CN106582252B - Flue gas desulfurization and mercury removal agent and preparation method thereof - Google Patents
Flue gas desulfurization and mercury removal agent and preparation method thereof Download PDFInfo
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- CN106582252B CN106582252B CN201611193668.8A CN201611193668A CN106582252B CN 106582252 B CN106582252 B CN 106582252B CN 201611193668 A CN201611193668 A CN 201611193668A CN 106582252 B CN106582252 B CN 106582252B
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- pyrolusite
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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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/81—Solid phase processes
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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
- 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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/48—Sulfur compounds
- B01D53/50—Sulfur oxides
- B01D53/508—Sulfur oxides by treating the gases with solids
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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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/64—Heavy metals or compounds thereof, e.g. mercury
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/10—Oxidants
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/60—Heavy metals or heavy metal compounds
- B01D2257/602—Mercury or mercury compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
- B01D2258/0283—Flue gases
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- Environmental & Geological Engineering (AREA)
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- Biomedical Technology (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
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- Exhaust Gas Treatment By Means Of Catalyst (AREA)
Abstract
The invention relates to a flue gas desulfurization and mercury removal agent and a preparation method thereof, wherein pyrolusite and Li are adopted2MnTiO4The manganese titanate is loaded on the carrier as an active component, and the proportion of the active component in the desulfurization and demercuration agent is controlled, so that the pore volume of the desulfurization and demercuration agent is high, the sulfur capacity and the mercury capacity reach more than 16.3 wt%, and the desulfurization and demercuration efficiency of the desulfurization and demercuration agent reaches more than 98%.
Description
Technical Field
The invention relates to a novel flue gas desulfurization and mercury removal agent and a preparation method thereof.
Background
Coal is the most abundant fossil fuel and the most basic and crude energy, and during combustion, it produces a large amount of pollutants with serious pollution to the atmosphere, such as dust, sulfur dioxide, nitrogen oxides, mercury components, and the like. The removal of sulfur dioxide and nitrogen oxides can cause acid rain to return to rivers and lakes on the ground surface, greatly influence the water demand quality of animals and plants, cause large-area industrial equipment corrosion, damage to the animals and plants, cause crop yield reduction and frequent occurrence of animal diseases; for the discharge of mercury components, methyl mercury is formed in organisms after the mercury components easily enter the organisms, the methyl mercury can inhibit the metabolism of the organisms, the health of the organisms is seriously threatened, and the method also belongs to the field of heavy metal pollution.
In view of this, in the prior art, it is greatly advocated to perform desulfurization and demercuration treatment on coal-fired flue gas to reduce the pollution to the environment caused by the emission of coal-fired flue gas, so that a large number of technologies related to desulfurization and demercuration appear, but most of desulfurization and demercuration technologies are individually treated aiming at desulfurization and demercuration, for example, lime water is used for absorbing sulfur dioxide for desulfurization, and an adsorbent is used for adsorption and demercuration, and the like. Nevertheless, most of the desulfurization and demercuration efficiencies in the prior art are still not ideal and are always maintained at about 70%, so that a large amount of sulfur dioxide and mercury components are still contained in the emission process of the flue gas.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a novel flue gas desulfurization and mercury removal agent and a preparation method thereof.
The method is realized by the following technical scheme:
a novel flue gas desulfurization and mercury removal agent comprises active components and a carrier, wherein the mass percent of the active components is 1-30%; the active component is Li2MnTiO4Manganese titanate and pyrolusite in any mass ratio different from zero.
The active component comprises the raw material components with the mass percentage of Li2MnTiO41-6% of manganese titanate, 15-37% of manganese titanate and the balance of pyrolusite.
The active component comprises the raw material components with the mass percentage of Li2MnTiO43 percent of manganese titanate, 25 percent of manganese titanate and the balance of pyrolusite.
The pyrolusite is treated by microwave radiation.
The microwave radiation has the microwave power of 100-300W and the radiation time of 10-30 min.
The pyrolusite is heated to the temperature of 300-600 ℃, and water is sprayed on the surface of the pyrolusite to pulverize the pyrolusite to obtain pyrolusite powder.
The carrier is molecular sieve, silicon dioxide or gamma-Al2O3。
The carrier has a specific surface area of 150-290m2A pore volume of 0.9 to 1.7 cm/g3/g。
The carrier has a specific surface area of 220m2G, pore volume of 1.3cm3/g。
The preparation method of the novel flue gas desulfurization and mercury removal agent comprises the following steps:
(1) putting pyrolusite at the temperature of 300-600 ℃, heating, and spraying water on the surface of the pyrolusite to pulverize the pyrolusite to obtain pyrolusite powder;
(2) mixing pyrolusite powder with Li2MnTiO4Mixing the manganese titanate and the water uniformly to prepare slurry with the liquid-solid ratio of 3-5: 1;
(3) soaking the carrier in the slurry for 2-3h, treating at 70-130 deg.C for 20-30min, and molding.
Compared with the prior art, the invention has the technical effects that:
the desulfurization and demercuration agent provided by the invention adopts pyrolusite and Li2MnTiO4The manganese titanate is loaded on the carrier as an active component, and the proportion of the active component in the desulfurization and demercuration agent is controlled, so that the pore volume of the desulfurization and demercuration agent is high, the sulfur capacity and the mercury capacity reach more than 16.3 wt%, and the desulfurization and demercuration efficiency of the desulfurization and demercuration agent reaches more than 98%.
