CN104148013B - The preparation method of fume mercury-removing active carbon - Google Patents
The preparation method of fume mercury-removing active carbon Download PDFInfo
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Abstract
The preparation method of fume mercury-removing active carbon, comprises the steps: the first step, and raw material is removed surface chemistry group: by 100-200 DEG C of oven dry after the NaOH solution washing of 10wt.%～30wt.% for seed activity carbon feedstock; Second step, dipping halide salt: raw material active carbon and the halide salt solution of removing surperficial oxy radical are carried out to hybrid infusion stirring 4 ~ 12 hours according to the mass ratio of 1:1～1:5, filtration drying, obtains being loaded with the active carbon of halide salt, and the concentration of described halide salt solution is 10wt.%～50wt.%; The 3rd step, load halogen: the active carbon that is loaded with halide salt, as in U-shaped pipe, is formed to packed layer, inputted by packed layer top with 100-500mL/min band halogen air, maintain 1～10h under room temperature, obtain the active carbon of saturated load halogen; The 4th step adds the active carbon of saturated load halogen the volatilizable halogen of heat abstraction at 80～120 DEG C, prepares fume mercury-removing active carbon.
Description
Technical field
The invention belongs to fume mercury-removing activated carbon technology field, relate in particular to the preparation method of high effective flue gas removal of mercury active carbon.
Background technology
Coal will remain the main energy sources of electric power in future, the coal-fired flue-gas mercury pollution causing thus has become another the global Significant Problems of Eco-environment after climate change. In coal fire discharged thing, mercury compound, sulfur dioxide dust are also the main causes that PM2.5 forms, and are the roots that causes haze weather. At present, coal in China consumption ranks first in the world, and still accounts for 72% to the year two thousand twenty CHINESE COAL electricity, needs coal-fired approximately 2,700,000,000 tons, estimates 2035, and the supply of electric power in the whole world 43% is still from coal. In coal-fired process, mercury evaporation also enters atmosphere with flue gas, and enter ecological recycle system by precipitation. Although the not high (n × l0 of the mercury content in coal-7The order of magnitude), but the consumption figure of whole world coal is very huge, causes thus mercury emission very large. Jiang Jingkun [Jiang Jingkun, Hao Jiming, Wu Ye, Deng. the preliminary foundation [J] of Coal Combustion in China mercury emissions inventory. environmental science, 2005,26 (2): 35-39.] etc. estimation China's coal-fired flue-gas mercury emission in 2000 is 219.5 tons, and wherein electric power discharge capacity accounts for 35%, Mercury Emissions from Coal-Fired Boilers amount has exceeded the U.S., and atmosphere and soil environment have been caused to severe contamination. Therefore, the whole world increases severely year by year to the demand of fume mercury-removing active carbon.
Mercury in coal-fired flue-gas is mainly with simple substance state mercury (Hg0), particle mercury (HgP) and oxidation state mercury (Hg2+) 3 kinds of forms exist, and under certain condition, in flue gas, the mercury of three kinds of forms can transform mutually. In coal, most mercury is discharged into atmosphere in combustion process, remains in very few (being less than 2%) of mercury in bottom ash. Particle mercury can utilize cleaner to collect and remove, and oxidation state mercury can be removed with wet desulphurization equipment. But Elemental Mercury fusing point low (38.9 DEG C), vapour pressure high (25 DEG C time 0.25Pa), poorly water-soluble (25 DEG C time 600 μ g/L), be difficult to utilize existing pollutant control appliance effectively to remove, harm is large, becomes in mercury pollution control tool challenge and be also the technology that solves be badly in need of.
Research shows, active carbon produces effect at the oxidation state mercury removing in flue gas at present, but is not very desirable for Elemental Mercury removal efficiency. USDOE estimates, is 90% if reach demercuration rate, and the cost that removes 0.45kg mercury is (2.5-7.0) × 104Dollar, so expensive cost, coal-burning power plant is difficult to bear, and active carbon is promoted very difficult in commercial applications, and by add additive in active carbon, this modified activated carbon significantly strengthens the absorption property of mercury, can significantly reduce active carbon demercuration cost.
