CN109603410A - A kind of method of Elemental Mercury in efficient removal flue gas - Google Patents
A kind of method of Elemental Mercury in efficient removal flue gas Download PDFInfo
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- CN109603410A CN109603410A CN201910109543.XA CN201910109543A CN109603410A CN 109603410 A CN109603410 A CN 109603410A CN 201910109543 A CN201910109543 A CN 201910109543A CN 109603410 A CN109603410 A CN 109603410A
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- mercury
- flue gas
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- selenizing
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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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0262—Compounds of O, S, Se, Te
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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
- B01D2253/112—Metals or metal compounds not provided for in B01D2253/104 or B01D2253/106
-
- 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
-
- 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 Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
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- Treating Waste Gases (AREA)
Abstract
The invention discloses a kind of methods of Elemental Mercury in efficient removal flue gas.For the present invention using metal selenizing mineral as demercuration medium, the metal selenizing mineral include marthozite (CuSe), selenium molybdenum ore (MoSex) and zinc selenide (ZnSe), contact it with the mercury in flue gas, to convert gaseous elemental mercury volatile in flue gas to stable selenization mercury；The natural reserves of metal selenizing mineral are higher and are relatively easy to synthesize, and have high mercury adsorption capacity and the rate of adsorption, and therefore, the present invention has high-efficient, small investment, and the advantages such as simple and easy have a vast market application prospect.
Description
Technical field
The invention belongs to environmental pollution prevention and control purification techniques fields, and in particular to Elemental Mercury in a kind of efficient removal flue gas
Method.
Background technique
The features such as mercury is because of its severe toxicity, high volatile, property easy to migrate and bioconcentration, by United Nations Environment Programme
(UNEP) global environmental contaminants are regarded as, are reported according to 2018 whole world mercury pollutions of the newest publication of UNEP, in atmosphere due to
Mankind's activity and the mercury discharged reaches 2500 tons/year, be discharged into mercury in nature considerably beyond due to activity naturally.
The whole world of in August, 2017 " Minamata pact " it is formally effective in its 128 signatories to a treaty, its object is to limit increasingly sharpen it is artificial
Mercury pollution discharge, receives extensive concern and the approval of international community.
" thermal power plant pollutant emission standard " is formulated in 2011, it is specified that since on January 1st, 2015 in China
The discharge of coal-burning boiler mercury is controlled, standard clear stipulaties mercury and mercuric compounds discharge amount is strictly limited in 0.03mgm-3Below；
From in " lead, the Zn Cr coating pollutant emission standard (GB 25466-2010) " that on October 1st, 2010 implements clearly stipulate that existing
Lead, Zn Cr coating enterprise mercury and mercuric compounds discharge amount no more than 1.0 mgm-3；Enterprise is created after on October 1st, 2010
Mercury and mercuric compounds discharge amount is strictly limited in 0.05mgm-3Below.Come into effect from July 1st, 2014 " tin, antimony,
Mercury emission of industrial pollutants standard (GB 30770-2014) " in, clear stipulaties existing mining, ore dressing, metallurgy industry enterprise
Mercury and mercuric compounds discharge amount is no more than 0.01 mgm-3, the mercury and mercuric compounds row of enterprise is created after on July 1st, 2014
High-volume strictly it is limited in 0.01mgm-3Below.After coming into force from August 16th, 2017 " Minamata pact " to China, China is not yet
The new regulation about limitation mercury emissions is put into effect；However it must be to fire coal, non-ferrous metal metallurgy and waste in view of pact regulation
Further limitation is taken in the Mercury In The Air disposal of pollutants in burning field, to alleviate the whole world mercury pollution problem increasingly sharpened instantly,
The appearance of new standard is extremely urgent, and State Ministry of Environmental Protection also will put into the more time and energy strictly to limit the discharge of gas mercury,
And multiple industries such as thermoelectricity, thermoelectricity, metallurgy, building materials, chemical industry can also be faced with bigger gas mercury emission reduction in the future, seek
Economically viable gas mercury control method is imperative.
