CN106064053A - A kind of flue gas demercuration adsorbent and preparation method thereof - Google Patents
A kind of flue gas demercuration adsorbent and preparation method thereof Download PDFInfo
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- CN106064053A CN106064053A CN201610390380.3A CN201610390380A CN106064053A CN 106064053 A CN106064053 A CN 106064053A CN 201610390380 A CN201610390380 A CN 201610390380A CN 106064053 A CN106064053 A CN 106064053A
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- ionic liquid
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
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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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- 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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- B01J20/3202—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
- B01J20/3204—Inorganic carriers, supports or substrates
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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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- 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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- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/46—Materials comprising a mixture of inorganic and organic materials
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
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Abstract
The invention belongs to purifying coal-fired flue gas association area, it discloses a kind of flue gas demercuration adsorbent, it is made up of ionic liquid and Bio-sil.Described ionic liquid is 1 butyl 3 Methylimidazole. iron chloride ionic liquid, and its mass percent is 10%～50%；Described Bio-sil is impregnated with described ionic liquid, and described ionic liquid adsorbs on the duct of described Bio-sil.The invention still further relates to the preparation method of described flue gas demercuration adsorbent.The flue gas demercuration adsorbent better heat stability of the present invention, renewable, demercuration efficiency is high, and operating temperature range is wider.Additionally, the preparation method of the flue gas demercuration adsorbent of present invention offer is simple, pollution-free.
Description
Technical field
The invention belongs to purifying coal-fired flue gas association area, more particularly, to a kind of flue gas demercuration adsorbent and system thereof
Preparation Method, described flue gas demercuration adsorbent coupled ion liquid and the characteristic of porous material, utilize ionic liquid to carry out aoxidizing also
Absorb Elemental Mercury, it is achieved the efficient removal of coal-fired flue-gas hydrargyrum；The bivalent mercury generated after oxidation is adsorbable in the surface of porous material,
Adsorbent better heat stability, renewable, operating temperature range is wider.
Background technology
Human health and the toxic action of ecological environment are received much concern by mercury contaminants because of it, and nature and human activity are all
Can cause the discharge of mercury contaminants, wherein coal-burning power plant's mercury emissions has become the main mercury pollution emission source in air.At present,
Multiple method is had to be applied to coal-fired mercury pollution emission control.Owing to the Elemental Mercury in coal-fired flue-gas removes difficulty, having of a kind of row
The mercury control method of effect is that elemental mercury oxidation becomes divalent mercuric compounds, and the bivalent mercury after oxidation enters wet scrubber can
It is captured down thus reaches the purpose of power plant soot fume demercuration.It is considered as a kind of effective for using adsorbent method demercuration
Coal-fired mercury pollution controls technology, and this is also worldwide study hotspot.The main active charcoal of demercuration adsorbent, flying dust, gold
Belong to class catalyst and nano adsorber etc..
Wherein, as a kind of environmentally friendly green solvent, ionic liquid has obtained widely due to the character of its uniqueness
Pay close attention to, be one of absorbent being applied to gas purification and separation field of numerous rise.Have the use of document report in recent years
In removing flue gas the ionic liquid of Elemental Mercury be mainly the blend absorbent of ionic liquid, i.e. imidazoles halogen ionic liquid with
The mixing of the mixed liquor of the mixed liquor of iodine, imidazoles halogen ionic liquid and hydrogen peroxide and iron-based glyoxaline ion liquid and water
Liquid.Imidazoles halogen ionic liquid does not have oxidisability with the mixed liquor intermediate ion liquid of iodine or hydrogen peroxide, really is able to oxygen
Change Elemental Mercury is iodine and hydrogen peroxide, and both absorbent are non-renewable；Iron-based glyoxaline ion liquid and the mixing of water
In liquid iron-based glyoxaline ion liquid can oxidative absorption Elemental Mercury and product at pure O2Under the conditions of renewable, yet with mixed
Close evaporation of water in liquid and limit its use temperature.The blend absorbent of these ionic liquids all also exists poor heat stability, work
Make the problem that temperature range is narrower.Additionally, Publication No. CN103877844B discloses a kind of by glyoxaline ion liquid and double
The demercuration absorbent that oxygen water mixes, the demercuration mechanism of this absorbent is the Oxidation due to hydrogen peroxide, and wherein imidazoles
Class ionic liquid is only used as reaction medium and is not involved in oxidation reaction.