[Dong Yong, explains quickly Dong Yong etc., and Wang Peng, waits .CaCl2Add the experimental study [J] on mercury Precipitation Behavior impact in pyrolyzing coal. chemistry of fuel journal, 2014,42 (01): 31-36] study the CaCl that adds different chlorinities (mass fraction 0.1%, 0.3%, 0.5%) in low chlorine coal2On the impact of mercury Precipitation Behavior in pyrolysis of coal process. Experimental result shows, temperature is to affect the key factor that mercury is separated out; Along with the increase of chlorine addition, Hg2+Separate out ratio in rising trend; [the LiX such as Li, LiuZ, KimJ, etal.Heterogeneouscatalyticreactionofelementalmercuryvap orovercupricchlorideformercuryemissionscontrol[J] .AppliedcatalysisB:environmental, 2013,132:401-407.] use 1% and 5% zinc chloride to process active carbon, the active carbon mercury adsorption capacity after modification is respectively 5.5 times and 9 times of original activity charcoal; Deng Xianlun etc. [Deng Xianlun, Jiang Jianchun. Development of S-loaded Activated Carbon Applied To Remove Mercury [J]. forest chemical engineering communication, 2004,38 (3): 13-16.] active carbon is mixed to sulphur modification after its demercuration rate reach 99%; [TianLH, LiCT, LiQ, the eta1.Removalofelementalmercurybyactivatedcarbonimpregnat edwithCeO such as Tian2[J] .Fuel, 2009,88 (9): 1687-1691.] prepared load C eO2Active carbon, when load capacity brings up to 80% to mercury clearance from 30% in 120min during at 1%-3%. U.S. PSCo/ADA[Vidic, RD, ChangMT, ThurnauRC, Kineticsofvapor-phasemercuryuptakebyvirginandsulfurimpre gnatedactivatedcarbons[J] .J.airandwaste, 2005,48:247-255.] carry out field trial in power station with industrial activited carbon, result shows: carbon mercury (C/Hg) than when the 5000:1 in ESP(electrostatic precipitator) outlet sprays into active carbon, its removal of mercury efficiency is 45%. Wang Li has just waited [adsorpting characteristic of flying dust carbon residue to nonvalent mercury steam] to study flying dust and do not fire the characterization of adsorption of carbon residue to nonvalent mercury steam. at low mercury equilibrium concentration (< 250ug/m3) under condition, carbon residue mercury adsorption capacity and business active carbon gap are not remarkable, business active carbon obviously raises in the mercury adsorbance of high mercury concentration end, and carbon residue mercury characterization of adsorption and its source correlation are stronger.
In sum, the existing research of fume mercury-removing active carbon, but exist removal of mercury rate not high, mercury capacity is only 1 ‰～10% left and right, especially little to the adsorption capacity of Elemental Mercury, causes application cost high, the problems such as commercial applications difficulty. It is raw material that the present invention selects the commercial active carbon that microporosity is high, first load halogenated alkali metal salt, then use vapor phase method load halogen, and form stable complex salt, finally at high temperature remove volatilizable halogen, make high effective flue gas removal of mercury active carbon. The method is easy to operate, and the active carbon mercury capacity of preparing, up to 150%, has significantly reduced use cost, is easy to commercialization and promotes
Summary of the invention
The technical problem solving:Low in order to solve existing fume mercury-removing adsorbent mercury saturated adsorption capacity, the shortcomings such as the easy secondary of mercury comes off, make full use of the chemisorbed that gaseous elementary mercury forms physical absorption and forms with bromine in micropore, the invention provides a kind of preparation method of fume mercury-removing active carbon, preparation technology is convenient, product mercury removal performance is good, does not produce secondary pollution, is easy to the features such as commercialization.
Technical scheme:The preparation method of fume mercury-removing active carbon, comprises the steps: the first step, and raw material is removed surface chemistry group: by 100-200 DEG C of oven dry after the NaOH solution washing of 10wt.%～30wt.% for seed activity carbon feedstock; Second step, dipping halide salt: raw material active carbon and the halide salt solution of removing surperficial oxy radical are carried out to hybrid infusion stirring 4 ~ 12 hours according to the mass ratio of 1:1～1:5, filtration drying, obtains being loaded with the active carbon of halide salt, and the concentration of described halide salt solution is 10wt.%～50wt.%; The 3rd step, load halogen: the active carbon that is loaded with halide salt, as in U-shaped pipe, is formed to packed layer, inputted by packed layer top with 100-500mL/min band halogen air, maintain 1～10h under room temperature, obtain the active carbon of saturated load halogen; The 4th step adds the active carbon of saturated load halogen the volatilizable halogen of heat abstraction at 80～120 DEG C, prepares fume mercury-removing active carbon.
Solution described in the first step is NaOH solution, and concentration is 30wt.%.
In second step, halide salt is the one in potassium chloride, KBr, KI, and halide salt solution concentration is 15wt.%.