In three kinds of existing forms of mercury, particle mercury (Hgp) volatility it is lower, can be more efficiently by flue gas ash removal
Device is removed, in addition to this, oxidation state mercury (Hg2+) removed since its water solubility can be cooperateed with by existing flue gas desulfurization device,
But Elemental Mercury (Hg0) due to the features such as its is not soluble in water and high volatile, it is difficult to be removed by existing flue gas processing device,
Therefore, Hg in flue gas0Effective removing be current mercury pollution emission reduction field problem.Although nowadays acticarbon is a kind of
More mature business demercuration medium, but demercuration efficiency is restricted by coal quality and flue gas condition, and at high cost, and consumption is big, fortune
Row somewhat expensive；Mercury is mainly physical absorption on the surface of active carbon, is easier to release again when active carbon is exposed in environment
It releases and secondary pollution is generated to environment；And the mercury adsorption capacity and rate of commercial activated carbons are smaller, are difficult to meet day from now on
The mercury emissions standard that benefit improves.
Compared to commercial activated carbons and metal sulfide, the interaction force between mercury and selenium reaches hundred between mercury and sulphur
Wan Bei ensure that mercury adsorption capacity and rate using metal selenizing mineral demercuration, to considerably reduce the use of adsorbent
The extremely stable compound (mercury selenide, HgSe) that amount and cost, mercury and selenium are formed can guarantee the mercurous absorption being exposed in environment
Mercury release rate in agent is lower than one magnitude of mercuric sulphide, and this new disclosed demercuration method based on metal selenizing mineral is relatively living
Property charcoal possesses more wide active temperature section, can be used for any position of fume treatment, and all have than traditional active carbon
Better demercuration effect.
Summary of the invention
For overcome the deficiencies in the prior art, the object of the present invention is to provide a kind of low pollutions, the efficient removal of low cost
The method of Elemental Mercury in flue gas.This method has ideal flue gas demercuration effect in the case where adsorbent additional amount is extremely low.
The present invention uses marthozite (CuSe), selenium molybdenum ore (MoSex) or zinc selenide (ZnSe) be used as demercuration medium, be based on mercury
The very strong interaction force between selenium atom can achieve the Hg in flue gas0It is completely converted into the purpose of HgSe, metallic selenium
Changing mineral adsorbent can be sprayed in any stage of fume treatment or be added in a manner of fixed bed, and be added in adsorbent
In the case that amount substantially reduces, there is more excellent demercuration effect than metal sulfide, when the adsorbent containing HgSe is concentrated
When collecting and being discharged into environment, possess mercury fixed effect more better than sulfide mineral, is leached and the mercury that discharges again
Ratio will substantially reduce.
Technical solution of the present invention is specifically described as follows.
A method of using the mercury in metal selenizing mineral purifying smoke, using metal selenizing mineral as demercuration matchmaker
It is situated between, will be unstable in flue gas, the gaseous elemental state of conversion easy to migrate is converted into stable, is not easy the selenization of Transport And Transformation
Mercury.
In the present invention, demercuration medium is the material that natural or synthetic metal selenizing mineral are active material, in which: metal
Selenizing mineral are selected from marthozite CuSe, selenium molybdenum ore MoSexWith it is any in zinc selenide ZnSe.
In the present invention, natural metal selenizing mineral BET specific surface area is greater than 0.01 m2/ g, grain diameter is in 5-200
Between mesh；The metal selenizing mineral BET specific surface area of synthesis is greater than 5m2/ g, grain diameter is between 10-300 mesh.
In the present invention, the reaction temperature section of demercuration is room temperature to 400 DEG C.
In the present invention, the concentration of Elemental Mercury is less than 100 mgm in flue gas-3。
In the present invention, the concentration of sulfureous in flue gas oxide is less than 10%, and the concentration of nitrogen oxides is less than 5%, water vapor concentration
Less than 20%.
In the present invention, mercury removal device is separately installed fixed bed reactors or sorbent injection tower.
