CN105344309B - Mercury removal agent and preparation method thereof with nanometer laminated structure - Google Patents
Mercury removal agent and preparation method thereof with nanometer laminated structure Download PDFInfo
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Abstract
The present invention provides a kind of mercury removal agent with nanometer laminated structure, it is prepared through infusion process with the method that sulphur-gas phase reaction combines by active component and carrier, wherein active component accounts for mass percent 0.5-20%, carrier is to account for mass percent 80-99.5%, the active component is two chalcogenide of transition metal with nanometer laminated structure, and the specific surface area of the carrier is greater than 10m2/g.The mercury removal agent can be not only used for that coal-burning power plant, coal heating boiler, oil refining factory industry, chemical industry, steel and non-ferrous metal metallurgy industry, cement industry, waste incineration and generating electricity and heavy metal pollution soil are administered and the exhaust gas demercuration of recovery project, and can be used for the demercuration of the related gas-purification industry of the fossil energies such as coke-stove gas, water-gas, natural gas and shale gas.
Description
Technical field
The present invention relates to flue gas, exhaust gas, industrial gasses and gas-purification technical fields, and in particular to one kind can be not only used for firing
Coal-fired plant, coal heating boiler, oil refining factory industry, chemical industry, steel and non-ferrous metal metallurgy industry, cement industry,
Waste incineration and generating electricity and heavy metal pollution soil are administered and the exhaust gas demercuration of recovery project, and can be used for coke-oven coal gas and water coal
The adsorbent of the related gas-purification industry demercuration of the fossil energies such as gas, natural gas and shale gas.
Background technique
A large amount of use of fossil resource results in global atmospheric environment problem.Coal-burning power plant, coal-burning boiler, petroleum refining
Change factory's industry, chemical industry, steel and non-ferrous metal metallurgy industry, waste incineration and generating electricity and heavy metal pollution soil are administered and
Gas related to the fossil energies such as coke-stove gas, water-gas, natural gas and shale gas in the process gas of recovery project, flue gas and exhaust gas
All contain heavy metal Hg in body.
Mercury with hypertoxicity, effumability, persistence and deposition in vivo due to becoming after sulfur dioxide
With the toxic carcinogenic contaminant of atmosphere of greatest concern after nitrogen oxides.Mercury causes very big harm to organism and environment, from
The mercury of above-mentioned industry release can propagate hundreds of kilometer in air, penetrate into the links of food chain, fish, crops, family
Poultry, even if quite remote from mercury pollution source, all none is infected with escaping by luck.Because mercury organism can react shape after absorbing mercury in vivo
At the methyl mercury of severe toxicity, methyl mercury can form mercaptides in conjunction with the sulfydryl of enzyme, the activity of enzyme is caused to be suppressed, to destroy
The analytic metabolism function of biological cell.Afterbody of the mankind as food chain, the mercury in other biological body is by being enriched with
After can be recycled into human body, a series of health problem can be caused, it is even dead such as heart disease, cerebral injury.
Environmental problem is by international concern caused by mercury emissions.In recent years, start the discharge to mercury in global range to formulate
Discharge standard, such as the U.S. and China.In December, 2014, Environmental Protection Agency announce national new standard, it is desirable that Utilities Electric Co.
It must be equipped with technology within 3 to 4 years futures, effectively reduce mercury pollution.Big country one of of the China as global mercury emissions, from 2015
January in year comes into effect new discharge standard (GB 13223-2011), limits the discharge of coal-burning power plant's mercury for the first time, also has processing
The top priority for being placed on National Environmental and administering project of noxious material.Therefore, the research and development of demercuration adsorbent have become research
Hot spot.