In the 3rd step, halogen is the one in chlorine, bromine, iodine, air mass flow 300mL/min.
In the 4th step, adding the volatilizable halogen temperature of heat abstraction is 110 DEG C, processing time 1h.
Active carbon prepared by the preparation method of described fume mercury-removing active carbon, halogen load capacity mass percent is 50%～100%, the clearance 80%～100% of mercury, the saturated extent of adsorption mass percent 80%～150% of mercury.
Beneficial effect:1. the preparation method of high effective flue gas removal of mercury active carbon, halogen load capacity is large, gas mercury saturated extent of adsorption high (mass ratio exceedes 100%), removal of mercury efficiency is high, and does not produce secondary pollution. 2. give full play to Elemental Mercury and oxidation state mercury in the micropore enrichment of active carbon and the chemisorption combined removal flue gas of halogen. 3. the NaOH solution of suitable concentration can effectively be removed surperficial oxy radical, and suitable surface pH value is conducive to the dipping of halide salt; 4. adopt suitable heat treatment temperature, can effectively remove unstable halogen, prevent the decomposition of halide salt simultaneously.
In concrete steps, adopt suitable NaOH solution can effectively remove Surface Chemistry of Activated Carbon group, cleaning inner surface, improves effective ratio area, gives full play to Accumulation with Activated Carbon effect; Meanwhile, suitable NaOH concentration both can reach the effect of removing oxy radical, can make again activated carbon surface be alkalescent, was conducive to the load of halide salt. Too high alkali concn can produce too much waste water simultaneously, is unfavorable for environmental protection.
Halogen is that 100% analysis is pure, and the concentration difference that different air capacities are carried must allow active carbon saturated adsorption halogen, could adsorb to greatest extent like this gas mercury. U-shaped pipe is in order to form certain malleation, increases load capacity.
Employing uniform temperature heating, can remove unstable halogen, can obtain the stable product of the removal of mercury, makes the abundant combination of halogen and halide salt, removes unconjugated halogen, makes product in the time of fume mercury-removing, can desorption, do not produce secondary pollution.
Brief description of the drawings
Fig. 1 micropore active carbon pore structure distribution map; The mesoporous scope of the active carbon pore distribution concentration 0-5nm selecting, after this pore diameter range load halogen, is very suitable for the absorption of gas mercury.
Fig. 2 active carbon pore structure surface topography mirror image figure; The coconut husk matrix activated carbon pore structure of selecting is very flourishing, is suitable for doing carrier active carbon.
The affect figure of Fig. 3 active carbon loadings on fume mercury-removing efficiency; The loadings of load halogen active carbon is larger to fume mercury-removing effectiveness affects, and along with the increase of loadings, removal of mercury efficiency increases.
The former active carbon of Fig. 4 and modified activated carbon demercuration efficiency chart; The removal efficiency of the active carbon of the different halogens of load to gas mercury, the active carbon that wherein carries bromine reaches as high as 95% to the removal efficiency of mercury, adsorbs the removal of mercury efficiency that still can preserve value high in 6 hours.
The former active carbon of Fig. 5 and the adsorption capacity figure of modified activated carbon to mercury. The activated carbon supported halogen modified adsorption capacity to gas mercury significantly improves, and carries bromine modified activated carbon the highest to the absorption affinity of gas mercury, secondly for carrying iodine modified activated carbon.
Detailed description of the invention
The active carbon raw material adopting in method of the present invention can comprise the samples such as cocoanut active charcoal, ature of coal column charcoal, steam method wood activated charcoal. The halogen load factor of removal of mercury active carbon of the present invention, mercury saturated adsorption performance, removal of mercury efficiency can be controlled by heat treatment temperature and the time of volatilizable halogen on the load capacity of the removal solution concentration of raw material microporosity, surface functional group, halide salt, air velocity, halogen load time, active carbon. By selecting the high business active carbon of micropore, first it is carried out to alkali liquid washing place to go surface group, with finite concentration halide salt Immesion active carbon oven dry, be filled in U-shaped pipe, then active carbon carried out to gas phase load, coutroi velocity and load time with air load halogen, adsorb saturated after, load type active carbon is heat-treated at a certain temperature, remove volatilizable bromine, prepare high effective flue gas removal of mercury active carbon. Result of the test is as shown in Fig. 4-5.
The method of testing of the absorption property of the present invention to prepared active carbon and specific area is as follows:
(1) MQ201 coal-fired flue-gas mercury vapourmeter for the mercury removal efficiency of active carbon.