In the present invention, when with fixed bed reactors demercuration, the installation site of Elemental Mercury elimination reaction device is full flue gas section, can
It is voluntarily adjusted according to flue-gas temperature.In the case, metal selenizing mineral must be carried on porous carrier, and divide 2-8 layers into
Row installation, to increase the contact area of metal selenizing mineral and mercury and reduce to resistance caused by flue gas.
In the present invention, when with sorbent injection tower demercuration, the installation site of Elemental Mercury elimination reaction device is full flue gas section, can
It is voluntarily adjusted according to flue-gas temperature, in spray tower, the time of contact of Elemental Mercury and metal selenizing mineral is greater than 1 s；It is installed
Injection apparatus be furnished with deduster, the metal selenizing mineral sprayed into flue gas can be collected and are recycled, until demercuration effect
Rate is supplemented new adsorbent lower than 99%.
Compared to the prior art, compared with the prior art, the present invention has the following advantages:
(1) metal selenizing mineral are present in a large amount of natural crystal, and are relatively easy to artificial synthesized, and raw material easily obtains,
It is low in cost, excellent effect.
(2) the features such as metal selenizing mineral have solubility extremely low, and decomposition temperature is higher, stablize under environmental exposure, therefore,
Secondary pollution of the discarded adsorbent to environment is significantly reduced using metal selenizing mineral as adsorbent.
(3) due to interaction force very strong between selenium and mercury atom, using metal selenizing mineral demercuration, adsorbance is reachable
To 100 times or more of conventional carbon, the 2 times or more of metal sulfide, the rate of adsorption up to 200 times of conventional carbon with
On, 10 times or more of metal sulfide.
(4) the leaching ratio of HgSe in the environment is even less than mercury in the most stable of existing forms of nature, i.e. mercuric sulphide
(HgS), therefore, doing demercuration medium using metal selenizing mineral can be effectively reduced discharging again for mercury.
(5) different from high request of the conventional carbon to temperature and atmosphere, flue-gas temperature and smoke components are to metal selenizing
The influence that mineral generate is smaller, so that its scope of application be made to significantly improve than conventional carbon.
Detailed description of the invention
Fig. 1 (a) spray tower (for having sorbent circulation pipeline) and (b) knot of fixed bed reactors (for 3 layers)
Structure schematic diagram.
Specific embodiment
Technical solution of the present invention is described further below by way of specific embodiment.Embodiment is not to protection scope
Limitation.
Fig. 1 (a) spray tower (for having sorbent circulation pipeline) and (b) knot of fixed bed reactors (for 3 layers)
Structure schematic diagram.
Embodiment 1
50 mg of natural marthozite (CuSe) is weighed, BET specific surface area is 0.18 m2 g-1, sieved with 100 mesh sieve after drying, by it
It is placed in a length of 10cm, internal diameter is in the cylindrical quartz glass fixed bed reactors of 1cm.Mercury, Hg are generated by mercury osmos tube0Just
75 μ gm of beginning concentration-3, and with 1 L min-1Nitrogen effect carrier gas by CuSe adsorbent, simulated flue gas flow velocity is
0.15m·s-1, Hg is imported and exported using VM3000 mercury vapourmeter monitoring reactor0Concentration.When reaction temperature is room temperature, to Hg0Suction
Attached efficiency is up to 100%.
Embodiment 2
Weigh synthesis selenium molybdenum ore (MoSe3) 10 mg, synthetic method are as follows: by selenium powder and sodium molybdate mixed dissolution in the hydration of 14 v%
In hydrazine solution, solution is transferred in reaction kettle and 180o12h is reacted under conditions of C, is sieved with 100 mesh sieve after centrifugal drying, BET
Specific surface area is up to 101.3 m2 g-1.By the MoSe of synthesis3It weighs 10 mg and is placed in a length of 10cm, internal diameter is the cylinder of 1cm
In quartz glass fixed bed reactors.Mercury, Hg are generated by mercury osmos tube01000 μ gm of initial concentration-3, and with 1 L min-1
Nitrogen effect carrier gas pass through MoSe3Adsorbent, simulated flue gas flow velocity are 0.5 ms-1, monitored using VM3000 mercury vapourmeter anti-
Device is answered to import and export elemental mercury concentration, reaction temperature 50oC, under high mercury content smoke condition, Hg0Removal efficiency be
100%, and 100h can be remained above, in the respective metal sulfide (MoS that same dose is added3) in the case where, Hg0Removal effect
Rate is kept for 100% time be reduced to 30h.