Currently, mainly there is the type of adsorbent in Chinese granted patent: active carbon (CN201010176708.4);Bromine is modified
Carbonaceous material (CN03816017.X);Magnesium-modified active carbon (CN200710120175.6);Sulfur loading active carbon
(CN200810237190.3, CN200910103024.9);Flying dust/absorbent charcoal composite material (CN201110039619.X);It is swollen
Moisten soil, iodine, chitosan and sulfuric acid synthetic material (CN200910061319.4);Biomass char is produced in seaweed pyrolysis
(CN201420687292.6);The modified biomass pyrolytic of ammonium halide salt is burnt (CN201010553069.9);Load Fe, Zn and Pd
γ-the Al2O3 (CN201110344268.3) of metal oxide;Load the active al2o3 of nickel oxide and copper oxide
(CN201310254794.X)。
In recent years, two-dimentional two chalcogenide of transition metal (Two-Dimensional Transition Metal
Dichalcogenides), because having special two-dimentional class graphene layer structure, become current research hotspot.Compared to stone
Black alkene, two-dimentional two chalcogenide of transition metal inherently has chemical activity point abundant, and graphene can only be used as other
Active component carrier could have extraordinary chemical activity.Two-dimentional two chalcogenide of transition metal shows very outstanding chemicals
Rationality matter is with a wide range of applications in each field, including such as field-effect of catalysis, energy stores, sensing and electronic device is brilliant
The fields such as body pipe and logic circuit.
However, being inhaled at present by the demercuration in activated centre of two chalcogenide of two-dimentional transition metal with nanometer laminated structure
Attached dose of research is rarely reported both at home and abroad.
Summary of the invention
The technical problem to be solved by the present invention is to be directed to the above prior art, a kind of new and effective demercuration absorption is provided
Agent, the mercury removal agent can not only be recycled, but also mercury resource is recycled while adsorbent reactivation.
The technical scheme adopted by the invention is as follows:
A kind of mercury removal agent with nanometer laminated structure, the mercury removal agent is by active component and carrier through infusion process and sulphur-gas
The method that phase reaction combines is prepared, and wherein active component accounts for mass percent 0.5-20%, carrier is to account for quality percentage
Than 80-99.5%, the active component is two chalcogenide of transition metal with nanometer laminated structure, the ratio table of the carrier
Area is greater than 10m2/g。
Two chalcogenide of transition metal is the compound being made of transition metal and element sulphur (S), the transition gold
Belong to the mixing for one or more of molybdenum (Mo), tungsten (W), tantalum (Ta), titanium (Ti), zirconium (Zr), so two chalcogen of transition metal
Compound is molybdenum sulfide (MoS2), tungsten sulfide (WS2), vulcanization tantalum (TaS2), titanium sulfide (TiS2), vulcanization zirconium (ZrS2) one of or
Several mixing.
The specific surface area is greater than 10m2The carrier of/g is activated alumina, TiO2, the organic bone of silica, silica gel, metal
Frame material (MOF), zeolite imidazole ester frame structure material (ZIF), molecular sieve, active carbon, graphene, in natural minerals carrier
One or more of mixing, wherein natural minerals carrier is one of diatomite, kaolin, natural pumice, expanded perlite
Or several mixing.
The present invention further provides the preparation methods of the above-mentioned mercury removal agent with nanometer laminated structure, specifically include following step
It is rapid:
(1) pore volume for measuring carrier first, further measures carrier inhalation solution according to carrier pore volume preliminary survey result
Ability, as need to prepare the amount of maceration extract;
(2) amount that corresponding active component presoma is conversed according to the proportion of active component and carrier, before active component
It drives body to be dissolved in the water at a temperature of 40-60 DEG C, is configured to the maceration extract of step (1) measured quantity;
(3) above-mentioned prepared maceration extract is uniformly sprayed at carrier surface, inhales the capillary channel of carrier by maceration extract
Enter in duct;
(4) dry 1-36 hours at a temperature of -135 DEG C of room temperature, then 250-620 DEG C temperature lower calcination 1-20 hours, obtain
To the carrier of uniform load transition metal oxide;
(5) carrier for the one or more transition metal oxide loads by calcining for obtaining step (4) is in H2S and
H2Mixed gas in, vulcanize 1 to 10 hours at 300-450 DEG C, transition metal oxide is vulcanized as two sulphur of transition metal
Belong to compound, for two chalcogenide uniform load of transition metal on the carrier of above-mentioned bigger serface, being formed has nano lamellar knot
The mercury removal agent of structure.
Active component presoma is metal ammonium salt or metal nitrate or metal carbonate in the step (2) or other contain
The substance of active component metals element.
The carrier gas calcined in the step (4) is air or nitrogen or argon gas or helium or carbon dioxide.
