.Preferable absorption
Agent, PC-5, PC-7 and PC-8 porous charcoal mercury absorbent in embodiment 5,7 and 8 can maintain more than 90% demercuration efficiency.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, all any modification, equivalent and improvement made within the spirit and principles of the invention etc., should all include
Within protection scope of the present invention.
Claims (10)
- A kind of 1. preparation method for the porous carbon adsorbent for removing mercury, it is characterised in that including：Biomass solution is obtained as carbon source using biomass, heating is stirred to the biomass solution obtains biomass and coagulate Glue；Charing presoma is obtained by freeze-drying to the biomass gel；The charing presoma is carbonized under an inert atmosphere；Use CO2Reaming is carried out to the charing presoma after charing to activate to obtain porous carbon material；The porous carbon material is ground, then using H2S is modified the porous carbon materials after grinding, and obtains Porous carbon adsorbent.
- 2. according to the method described in claim 1, it is characterized in that, the biomass solution concentration is 10%~30%.
- 3. according to the method described in claim 2, it is characterized in that, the biomass gel for the biomass solution in 90 DEG C Stir 20min~50min, and the shaping biomass gel that shaping 4h~8h is obtained in a mold.
- 4. according to the method described in claim 3, it is characterized in that, the charing presoma is by the shaping biomass gel 60h~84h is freeze-dried in -52 DEG C to obtain.
- 5. method according to any one of claims 1 to 4, it is characterised in that described under an inert atmosphere to the charcoal Change presoma to be carbonized, including：Using nitrogen atmosphere, with 3 DEG C/min~8 DEG C/min, from room temperature to 600 DEG C, and carbonize at 600 DEG C 0.5h~ 2h。
- 6. according to the method described in claim 5, it is characterized in that, the gas flow rate of the nitrogen is 50mL/min~200mL/ min。
- 7. method according to any one of claims 1 to 4, it is characterised in that described to use CO2To the charing after charing Presoma carries out reaming and activates to obtain porous carbon material, including：CO is used under the conditions of 900 DEG C2Reaming activation 2h~4h is carried out to the charing presoma after charing and obtains porous carbon material.
- 8. the method according to the description of claim 7 is characterized in that CO2Gas flow rate be 50mL/min~200mL/min.
- 9. method according to any one of claims 1 to 4, it is characterised in that described to use H2After S is to grinding Porous carbon materials are modified, and obtain porous carbon adsorbent, including：With the H of 200ppm~600ppm2S handles porous carbon materials 1h~3h after grinding at room temperature, obtains porous charcoal suction Attached dose.
- A kind of 10. porous carbon adsorbent of the removing mercury prepared such as claim 1 to 9 any one the method.
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| CN109817923A (en) * | 2019-01-23 | 2019-05-28 | 重庆工商大学 | A kind of nitrogen-doped porous carbon material and its preparation method and application |
| CN109985602A (en) * | 2019-03-13 | 2019-07-09 | 北京化工大学 | CaC2And CO2Or the method and its absorption demercuration application of carbonate ball milling preparation carbon material containing oxycetylene |
| CN110255528A (en) * | 2019-07-25 | 2019-09-20 | 燕山大学 | The method and its application of porous carbon materials are prepared using dyestuff waste liquid |
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| CN112058226A (en) * | 2020-08-28 | 2020-12-11 | 华南理工大学 | Organic silicon-activated carbon modified composite material and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109817923A (en) * | 2019-01-23 | 2019-05-28 | 重庆工商大学 | A kind of nitrogen-doped porous carbon material and its preparation method and application |
| CN109985602A (en) * | 2019-03-13 | 2019-07-09 | 北京化工大学 | CaC2And CO2Or the method and its absorption demercuration application of carbonate ball milling preparation carbon material containing oxycetylene |
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| CN110255528A (en) * | 2019-07-25 | 2019-09-20 | 燕山大学 | The method and its application of porous carbon materials are prepared using dyestuff waste liquid |
| CN112058226A (en) * | 2020-08-28 | 2020-12-11 | 华南理工大学 | Organic silicon-activated carbon modified composite material and preparation method thereof |
| CN112058226B (en) * | 2020-08-28 | 2022-05-10 | 华南理工大学 | Organic silicon-activated carbon modified composite material and preparation method thereof |
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Application publication date: 20180504 |