CN110115972A - A kind of structural formula adsorbent material and preparation method thereof removing mercury in flue gas - Google Patents

A kind of structural formula adsorbent material and preparation method thereof removing mercury in flue gas Download PDF

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CN110115972A
CN110115972A CN201910410005.4A CN201910410005A CN110115972A CN 110115972 A CN110115972 A CN 110115972A CN 201910410005 A CN201910410005 A CN 201910410005A CN 110115972 A CN110115972 A CN 110115972A
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foam metal
adsorbent material
mercury
structural formula
foam
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CN110115972B (en
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杨建平
李琴
李海龙
屈文麒
胡迎超
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Central South University
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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
    • 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
    • B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
    • 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
    • B01J20/0233—Compounds of Cu, Ag, Au
    • B01J20/0237—Compounds of Cu
    • 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
    • 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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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Treating Waste Gases (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention discloses a kind of structural formula adsorbent materials and preparation method thereof for removing mercury in flue gas.Structural formula adsorbent material of the invention loads selenides on foam metal using foam metal as carrier in situ；Foam metal is one of foam copper, nickel foam.It is made by foam metal and sodium hydrogen selenide NaHSe solution ultrasound selenylation reaction in situ.Adsorbent material of the invention has good permeability and mechanical performance, it can be not only made into honeycomb, plank frame is also constituted, demercuration in flue can be arranged in, the mercury solved in coal-fired flue-gas is shifted into flying dust and desulfuration byproduct, realizes the disposable efficient removal of coal-fired flue-gas mercury；The adsorbent material also has good anti-SO simultaneously2And H2O performance is suitable for flue gas during smelting demercuration.