H in step (5) mixed gas2It is 1-65%, H that S, which accounts for percent by volume,2Accounting for percent by volume is 35-99%.
The carrier for the carrying transition metal oxide that the step (4) obtains can also further add it before vulcanization
His reactive metal oxides, the reactive metal oxides account for carrier quality percentage 0.05-15%, and wherein metal is cobalt
(Co), one of copper (Cu), manganese (Mn), chromium (Cr), iron (Fe), nickel (Ni), tin (Sn), magnesium (Mg), cerium (Ce), ruthenium (Ru) or
The same step of step (2)-(4) are added in several mixing.
Compared with prior art, the present invention has following remarkable advantage and the utility model has the advantages that a kind of first public tool of the present invention
There is the mercury removal agent of this nanometer laminated structure, nanometer laminated structure makes the adsorbent have superpower mercury adsorption capacity, both can be used
In coal-burning power plant, coal heating boiler, oil refining factory industry, chemical industry, steel and non-ferrous metal metallurgy industry, rubbish are burnt
It burns power generation and heavy metal pollution soil is administered and process gas, flue gas and the exhaust gas demercuration of recovery project, and can be used for coke-oven coal
The related gas-purification industry demercuration of the fossil energies such as gas and water coal gas, natural gas and shale gas.
Detailed description of the invention
Shown in FIG. 1 is the preparation flow figure of the mercury removal agent in the embodiment of the present invention 1 with nanometer laminated structure;
Shown in Fig. 2 is characterization of the obtained mercury removal agent of the embodiment of the present invention 1 at high resolution TEM (HRTEM)
As a result;
Shown in Fig. 3 is the adsorbent activity test result for the mercury removal agent that the embodiment of the present invention 1 obtains.
Specific embodiment
The present invention is further described in detail with reference to embodiments.It is noted that detailed description below is all to illustrate
Property, it is intended to further instruction is provided to the present invention.Unless otherwise indicated, all scientific and technical terms that the present invention uses
With with the normally understood identical meanings of the technical field of the invention personnel.
Embodiment 1:
The selection spherical gama-alumina of 40g is carrier.Its pore volume is measured first, is surveyed again according to pore volume preliminary survey result
The ability of its fixed carrier inhalation solution, as needs required active constituent load capacity to prepare the amount for impregnating all solution.Second step,
By the ammonium molybdate ((NH relative to carrier quality 10%4)6Mo7O24·4H2O) this load is dissolved in as the active component of adsorbent
Amount of solution needed for body thorough impregnation is loaded on this spherical gamma-aluminium oxide carrier and is carried out;It is subsequently placed in drying box at 120 DEG C
Lower drying for 24 hours, calcines 12h in air atmosphere at 500 DEG C in Muffle furnace.Third step, second of dipping, using similar approach
It will be relative to the cobalt nitrate of carrier quality 5% (Co (NO3)2·6H2O it) loads on the adsorbent calcined for the first time, then again
By processes such as dry and roastings.Final step, adsorbent is in 5vol%H2S/H2Vulcanization 3h is carried out at 390 DEG C under atmosphere, it will be golden
Category oxide curative is metal sulfide, forms the mercury removal agent with nanometer laminated structure.The CoMoS/Al of vulcanization is made2O3It inhales
Attached dose.Its preparation process schematic diagram is as shown in Figure 1.Characterization of the prepared adsorbent through high resolution TEM (HRTEM)
As a result confirm that this material has MoS2The active component Co of nanometer laminated structure, addition is modified in this layer structure, such as Fig. 2 institute
Show.
Active testing, test result are carried out using mercury removal agent adsorbent of the U.S. Tekran mercury on-line analysis system to preparation
As shown in figure 3, mercury removal rate is almost stable 100% in test in 2000 minutes.Confirm that this adsorbent has super-active.
Integral calculation has the mercury of 45.31 μ g/g to be adsorbed in this adsorbent the results show that in this is 2000 minutes.