Summary of the invention
For disadvantages described above or the Improvement requirement of prior art, the invention provides a kind of flue gas demercuration adsorbent and system thereof
Preparation Method, it is carried out based on demercuration mechanism, coupled ion liquid and the characteristic of porous material, composition and composition to adsorbent
Design.Described adsorbent utilizes ionic liquid to carry out aoxidizing and absorbing Elemental Mercury, it is achieved the efficient removal of Mercury In Coal Combustion Flue Gas, oxygen
Changing the bivalent mercury obtained and be adsorbed in porous material, and this adsorbent heat good stability, renewable, operating temperature range is wider.
For achieving the above object, it is an aspect of this invention to provide that provide the preparation method of a kind of flue gas demercuration adsorbent,
It comprises the following steps:
(a) use equimolar 1-butyl-3-Methylimidazole. chloride salt ions liquid and ferric chloride hexahydrate carry out mixing with
Preparation 1-butyl-3-Methylimidazole. iron chloride ionic liquid, and described 1-butyl-3-Methylimidazole. iron chloride ionic liquid is put
Drying basin is put into standby after being dried 48 hours in the air dry oven that temperature is 80 DEG C；
B Bio-sil is impregnated described 1-butyl-3-Methylimidazole. iron chloride ionic liquid 2 hours by (), make described 1-fourth
Base-3-Methylimidazole. iron chloride ionic liquid adsorbs on the duct of described Bio-sil, to obtain coal-fired demercuration adsorbent；Its
In, the mass percent of described 1-butyl-3-Methylimidazole. iron chloride ionic liquid is 10%～50%.
According to another aspect of the present invention, it is provided that a kind of flue gas demercuration adsorbent, it is by ionic liquid and porous silicon
Glue forms, it is characterised in that:
Described ionic liquid is 1-butyl-3-Methylimidazole. iron chloride ionic liquid, and its mass percent is 10～50%；
Described Bio-sil is impregnated with described ionic liquid, and described ionic liquid adsorbs in the duct of described Bio-sil
On.
Further, the operating temperature of described flue gas demercuration adsorbent is 80～300 DEG C.
Further, the best in quality percentage ratio of described ionic liquid is 30%.
In general, by the contemplated above technical scheme of the present invention compared with prior art, the cigarette that the present invention provides
QI prostration mercury absorbent and preparation method thereof, described flue gas demercuration adsorbent combine the oxidisability of ionic liquid and heat stability with
The high-specific surface area characteristic of Bio-sil, ionic liquid carries out aoxidizing and absorbing Elemental Mercury, it is achieved Mercury In Coal Combustion Flue Gas efficient
Removing, the bivalent mercury that oxidation obtains is adsorbed in porous material, and this adsorbent heat good stability, renewable, operating temperature range
Wider.Additionally, the preparation method of the flue gas demercuration adsorbent of present invention offer is simple, pollution-free.
Accompanying drawing explanation
Fig. 1 is the flow chart of the preparation method of the flue gas demercuration adsorbent that better embodiment of the present invention provides.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, right
The present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, and
It is not used in the restriction present invention.If additionally, technical characteristic involved in each embodiment of invention described below
The conflict of not constituting each other just can be mutually combined.