Embodiment 3
Weigh synthesis zinc selenide (ZnSe) 200 mg, synthetic method are as follows: by the zinc sulfate and sodium selenate mixed dissolution of equimolar ratio
In the hydrazine hydrate solution of 10 v%, and 150 in reaction kettleoReact 12h under the conditions of C, 100 meshes after centrifugal drying,
BET specific surface area reaches 202 m2 g-1.The ZnSe of synthesis is weighed into 200 mg and is placed in a length of 10cm, internal diameter is the cylinder of 1cm
In shape quartz glass fixed bed reactors.Hg is generated by mercury osmos tube0, Hg060 μ gm of initial concentration-3, and with 1 L min-1Nitrogen effect carrier gas by ZnSe adsorbent, while 300 ppm NO of simulated flue gas ingredient, 400 ppm SO is added2、30
Ppm HCl and 8% H2O imports and exports elemental mercury concentration using VM3000 mercury vapourmeter monitoring reactor.Reaction temperature is 200 DEG C, Hg0
Eliminating efficiency reaches 100%, sustainable to use more than 100h.The respective metal sulfide of the quality such as addition under the same terms
(ZnS), Hg0Removal efficiency is only 80%, and the up time is obviously shortened.
Embodiment 4
It weighs natural marthozite (CuSe), 100 meshes after drying, being sprayed into volume is 1 m3Pilot scale spray tower in, Hg0's
Initial concentration is 100 μ gm-3, flue gas flow rate is 0.2 m/s, and flue gas flow is 1 m3·min-1, while simulated flue gas is added
4% O of ingredient2、1% NO、2% SO2With 10% H2O, when CuSe the amount of injection is greater than 50 mgm-3When, Hg0Removal efficiency reaches
100%。
Embodiment 5
It is tested in the small power plant that certain installed capacity is 5MW, fuel is lignite, 12,135 m of exhaust gas volumn3·min-1,
The mass concentration of mercury is 0.327 mgm-3, sorbent injection tower (temperature is installed in wet desulphurization and wet dedusting upstream respectively
Respectively 103.5 DEG C and 68.3 DEG C) spray into the CuSe synthesized, synthetic method are as follows: mix the copper sulphate of equimolar ratio and sodium selenate
Conjunction is dissolved in the hydrazine hydrate solution of 10 v%, and 120 in reaction kettleo6h, 100 mesh after centrifugal drying are reacted under the conditions of C
Sieve, BET specific surface area are 35 m2 g-1.When straying quatity is 10 mgm-3, Hg0Extrusion rate all reach 100%, pass through 0.6%
Acetum simulated environment leach, the mercury of leaching is only adsorb mercury content 0.05%, almost be can be ignored.It surveys simultaneously
The mercury adsorption effect for having tried CuS, when the amount for spraying into CuS reaches 50mg m-3When, effect can be only achieved 100%, and the mercury leached reaches
To the 0.7% of absorption mercury content, it is higher than and uses one magnitude of CuSe demercuration.
Embodiment 6
With natural selenium molybdenum ore (MoSex) it is used as demercuration medium, it is carried out in certain the small-sized zinc smelting factory for carrying out zinc abstraction technique
Experiment, zinc abstraction amount are 7.6 th-1, exhaust gas volumn is 18000 m3·h-1, electrostatic precipitator (including wet cottrell)
Hg afterwards0Discharge amount is 3.77 mgm-3, ZnSe is added in a manner of fixed bed after electrostatic precipitator, and fixed bed ZnSe is carried
Amount is 10kg, point 3 layers of load, Hg0Extrusion rate up to 100%, serviceable bife was more than 1 month；Use the natural sulphur of equal quality instead
Molybdenum ore load, reduced service life are less than 10 days.