Embodiment 2:
Choosing 40g zeolite imidazole ester frame structure material (ZIF) is carrier.Its pore volume is measured first, according to pore volume
Preliminary survey result measures the ability of its carrier inhalation solution again, as needs to prepare the amount for impregnating all solution.Second step, by phase
For the ammonium metatungstate ((NH4) of carrier quality 5%6H2W12O40NH2O) this carrier is dissolved in as the active component of adsorbent
Amount of solution needed for thorough impregnation is loaded on this zeolite imidazole ester frame structure material carrier and is carried out;It is subsequently placed in drying box
Drying for 24 hours, calcines 20h in helium atmosphere at 350 DEG C in Muffle furnace at 120 DEG C.Third step, second of dipping, uses
Similar approach is by the manganese nitrate Mn (NO3) relative to carrier quality 2%24H2O loads to the adsorbent calcined for the first time
On, then drying and calcining etc. processes.Final step, adsorbent is in 5vol%H2S/H2In 350 DEG C of progress sulphur under atmosphere
Change 4h, is metal sulfide by metal oxide vulcanization, forms the mercury removal agent with nanometer laminated structure.Vulcanization is made
MnWS/ZIF adsorbent.
Embodiment 3:
Selection 40g molecular sieve is carrier.Its pore volume is measured first, its carrier is measured according to pore volume preliminary survey result again
The ability of inhalation solution as needs to prepare the amount for impregnating all solution.Second step, by the inclined titanium relative to carrier quality 6%
Acid (H2TiO3) as adsorbent active component be dissolved in this carrier thorough impregnation needed for amount of solution to load to this molecular sieve supported
It is carried out on body;The drying at 120 DEG C is subsequently placed in drying box for 24 hours, to calcine in air atmosphere at 520 DEG C in Muffle furnace
12h.Third step, second impregnates, and using similar approach is by the copper nitrate Cu (NO relative to carrier quality 3%3)2·3H2O is negative
It is downloaded on the adsorbent calcined for the first time, then the processes such as drying and roasting.Final step, adsorbent is in 5vol%
H2S/H2Vulcanization 3h is carried out at 400 DEG C under atmosphere, is metal sulfide by metal oxide vulcanization, being formed has nano lamellar knot
The mercury removal agent of structure.The CuTiS/ adsorbent of molecular sieve of vulcanization is made.
Embodiment 4:
Selection 40g graphene is carrier.Its pore volume is measured first, its carrier is measured according to pore volume preliminary survey result again
The ability of inhalation solution as needs to prepare the amount for impregnating all solution.Second step, by the nitric acid relative to carrier quality 2%
Oxygen zirconium (ZrO (NO3)2·2H2O the load of amount of solution needed for) being dissolved in this carrier thorough impregnation as the active component of adsorbent
It is carried out on to this molecular sieve carrier;Be subsequently placed in drying box at 100 DEG C it is dry for 24 hours, in Muffle furnace at 300 DEG C nitrogen
12h is calcined in atmosphere.Third step, second impregnates, and using similar approach is by the copper nitrate Ni relative to carrier quality 3%
(NO3)2·6H2O is loaded on the adsorbent calcined for the first time, then the processes such as drying and calcining.Final step,
Adsorbent is in 5vol%H2S/H2Vulcanization 4h is carried out at 300 DEG C under atmosphere, is metal sulfide by metal oxide vulcanization, is formed
Mercury removal agent with nanometer laminated structure.The NiZrS/ graphene adsorbent of vulcanization is made.
Corresponding mercury adsorption activity test is equally carried out to the mercury removal agent that embodiment 2-4 is obtained, is attained by and 1 phase of embodiment
When mercury adsorption capacity.
The present embodiments relate to the material arrived, reagent and experimental facilities, are to meet demercuration absorption unless otherwise instructed
The commercial product of agent technical field.
The above is merely a preferred embodiment of the present invention, it is noted that for those skilled in the art
For, under the premise of not departing from core of the invention technology, improvements and modifications can also be made, these improvements and modifications are also answered
Belong to scope of patent protection of the invention.With any change in the comparable meaning and scope of claims of the present invention, all
It is considered as being included within the scope of the claims.