(2) mercury of active carbon inductive coupling plasma emission spectrograph (PE company of the U.S. for saturated extent of adsorption, model optima7000) measure, Adsorption of Mercury is reached to saturated activity charcoal strong acid dissolution, measure the content of mercury in solution, calculate the saturated extent of adsorption of active carbon to mercury.
NaOH solution concentration 10wt.%～30wt.%, dipping halide salt solution concentration 10wt.%～50wt.%, air velocity 100-500mL/min, load time 1～5h, making active carbon halogen load capacity mass percent is 50wt.%～90wt.%, the clearance 80%～100% of mercury, mercury capacity mass percent 80wt.%～150wt.%.
Embodiment 1
(1) raw material is removed surface chemistry group: the NaOH solution washing by coconut husk base seed activity carbon feedstock with 10wt.%, 150 DEG C of oven dry.
(2) dipping halide salt: 30g active carbon raw material be impregnated in the Klorvess Liquid of mass concentration 15wt.%, stir filtration drying 4 hours.
(3) load halogen: by the active carbon that is loaded with potassium chloride as in U-shaped pipe, form packed layer, inputted by packed layer top with 300mL/min air band chlorine, chlorine gas concentration is 0.13mg/L, under room temperature, maintain 10h, chlorine molecule is evenly written in activated carbon capillary, and chlorine is combined with potassium chloride and is formed thermally-stabilised good terchoride KCl3。
(4) active carbon of load chlorine is heated at 110 DEG C to 1h and remove volatilizable halogen, prepare the good fume mercury-removing active carbon of thermally-stabilised good property. Carry chlorine dose 50wt.%, mercury saturated extent of adsorption 80wt.%, removal of mercury efficiency 86%(air-flow 4L/min in 72h, mercury concentration 10mg/m3）。
Embodiment 2
(1) raw material is removed surface chemistry group: the NaOH solution washing by coconut husk base seed activity carbon feedstock with 30wt.%, 150 DEG C of oven dry.
(2) dipping halide salt: 30g active carbon raw material be impregnated in the potassium bromide solution of mass concentration 20wt.%, stir filtration drying 12 hours.
(3) load halogen: by the active carbon that is loaded with KBr as in U-shaped pipe, form packed layer, inputted by packed layer top with 300mL/min air band bromine, bromine concentration is 0.21mg/L, under room temperature, maintain 10h, bromine molecule is evenly written in activated carbon capillary, and bromine is combined with KBr and is formed thermally-stabilised good tribromide KBr3。
(4) active carbon of load bromine is heated at 110 DEG C to 2h and remove volatilizable bromine, prepare the good fume mercury-removing active carbon of thermally-stabilised good property. Carry bromine amount 80wt.%, mercury saturated extent of adsorption 150wt.%, removal of mercury efficiency 100%(air-flow 4L/min in 72h, mercury concentration 10mg/m3）。
Embodiment 3
(1) raw material is removed surface chemistry group: the NaOH solution washing by coconut husk base seed activity carbon feedstock with 30wt.%, 150 DEG C of oven dry.
(2) dipping halide salt: 50g active carbon raw material be impregnated in the liquor kalii iodide of mass concentration 50wt.%, stir filtration drying 12 hours.
(3) load halogen: by the active carbon that is loaded with KI as in U-shaped pipe, form packed layer, inputted by packed layer top with 300mL/min air band iodine, iodine concentration is 0.23mg/L, under room temperature, maintain 10h, bromine molecule is evenly written in activated carbon capillary, and bromine is combined with KBr and is formed thermally-stabilised good teriodide KI3。
(4) active carbon of load iodine is heated at 100 DEG C to 1h and remove volatilizable iodine, prepare the fume mercury-removing active carbon of thermally-stabilised good property. Carry iodine amount 60wt.%, mercury saturated extent of adsorption 120wt.%, in 42h removal of mercury efficiency after 100%, 72 hour removal of mercury rate be down to 78%(air-flow 4L/min, mercury concentration 10mg/m3）。
Embodiment 4
(1) raw material is removed surface chemistry group: the NaOH solution washing by coconut husk base seed activity carbon feedstock with 10wt.%, 150 DEG C of oven dry.
(2) dipping halide salt: do not flood halide salt.
(3) load halogen: active carbon, as in U-shaped pipe, is formed to packed layer, inputted by packed layer top with 300mL/min air band chlorine, chlorine gas concentration is 0.13mg/L, maintains 10h under room temperature, and chlorine molecule is evenly written in activated carbon capillary.