Referring to Fig. 1, the preparation method of the flue gas demercuration adsorbent that better embodiment of the present invention provides, it includes following
Step:
Step 1, prepares ionic liquid.Concrete, the preparation of described ionic liquid comprises the following steps:
(1-1) weigh equimolar 1-butyl-3-Methylimidazole. chloride salt ions liquid and ferric chloride hexahydrate mixes
To obtain mixture, and described mixture is positioned in magnetic agitation water-bath, is stirred continuously under the conditions of temperature is 40 DEG C
Until described mixture is gradually become homogeneous liquid, stratification by crystalline state；
(1-2) use pear shape separatory funnel to the described mixture separation aqueous phase of stratification and ionic liquid phase, remove
After aqueous phase, described ionic liquid is placed in the air dry oven that temperature is 80 DEG C and is dried 48 hours, the 1-butyl-3-first prepared
It is standby that base imidazoles iron chloride ionic liquid puts into drying basin.
In present embodiment, also include the described 1-butyl-3-Methylimidazole. iron chloride ion that will obtain in step (1-2)
Liquid carries out Fourier infrared FT IR and Raman Raman to be tested, to confirm the step of the zwitterion structure of described ionic liquid
Suddenly.
Step 2, impregnates porous material described 1-butyl-3-Methylimidazole. iron chloride ionic liquid 2 hours, makes described 1-
Butyl-3-Methylimidazole. iron chloride ionic liquid adsorbs on the duct of described porous material, to obtain flue gas demercuration adsorbent.
Concrete, with Bio-sil as support materials, use physical impregnation evaporation by described 1-butyl-3-Methylimidazole. iron chloride from
Sub-liquid load is as follows to the step of described Bio-sil:
(2-1) Bio-sil is placed in temperature to be 500 DEG C, be filled with N2Calcining and activating 6 hours in the high temperature process furnances of gas,
And according to described 1-butyl-3-Methylimidazole. iron chloride ionic liquid loaded amount the mass percent of adsorbent (ionic liquid account for)
It is 10%～50%, weighs the described 1-butyl-3-Methylimidazole. iron chloride ionic liquid of respective quality and described porous respectively
Silica gel.Being appreciated that in other embodiments, described Bio-sil can be substituted by other porous materials, such as porous silicon carbide
Silicon.
(2-2) methanol described 1-butyl-3-Methylimidazole. iron chloride ionic liquid being completely dissolved in corresponding volume is molten
In agent, then mix described silica gel with described 1-butyl-3-Methylimidazole. iron chloride ionic liquid and first solution equal-volume to obtain
To mixture, and the described mixture obtained by equal-volume mixing is placed in magnetic agitation water-bath, is 30 DEG C of bars in temperature
Being stirred continuously under part, slow evaporation removes methanol solvate, finally by described mixture in the air dry oven that temperature is 80 DEG C
It is dried 48 hours until the volatilization of all methanol, prepares the different described 1-butyl-3-ionic liquid loaded amounts of Methylimidazole. iron chloride
Flue gas demercuration adsorbent.
The described flue gas demercuration adsorbent that present embodiment prepares includes 1-butyl-3-Methylimidazole. iron chloride ionic liquid
And it is impregnated with the Bio-sil of described 1-butyl-3-Methylimidazole. iron chloride ionic liquid, described 1-butyl-3-Methylimidazole. chlorine
Change iron ion liquid adsorption on the duct of described Bio-sil.The flue gas demercuration adsorbent of present embodiment is primarily adapted for use in combustion
The demercuration of flue-gas.
Active substance [C in described flue gas demercuration adsorbent4mim][FeCl4] and Elemental Mercury Hg0Carry out adsorption reaction, raw
Become bivalent mercury HgCl2Ionic liquid [the C ferrous with chloride containing4mim][FeCl3], bivalent mercury HgCl2It is adsorbed in described porous silicon
Glue SiO2Duct inwall on, and described ionic liquid [C4mim][FeCl3] at pure O2Under conditions of can regeneration have
[the C of oxidisability4mim][FeCl4]。
Present embodiment has also carried out sign and demercuration performance test to described flue gas demercuration adsorbent, to obtain described cigarette
The performance characteristic of QI prostration mercury absorbent.The described flue gas demercuration adsorbent of powder is carried out thermogravimetric TGA and duct feature BET table
Levying, find that the actual loading rate of described flue gas demercuration adsorbent may be up to more than 95%, better heat stability, temperature is 350 DEG C
Time just start decompose；The load factor of described 1-butyl-3-Methylimidazole. iron chloride ionic liquid is more than or equal to 10% and is less than
When 50wt%, the Bio-sil of described flue gas demercuration adsorbent still has a pore passage structure of relatively horn of plenty, and described 1-butyl-
3-Methylimidazole. iron chloride ionic liquid still can be stable absorption on the duct of described Bio-sil.