Claims (6)
1. a kind of mercury removal agent with nanometer laminated structure, it is characterised in that: by transition metal precursor, before other active metals
It drives body and carrier is prepared through infusion process with the method that sulphur-gas phase reaction combines, the active component of the mercury removal agent is served as reasons
Transition metal oxide and the vulcanization of other reactive metal oxides are prepared, and the transition metal oxide is after over cure
Two chalcogenide of transition metal with nanometer laminated structure, i.e. molybdenum sulfide, vulcanization tantalum, titanium sulfide, vulcanize in zirconium tungsten sulfide
One or more of mixing;The specific surface area of the carrier is greater than 10 ㎡/g;With two chalcogenide of transition metal in mercury removal agent and
On the basis of second seals' total amount, two chalcogenide of transition metal accounts for mass percent 0.5-20%, carrier is to account for mass percent
80-99.5%;
The preparation method of the mercury removal agent includes the following steps:
(1) pore volume for measuring carrier first, the energy of carrier inhalation solution is further measured according to carrier pore volume preliminary survey result
Power as needs to prepare the amount of maceration extract;
(2) corresponding transition metal precursor is conversed to the proportion of carrier according to two chalcogenide of transition metal in active component
Amount, transition metal precursor are dissolved in the water at a temperature of 40-60 DEG C, are configured to the maceration extract of step (1) measured quantity;
(3) above-mentioned prepared maceration extract is uniformly sprayed at carrier surface, makes the capillary channel of carrier by maceration extract inlet hole
In road;
(4) dry 1-36 hour at a temperature of -135 DEG C of room temperature, then 250-620 DEG C temperature lower calcination 1-20 hours, obtain equal
The carrier of even carrying transition metal oxide;
(5) other reactive metal oxides are further added, the reactive metal oxides account for carrier quality percentage 0.05-
15%, wherein metal is cobalt (Co), copper (Cu), manganese (Mn), chromium (Cr), iron (Fe), nickel (Ni), tin (Sn), magnesium (Mg), cerium
(Ce), the same step of step (2)-(4) are added in the mixing of one or more of ruthenium (Ru);
(6) the one or more carriers by calcining for obtaining step (5) are in H2S and H2Mixed gas in, in 300-450
Vulcanize 1 to 10 hours at DEG C, transition metal oxide is vulcanized as two chalcogenide of transition metal, being formed has nano lamellar knot
The mercury removal agent of structure.
2. the mercury removal agent according to claim 1 with nanometer laminated structure, it is characterised in that: the carrier is active oxygen
Change aluminium, TiO2, silica, silica gel, metal-organic framework materials, zeolite imidazole ester frame structure material, molecular sieve, activity
The mixing of one or more of charcoal, graphene, natural minerals carrier.
3. the mercury removal agent according to claim 2 with nanometer laminated structure, it is characterised in that: the natural minerals carrier
For the mixing of one or more of diatomite, kaolin, natural pumice, expanded perlite.
4. the mercury removal agent according to claim 1 with nanometer laminated structure, it is characterised in that: mistake in the step (2)
Crossing metal precursor is metal ammonium salt or metal nitrate or metal carbonate or other substances for containing transition metal element.
5. the mercury removal agent according to claim 1 with nanometer laminated structure, it is characterised in that: forged in the step (4)
The carrier gas of burning is air or nitrogen or argon gas or helium or carbon dioxide.
6. the mercury removal agent according to claim 1 with nanometer laminated structure, it is characterised in that: step (6) mixing
H in gas2It is 1-65%, H that S, which accounts for percent by volume,2Accounting for percent by volume is 35-99%.
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CN107715854A (en) * | 2017-10-23 | 2018-02-23 | 天津大学 | For modified Nano zeroth order iron complexes containing heavy metal ion and the Industrial Wastewater Treatment of organic matter and preparation method thereof |
CN108187451B (en) * | 2018-01-29 | 2020-06-26 | 中南大学 | Method for removing gaseous elementary mercury from nano molybdenum sulfide material by wet method |
CN108246237A (en) * | 2018-03-23 | 2018-07-06 | 上海电力学院 | A kind of demercuration molybdenum base adsorbent and preparation method thereof |
CN108686710B (en) * | 2018-05-15 | 2021-02-23 | 西京学院 | Two-dimensional metal organic framework/molybdenum disulfide nano composite electro-catalytic hydrogen evolution material and preparation method thereof |
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