Above embodiments are the description of the invention, are not limitation of the invention, and any couple of present invention is simply repaired
Scheme after changing, belongs to protection scope of the present invention.
Claims (9)
1. a kind of method of Elemental Mercury in efficient removal flue gas, which is characterized in that using metal selenizing mineral as demercuration medium,
Selenization mercury is converted by gaseous elemental state in flue gas.
2. the method according to claim 1, wherein demercuration medium is that natural or synthetic metal selenizing mineral are
The material of active material, in which: metal selenizing mineral include marthozite CuSe, selenium molybdenum ore MoSexWith zinc selenide ZnSe.
3. according to the method described in claim 2, it is characterized in that, natural metal selenizing mineral BET specific surface area is greater than
0.01 m2/ g, grain diameter is between 5-200 mesh；The metal selenizing mineral BET specific surface area of synthesis is greater than 5m2/ g, particle
Diameter is between 10-300 mesh.
4. the method according to claim 1, wherein the reaction temperature section of demercuration is room temperature to 300 DEG C.
5. the method according to claim 1, wherein the concentration of gaseous elemental mercury is less than 100 mgm in flue gas-3。
6. the method according to claim 1, wherein the concentration of the oxysulfide in flue gas is less than 10%, nitrogen oxidation
The concentration of object is less than 5%, and water vapor concentration is less than 20%.
7. the method according to claim 1, wherein mercury removal device is separately installed fixed bed reactors or suction
Attached dose of spray tower.
8. the method according to the description of claim 7 is characterized in that when with fixed bed reactors demercuration, Elemental Mercury elimination reaction
The installation site of device is full flue gas section, can voluntarily be adjusted according to flue-gas temperature, and metal selenizing is mineral loaded on porous carrier, and
Divide 2-8 layers to be installed.
9. the method according to the description of claim 7 is characterized in that simple substance mercury removal sprays when with sorbent injection tower demercuration
The installation site of tower is full flue gas section, can voluntarily be adjusted according to flue-gas temperature, in spray tower, Elemental Mercury and metal selenizing mineral
Time of contact be greater than 1s；The injection apparatus installed is furnished with bag filter, the metal selenizing mine for that will spray into flue gas
Object is collected.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110115972A (en) * | 2019-05-17 | 2019-08-13 | 中南大学 | A kind of structural formula adsorbent material and preparation method thereof removing mercury in flue gas |
| CN110170302A (en) * | 2019-05-31 | 2019-08-27 | 贵州重力科技环保有限公司 | The preparation method and material of grade nanometer selenium charcoal base demercuration sorbing material in situ and application |
| CN110694582A (en) * | 2019-10-22 | 2020-01-17 | 中南大学 | Mercury enrichment material for mercury detector, preparation method and application |
| CN110732303A (en) * | 2019-12-05 | 2020-01-31 | 中南大学 | transition metal selenide modified molding demercuration material and preparation method thereof |
| CN112755764A (en) * | 2020-12-16 | 2021-05-07 | 中南大学 | Stable suspension system for removing mercury in flue gas and recovery method thereof |
| CN113231004A (en) * | 2021-05-28 | 2021-08-10 | 中南大学 | Normal temperature and pressure preparation method and application of metal selenide mercury adsorbent |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110170302A (en) * | 2019-05-31 | 2019-08-27 | 贵州重力科技环保有限公司 | The preparation method and material of grade nanometer selenium charcoal base demercuration sorbing material in situ and application |
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| CN110732303A (en) * | 2019-12-05 | 2020-01-31 | 中南大学 | transition metal selenide modified molding demercuration material and preparation method thereof |
| CN112755764A (en) * | 2020-12-16 | 2021-05-07 | 中南大学 | Stable suspension system for removing mercury in flue gas and recovery method thereof |
| CN112755764B (en) * | 2020-12-16 | 2021-10-19 | 中南大学 | Stable suspension system for removing mercury in flue gas and recovery method thereof |
| CN113231004A (en) * | 2021-05-28 | 2021-08-10 | 中南大学 | Normal temperature and pressure preparation method and application of metal selenide mercury adsorbent |
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