Description

A kind of structural formula adsorbent material and preparation method thereof removing mercury in flue gas
Technical field
The invention belongs to mercury in flue gas removing sulfuldioxide fields, and in particular to a kind of structural formula adsorption material for removing mercury in flue gas Material and preparation method thereof.
Background technique
Mercury is a kind of neurotoxic substance, has extremely strong cumulative bad and irreversibility, has very big threat to human health. Fire coal is one of most important artificial mercury emissions source.On August 16th, 2017 has the " water about mercury of global legally binding Yu pact " it is formally effective, pact regulation, it is necessary to take measures to coal-burning boiler, flue gas during smelting, control and reduce mercury in flue gas and The discharge of its compound.Mercury mainly exists in the form of 3 kinds in flue gas, is respectively as follows: Elemental Mercury (Hg0), oxidation state mercury (Hg2+) and Particle mercury (Hgp).Wherein particle mercury (Hgp) can be captured by dust-extraction unit, and oxidation state mercury (Hg2+) soluble easily in water, it can quilt Wet flue gas purifier efficiently removes, and Elemental Mercury (Hg0) because of its highly volatile and not soluble in water, it is difficult with existing cigarette Flash Gas Compression Skid System directly removes.Therefore, Hg0Emphasis and problem as flue gas mercuric pollution treatment.
Active carbon injection is coal-fired flue gas mercury removal technology more mature at present, however, to reach higher demercuration efficiency, Need to spray into a large amount of active carbon, high cost limits its application at home, and its active carbon introduced will affect The use of flying dust, to limit its large-scale commercial application.In view of active carbon spraying technique shortcomings with work The characteristic of property charcoal itself is related, and many non-carbon adsorbing materials are developed for flue gas demercuration, such as flying dust, zeolite, metal oxygen Compound etc. generallys use halogen, sulphur, noble metal etc. and is modified processing to adsorbent to obtain higher demercuration efficiency.But It is that the affinity of these materials and mercury is usually lower, causes adsorption efficiency limited.In addition, although sorbent injection technology can Mercury effectively in removing flue gas, but this part mercury is transferred in flying dust or desulfuration byproduct.Flyash, desulfurized gypsum etc. are all It is the important raw materials for production of the industries such as building materials, the enrichment of mercury is undoubtedly by the pollution transfer of mercury to other industrial processes, not There is the thorough improvement for really realizing coal-fired mercury pollution.The adsorbent material of structuring can effectively reduce the mercury in flue gas to flying dust and take off The disposable efficient removal of Mercury In Coal Combustion Flue Gas is realized in transfer in sulphur byproduct.Currently, ceramic honey comb and molding anatase TiO2Structural carrier be widely used to prepare catalyst, generallys use infusion process for active component and loads to structural formula load On body, but the mechanical strength of these carriers is lower, mass transfer rate is slower, and active component is not strong for load solid, uneven.
Mercury concentration is higher by thousands of times of concentration of coal-fired flue-gas mercury in flue gas during smelting, and at the same time the SO containing high concentration2.It smelts Flue gas demercuration technology mainly includes liquid phase oxidation absorption process and adsorbent absorption method.Typical liquid phase oxidation absorption process includes chlorination Mercury absorption process, liquor natrii hypochloritis's absorption process, pyrolusite-sulfuric acid absorption method, liquor potassic permanganate absorption process and iodine complexing are inhaled Receipts method etc., principle be nonvalent mercury is oxidized to by bivalent mercury by oxidant, or mercury is complexed as water-soluble complex compound, and And then it is absorbed by solution.For such method although mercury removal rate with higher, operating cost is high, and there is useless absorbing liquid Safe disposal problem.In addition, can also be removed by absorption method to the mercury in flue gas during smelting, including selenium filter method, carbon Filter method, sodium polysulfide absorption method, these methods are to SO2And H2O is extremely sensitive, limits its application.
Summary of the invention
Aiming at the above defects or improvement requirements of the prior art, the present invention provides a kind of structural formulas for removing mercury in flue gas Adsorbent material and preparation method thereof.The present invention prepares selenides modification using foam metal as carrier, using selenizing method in situ Foam metal, active component securely, equably load on foam metal；The adsorbent material and mercury have strong affinity, absorption Capacity is big, the rate of adsorption is fast；The good permeability of the adsorbent material and mechanical performance can not only be made into honeycomb, also constitute plate Formula structure can be arranged in demercuration in flue, and the mercury solved in coal-fired flue-gas is shifted into flying dust and desulfuration byproduct, real The disposable efficient removal of existing coal-fired flue-gas mercury；The adsorbent material also has good anti-SO2And H2O performance is suitable for smelting cigarette Qi exhaustion mercury.
Technical solution of the present invention is specifically described as follows.
The present invention provides a kind of structural formula adsorbent material for removing mercury in flue gas, using foam metal as carrier, foam gold Load selenides in situ on category；Foam metal is one of foam copper, nickel foam.
Preferably, the porosity of foam metal is 60%-90%.
Preferably, structural formula adsorbent material is by foam metal and sodium hydrogen selenide NaHSe solution ultrasound selenylation reaction system in situ ?.
The present invention further provides a kind of preparation methods according to above-mentioned structural formula adsorbent material, the specific steps are as follows:
(1) foam metal is ultrasonically treated in hydrochloric acid solution certain time, be then washed with deionized for several times, to remove Defoam the impurity of metal surface；
(2) by selenium powder and sodium borohydride NaBH4It is dissolved in deionized water and is heated to dissolving, obtain NaHSe solution；
(3) foam metal is immersed in NaHSe solution, ultrasonic treatment is taken out after a certain period of time, is then washed with deionized water It washs for several times, obtains structural formula adsorbent material after dry.
Preferably, in step (1), concentration of hydrochloric acid 0.1-3mol/L, sonication treatment time 5-60min.
Preferably, the molar ratio of foam metal and selenium powder is 1:0.2-1:2.