The demercuration performance test of described flue gas demercuration adsorbent is carried out on fixed-bed reactor, the simulation containing mercury vapour
Flue gas N2/O2/CO2It is passed through in tube furnace reaction tube, by ionic liquid loaded for 0.1g difference 1-butyl-3-Methylimidazole. iron chloride
The described flue gas demercuration adsorbent of rate is positioned over and is connected with N2/O2/CO2Reaction tube in, operating temperature is 160 DEG C, export mercury vapour
Concentration is measured in real time by mercury vapour on-line detector and is obtained demercuration efficiency to calculate.Described 1-butyl-3-Methylimidazole. chlorine
The load capacity changing iron ion liquid is 10wt%, and accordingly, its demercuration efficiency is 87%；Described 1-butyl-3-Methylimidazole. chlorine
The load capacity changing iron ion liquid is 30wt%, and accordingly, its demercuration efficiency is 97%；Described 1-butyl-3-Methylimidazole. chlorine
The load capacity changing iron ion liquid is 50wt%, and accordingly, its demercuration efficiency is 95%.Experiment display, described 1-butyl-3-first
The optimum load amount of base imidazoles iron chloride ionic liquid is 30wt%, and accordingly, its demercuration efficiency may be up to 97%.
Present embodiment has also carried out demercuration performance test to flue gas demercuration adsorbent described at a temperature of other different operatings,
Equally, first by the simulated flue gas N containing mercury vapour2/O2/CO2It is passed through in tube furnace reaction tube, by 1-butyl-3-first described in 0.1g
The ionic liquid loaded amount of base imidazoles iron chloride is that the described flue gas demercuration adsorbent of 30wt% is positioned over and is connected with N2/O2/CO2Anti-
Ying Guanzhong, operating temperature controls more than or equal to 60 DEG C and less than or equal within 400 DEG C, and outlet mercury vapour concentration is steamed by hydrargyrum equally
Gas on-line detector is measured to calculate the demercuration effect obtaining described flue gas demercuration adsorbent at a temperature of different operating in real time
Rate.Being obtained by experiment, described flue gas demercuration adsorbent is under conditions of temperature is more than or equal to 80 DEG C and is less than or equal to 300 DEG C
Demercuration efficiency is maintained at more than 90%, and the active temperature interval of demercuration is wider, and temperature the highest demercuration performance is the best.
Flue gas demercuration adsorbent that the present invention provides and preparation method thereof, described adsorbent combines the oxidation of ionic liquid
Property and the high-specific surface area characteristic of heat stability and porous material, ionic liquid carries out aoxidizing and absorbing Elemental Mercury, it is achieved coal-fired
The efficient removal of mercury in flue gas, the bivalent mercury that oxidation obtains is adsorbed in porous material, and this adsorbent heat good stability, can be again
Raw, operating temperature range is wider.Additionally, the preparation method of the flue gas demercuration adsorbent of present invention offer is simple, pollution-free.
As it will be easily appreciated by one skilled in the art that and the foregoing is only presently preferred embodiments of the present invention, not in order to
Limit the present invention, all any amendment, equivalent and improvement etc. made within the spirit and principles in the present invention, all should comprise
Within protection scope of the present invention.
Claims (4)
1. a flue gas demercuration adsorbent, it is made up of ionic liquid and Bio-sil, it is characterised in that:
Described ionic liquid is 1-butyl-3-Methylimidazole. iron chloride ionic liquid, and its mass percent is 10%～50%；
Described Bio-sil is impregnated with described ionic liquid, and described ionic liquid adsorbs on the duct of described Bio-sil.