(4) active carbon of load chlorine is heated at 110 DEG C to 1h and remove volatilizable halogen. Carry chlorine dose 5wt.%, mercury saturated extent of adsorption 1wt.%, the removal of mercury is most effective 46%, and 3h reaches absorption saturated (air-flow 4L/min, mercury concentration 10mg/m3）。
Embodiment 5
Klorvess Liquid concentration in embodiment 1 is changed to 50wt.%, and all the other obtain carried by active carbon chlorine dose 43wt.% with embodiment 1, mercury saturated extent of adsorption 70wt.%, removal of mercury efficiency 90%(air-flow 4L/min in 72h, mercury concentration 10mg/m3）。
Embodiment 6
Change the bromine time of carrying in embodiment 2 into 5h, all the other obtain carried by active carbon bromine amount 67wt.% with embodiment 2, mercury saturated extent of adsorption 110wt.%, removal of mercury efficiency 84%(air-flow 4L/min in 72h, mercury concentration 10mg/m3）。
Embodiment 7
Liquor kalii iodide concentration in embodiment 3 is changed to 30wt.%, and all the other obtain carried by active carbon iodine amount 53wt.% with embodiment 3, mercury saturated extent of adsorption 107wt.%, removal of mercury efficiency 62%(air-flow 4L/min after 72h, mercury concentration 10mg/m3）。
Claims (5)
1. the preparation method of fume mercury-removing active carbon, is characterized in that, comprises the steps:
The first step, raw material is removed surface chemistry group: by 100-200 DEG C of oven dry after the NaOH solution washing of 10wt.%～30wt.% for seed activity carbon feedstock;
Second step, dipping halide salt: raw material active carbon and the halide salt solution of removing surperficial oxy radical are carried out to hybrid infusion stirring 4 ~ 12 hours according to the mass ratio of 1:1～1:5, filtration drying, obtains being loaded with the active carbon of halide salt, and the concentration of described halide salt solution is 10wt.%～50wt.%;
The 3rd step, load halogen: the active carbon that is loaded with halide salt is placed in to U-shaped pipe, forms packed layer, inputted by packed layer top with 100-500mL/min band halogen air, maintain 1～10h under room temperature, obtain the active carbon of saturated load halogen;
The 4th step adds the active carbon of saturated load halogen the volatilizable halogen of heat abstraction at 80～120 DEG C, prepares fume mercury-removing active carbon.
2. the preparation method of fume mercury-removing active carbon as claimed in claim 1, is characterized in that, the solution described in the first step is NaOH solution, and concentration is 30wt.%.
3. the preparation method of fume mercury-removing active carbon as claimed in claim 1, is characterized in that, in second step, halide salt is the one in potassium chloride, KBr, KI, and halide salt solution concentration is 15wt.%.
4. the preparation method of fume mercury-removing active carbon as claimed in claim 1, is characterized in that, in the 3rd step, halogen is the one in chlorine, bromine, iodine, band halogen air mass flow 300mL/min.
5. the preparation method of fume mercury-removing active carbon as claimed in claim 1, is characterized in that, in the 4th step, adding the volatilizable halogen temperature of heat abstraction is 110 DEG C, processing time 1h.
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| CN105363067B (en) * | 2015-12-24 | 2018-08-10 | 上海复榆医药科技有限公司 | A kind of hemostasis sterilization wound treatment agent and preparation method thereof |
| CN105561924A (en) * | 2016-01-29 | 2016-05-11 | 北京市劳动保护科学研究所 | Preparation method and application of modified activated carbon adsorbing agent for mercury in flue gas and collection tube of modified activated carbon adsorbing agent |
| GB201711157D0 (en) | 2017-07-11 | 2017-08-23 | Univ Liverpool | Sulfur-Doped Carbonaceous porous materials |
| CN108554382B (en) * | 2018-03-14 | 2020-09-25 | 河南正清环境科技有限公司 | Halogenated modified activated carbon material and preparation method thereof |
| CN110404505B (en) * | 2018-04-27 | 2021-06-08 | 中国矿业大学(北京) | Preparation method of activated carbon for measuring gaseous mercury and activated carbon |
| CN115739018A (en) * | 2022-11-15 | 2023-03-07 | 中盐金坛盐化有限责任公司 | Preparation method and application of molten salt method sulfur modified porous material |
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| CN103223330A (en) * | 2013-05-13 | 2013-07-31 | 中国林业科学研究院林产化学工业研究所 | Preparation method of special modified active carbon for removing mercury |
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