Preferably, in step (2), selenium powder and NaBH4Molar ratio be 1:1-1:5, heating temperature be 60-120 DEG C；Step (3) in, sonication treatment time 20-120min.
A kind of structural formula adsorbent material removing mercury in flue gas provided by the invention, the i.e. foam metal of selenides modification, It can be used for removing the Elemental Mercury in coal-fired flue-gas, have strong affinity with mercury, adsorption capacity can reach 148.19- 280.36mg·g-1, it is 154-705 times of different commercial activated carbons, the rate of adsorption can achieve 44.8-96.4 μ gg-1· min-1, it is 89-1659 times of active carbon；The material can be made into honeycomb, also constitute plank frame, be arranged in flue The mercury in flue gas can effectively be adsorbed.The position of the adsorbent material can specifically include depending on the actual conditions of power plant Deduster is front/rear, desulfurizer is front/rear, wet electrical dust precipitator is front/rear.
It is provided in the present invention a kind of for removing the structural formula adsorbent material of mercury in flue gas, there is good anti-SO2With H2O performance is suitable for high SO2And H2The flue gas during smelting demercuration of O content.
In general, through the invention it is contemplated above technical scheme is compared with the prior art, have below beneficial to effect Fruit:
The present invention provides a kind of structural formula adsorbent materials and preparation method thereof for removing mercury in flue gas.On the one hand, it utilizes Structural formula adsorbent material can realize the disposable efficient removal of Mercury In Coal Combustion Flue Gas, effectively reduce the mercury in flue gas to flying dust and take off Transfer in sulphur byproduct substantially reduces the secondary cost of disposal of mercury；On the other hand, selenizing method in situ, which simplifies, synthesized Journey avoids introducing adhesive layer between active component and carrier, can make active component securely, equably load to structural formula carrier I.e. on foam metal；In another aspect, there is foam metal excellent mechanical performance can inhale structural formula convenient for welding and cutting out Enclosure material is made into honeycomb, also constitutes plank frame, is adsorbed in flue gas in flue according to power plant's actual conditions flexible arrangement Mercury；In addition, the material has good anti-SO2And H2O performance is suitable for high SO2And H2The flue gas during smelting demercuration of O.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to Limit the present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below each other it Between do not constitute conflict and can be combined with each other.
Embodiment 1
(1) 1g foam copper is ultrasonically treated in 0.1M hydrochloric acid solution 5min, be then washed with deionized for several times, to remove Defoam the impurity on copper surface；
(2) by 0.248g selenium (Se) powder and 0.594g sodium borohydride (NaBH4) be dissolved in deionized water and be heated to 90 DEG C Dissolution obtains selenium hydrogenation and receives (NaHSe) solution；
(3) foam copper is immersed in above-mentioned NaHSe solution, is taken out after ultrasonic 20min, number is then washed with deionized It is secondary, Cu is obtained after dry2The foam copper of Se modification.
(4) by above-mentioned Cu2Se modification foam copper be used for coal-fired flue gas mercury removal, flue-gas temperature be 60 DEG C i.e. desulfurizer it Flue-gas temperature afterwards, the concentration of mercury in flue gas are 60 μ g/m3, demercuration efficiency can maintain 100% in 50h, and adsorbance reaches 240.92mg·g-1, it is 551 times of business chlorization activity charcoal, the rate of adsorption can achieve 69.4 μ gg-1·min-1, it is chlorination 569 times of active carbon.
Embodiment 2
(1) 1g foam copper is ultrasonically treated in 0.1M hydrochloric acid solution 5min, be then washed with deionized for several times, to remove Defoam the impurity on copper surface；
(2) by 1.242g selenium (Se) powder and 2.975g sodium borohydride (NaBH4) be dissolved in deionized water and be heated to 90 DEG C Dissolution obtains selenium hydrogenation and receives (NaHSe) solution；
(3) foam copper is immersed in above-mentioned NaHSe solution, is taken out after ultrasonic 20min, number is then washed with deionized It is secondary, the foam copper of CuSe modification is obtained after dry.
(4) the foam copper blast furnace off-gas demercuration for modifying above-mentioned CuSe, flue-gas temperature are 90 DEG C, and the concentration of mercury in flue gas is 600μg/m3, SO2Concentration is 5000ppm, H2O concentration is 8%, and demercuration efficiency can maintain 95% or more in 80h, adsorbance Reach 270.36mgg-1, it is 691 times of business bromination active carbon, the rate of adsorption can achieve 79.5 μ gg-1·min-1, it is 697 times of bromination active carbon.
Embodiment 3
(1) 1g nickel foam is ultrasonically treated in 1M hydrochloric acid solution 20min, be then washed with deionized for several times, to remove Defoam the impurity of nickel surface；
(2) by 1.345g selenium (Se) powder and 3.222g sodium borohydride (NaBH4) be dissolved in deionized water and be heated to 120 DEG C Dissolution obtains selenium hydrogenation and receives (NaHSe) solution；
(3) nickel foam is immersed in above-mentioned NaHSe solution, is taken out after ultrasonic 60min, number is then washed with deionized It is secondary, the nickel foam of NiSe modification is obtained after dry.
(4) the above-mentioned NiSe nickel foam modified is used for coal-fired flue gas mercury removal, flue-gas temperature be 120 DEG C i.e. dust-extraction unit it Preceding flue-gas temperature, the concentration of mercury in flue gas are 60 μ g/m3, demercuration efficiency can maintain 90% or more in 100h, and absorption is held Amount can reach 148.19mgg-1, it is 154 times of business sulfurate activity charcoal, the rate of adsorption can achieve 44.8 μ gg-1·min-1, it is 89 times of sulfurate activity charcoal.
Embodiment 4
(1) 1g nickel foam is ultrasonically treated in 2M hydrochloric acid solution 60min, be then washed with deionized for several times, to remove The impurity on the titanium that defoams surface；
(2) by 2.018g selenium (Se) powder and 4.834g sodium borohydride (NaBH4) be dissolved in deionized water and be heated to 120 DEG C Dissolution obtains selenium hydrogenation and receives (NaHSe) solution；
(3) nickel foam is immersed in above-mentioned NaHSe solution, is taken out after ultrasonic 60min, number is then washed with deionized It is secondary, Ni is obtained after dry2Se3The nickel foam of modification.
(4) by above-mentioned Ni2Se3The nickel foam of modification is used for flue gas during smelting demercuration, and flue-gas temperature is 90 DEG C, mercury in flue gas Concentration is 600 μ g/m3, SO2Concentration is 5000ppm, H2O concentration is 8%, and demercuration efficiency can maintain 95% or more in 30h, Adsorption capacity can reach 216.94mgg-1, it is 552 times of business bromination active carbon, the rate of adsorption can achieve 50.2 μ gg-1·min-1, it is 441 times of active carbon.