Flue gas demercuration adsorbent the most according to claim 1, it is characterised in that: the work temperature of described flue gas demercuration adsorbent
Degree is 80～300 DEG C.
Flue gas demercuration adsorbent the most according to claim 1, it is characterised in that: the best in quality percentage of described ionic liquid
Ratio is 30%.
4. a preparation method for flue gas demercuration adsorbent, it comprises the following steps:
A () uses equimolar 1-butyl-3-Methylimidazole. chloride salt ions liquid and ferric chloride hexahydrate to carry out mixing with preparation
1-butyl-3-Methylimidazole. iron chloride ionic liquid, and described 1-butyl-3-Methylimidazole. iron chloride ionic liquid is placed in temperature
Degree be the air dry oven of 80 DEG C is dried 48 hours after to put into drying basin standby；
B Bio-sil is impregnated described 1-butyl-3-Methylimidazole. iron chloride ionic liquid 2 hours by (), make described 1-butyl-3-
Methylimidazole. iron chloride ionic liquid adsorbs on the duct of described Bio-sil, to obtain coal-fired demercuration adsorbent；Wherein, institute
The mass percent stating 1-butyl-3-Methylimidazole. iron chloride ionic liquid is 10%～50%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109731455A (en) * | 2019-02-01 | 2019-05-10 | 四川大学 | Inhibit mercury method for releasing again in Limestone-gypsum Wet Flue Gas Desulfurization Process technique |
| CN109758897A (en) * | 2019-02-01 | 2019-05-17 | 四川大学 | Mercury contaminants method is removed in a kind of wet desulfurizing process |
| CN113058561A (en) * | 2021-04-09 | 2021-07-02 | 浙江工业大学 | Recyclable ionic liquid adsorbent and preparation method and application thereof |
| CN113926304A (en) * | 2021-03-22 | 2022-01-14 | 青岛大学 | Low-temperature demercuration adsorbent for coal-fired flue gas |
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|---|---|---|---|---|
| CN102020610A (en) * | 2009-09-16 | 2011-04-20 | 北京化工大学 | Low-viscosity ionic liquid |
| CN102513064A (en) * | 2011-12-23 | 2012-06-27 | 广东工业大学 | Preparation method and application of ionic liquid bonded silica adsorbent |
| CN104324585A (en) * | 2014-11-05 | 2015-02-04 | 朱忠良 | Method for purifying blast furnace flue gas by using ionic liquid |
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2016
- 2016-06-03 CN CN201610390380.3A patent/CN106064053A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102020610A (en) * | 2009-09-16 | 2011-04-20 | 北京化工大学 | Low-viscosity ionic liquid |
| CN102513064A (en) * | 2011-12-23 | 2012-06-27 | 广东工业大学 | Preparation method and application of ionic liquid bonded silica adsorbent |
| CN104324585A (en) * | 2014-11-05 | 2015-02-04 | 朱忠良 | Method for purifying blast furnace flue gas by using ionic liquid |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109731455A (en) * | 2019-02-01 | 2019-05-10 | 四川大学 | Inhibit mercury method for releasing again in Limestone-gypsum Wet Flue Gas Desulfurization Process technique |
| CN109758897A (en) * | 2019-02-01 | 2019-05-17 | 四川大学 | Mercury contaminants method is removed in a kind of wet desulfurizing process |
| CN113926304A (en) * | 2021-03-22 | 2022-01-14 | 青岛大学 | Low-temperature demercuration adsorbent for coal-fired flue gas |
| CN113926304B (en) * | 2021-03-22 | 2024-01-16 | 青岛大学 | Low-temperature mercury-removing adsorbent for coal-fired flue gas |
| CN113058561A (en) * | 2021-04-09 | 2021-07-02 | 浙江工业大学 | Recyclable ionic liquid adsorbent and preparation method and application thereof |
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