Claims (7)

1. a kind of structural formula adsorbent material for removing mercury in flue gas, which is characterized in that it is using foam metal as carrier, foam metal Upper load selenides in situ；Foam metal is one of foam copper, nickel foam.
2. structural formula adsorbent material according to claim 1, which is characterized in that the porosity of foam metal is 60%-90%.
3. structural formula adsorbent material according to claim 1, which is characterized in that it is by foam metal and sodium hydrogen selenide NaHSe solution ultrasound selenylation reaction in situ is made.
4. a kind of preparation method of structural formula adsorbent material according to claim 1, which is characterized in that specific steps are such as Under:
(1) foam metal is ultrasonically treated in hydrochloric acid solution certain time, be then washed with deionized for several times, to remove de-soak The impurity of foam metal surface；
(2) by selenium powder and sodium borohydride NaBH4It is dissolved in deionized water and is heated to dissolving, obtain NaHSe solution；
(3) foam metal is immersed in NaHSe solution, ultrasonic treatment is taken out after a certain period of time, and number is then washed with deionized It is secondary, structural formula adsorbent material is obtained after dry.
5. the preparation method according to claim 4, which is characterized in that in step (1), concentration of hydrochloric acid 0.1-3mol/L, Sonication treatment time is 5-60min.
6. the preparation method according to claim 4, which is characterized in that the molar ratio of foam metal and selenium powder is 1:0.2-1: 2。
7. the preparation method according to claim 4, which is characterized in that in step (2), selenium powder and NaBH4Molar ratio be 1: 1-1:5, heating temperature are 60-120 DEG C；In step (3), sonication treatment time 20-120min.
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Cited By (3)

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Publication number Priority date Publication date Assignee Title
CN110732303A (en) * 2019-12-05 2020-01-31 中南大学 transition metal selenide modified molding demercuration material and preparation method thereof
CN112028131A (en) * 2020-06-16 2020-12-04 暨南大学 Vulcanized nano zero-valent iron and preparation method and application thereof
CN115193389A (en) * 2022-06-29 2022-10-18 上海电力大学 Preparation method and application of selenide mercury removal adsorbent with lamellar structure

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110732303A (en) * 2019-12-05 2020-01-31 中南大学 transition metal selenide modified molding demercuration material and preparation method thereof
CN112028131A (en) * 2020-06-16 2020-12-04 暨南大学 Vulcanized nano zero-valent iron and preparation method and application thereof
CN112028131B (en) * 2020-06-16 2024-03-12 暨南大学 Vulcanized nano zero-valent iron and preparation method and application thereof
CN115193389A (en) * 2022-06-29 2022-10-18 上海电力大学 Preparation method and application of selenide mercury removal adsorbent with lamellar structure
CN115193389B (en) * 2022-06-29 2023-12-12 上海电力大学 Preparation method and application of selenide mercury-removal adsorbent with lamellar structure

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