The desulfurization and demercuration agent provided by the invention can be used for performing desulfurization and demercuration treatment on flue gas at a lower temperature, so that the problem that Li is easy to cause when flue gas is treated at a high temperature is avoided2MnTiO4And the decomposition avoids the inactivation of active components, improves the efficiency of desulfurization and demercuration, and reduces the dosage of the desulfurization and demercuration agent.
The pyrolusite is directly used as a raw material to prepare the desulfurization and demercuration agent, so that the cost of the desulfurization and demercuration agent can be effectively reduced, the cost of flue gas desulfurization and demercuration is reduced, and the desulfurization and demercuration efficiency is improved.
The microwave radiation treatment is adopted for the pyrolusite, so that the main component manganese dioxide in the pyrolusite can be activated, the oxidation and adsorption effects of the pyrolusite on sulfur dioxide and elemental mercury are improved, and the desulfurization and demercuration performance is improved.
The limitation on the microwave radiation treatment time and the microwave radiation power can not only reduce the treatment energy consumption, but also avoid the defect of poor activity of manganese dioxide caused by over-treatment of manganese dioxide, so that the activity of pyrolusite for flue gas desulfurization and demercuration is ensured.
The specific surface area of the carrier selection is 150-290m2A pore volume of 0.9 to 1.7 cm/g3(ii)/g; improve Li2MnTiO4The uniformity of the combination of the manganese titanate and the carrier is improved, and the Li is improved2MnTiO4The contact area of manganese titanate, sulfide and mercury is increased, the adsorption capacity of sulfide and mercury is increased, and the removal efficiency is improved; in particular a specific surface area of 220m2G, pore volume of 1.3cm3The removal rate of the sulfur and mercury in the flue gas can reach more than 98.5 percent when the sulfur and mercury in the flue gas are absorbed and removed, and the content of sulfur and mercury in the discharged flue gas is effectively reduced.
Detailed Description
The technical solution of the present invention is further defined below with reference to the specific embodiments, but the scope of the claims is not limited to the description.
In some embodiments, the flue gas desulfurization and mercury removal agent consists of active components and a carrier, wherein the mass percent of the active components is 1-30%; the active component is Li2MnTiO4Manganese titanate and pyrolusite in any mass ratio different from zero.
In some embodiments, the active component comprises the raw material components in percentage by mass of Li2MnTiO41-6% of manganese titanate, 15-37% of manganese titanate and the balance of pyrolusite.
In some embodiments, the active component comprises the raw material components in percentage by mass of Li2MnTiO43 percent of manganese titanate, 25 percent of manganese titanate and the balance of pyrolusite.
In certain embodiments, the pyrolusite is treated with microwave radiation.
In some embodiments, the microwave radiation has a microwave power of 100-.
In some embodiments, the pyrolusite powder is obtained by heating pyrolusite to 600 ℃ below zero and spraying water on the surface of pyrolusite to pulverize the pyrolusite powder.
In certain embodiments, the support is molecular sieve, silica, or γ -Al2O3。
In some embodiments, the carrier has a specific surface area of 150-290m2A pore volume of 0.9 to 1.7 cm/g3/g。
In some embodiments, the carrier has a specific surface area of 220m2G, pore volume of 1.3cm3/g。
In certain embodiments, a method for preparing a flue gas desulfurization and mercury removal agent comprises the following steps:
(1) putting pyrolusite at the temperature of 300-600 ℃, heating, and spraying water on the surface of the pyrolusite to pulverize the pyrolusite to obtain pyrolusite powder;
(2) mixing pyrolusite powder with Li2MnTiO4Mixing the manganese titanate and the water uniformly to prepare slurry with the liquid-solid ratio of 3-5: 1;
(3) soaking the carrier in the slurry for 2-3h, treating at 70-130 deg.C for 20-30min, and drying.
Example 1
Grinding pyrolusite into powder, mixing with Li2MnTiO4And manganese titanate are uniformly mixed to obtain active ingredients, and the mixing mass percentage is 80 percent of pyrolusite powder and Li2MnTiO45 percent of manganese titanate and 15 percent of manganese titanate, taking 10g of active component, adding water to prepare slurry, and adding gamma-Al with the diameter of 0.02mm2O3Soaking 80g of the above extract in water for 2h, treating at 70 deg.C for 30min, and drying.
Example 2
Heating pyrolusite to 600 ℃, adding water to pulverize the pyrolusite to obtain pyrolusite powder; mixing pyrolusite powder with Li2MnTiO4And manganese titanate are uniformly mixed to obtain active ingredients, and the mixing mass percentage is 60 percent of pyrolusite powder and Li2MnTiO420 percent of manganese titanate and 20 percent of manganese titanate, 5g of active component is taken, water is added to prepare slurry, and the diameter isSoaking 0.06mm silicon dioxide particles 95g for 3 hr, treating at 130 deg.C for 20min, and drying.
Example 3
Heating pyrolusite to 300 ℃, adding water to pulverize the pyrolusite to obtain pyrolusite powder; mixing pyrolusite powder with Li2MnTiO4And manganese titanate are uniformly mixed to obtain active ingredients, and the mixing mass percentage is 80 percent of pyrolusite powder and Li2MnTiO413 percent of manganese titanate and 7 percent of manganese titanate, taking 1g of active component, adding water to prepare slurry, and setting the specific surface area to be 150m2Per g, pore volume of 0.9cm3Adding 99g of SBA-15 molecular sieve per g, soaking for 2.5h, treating at 80 ℃ for 25min, and drying to obtain the product.
Example 4
Heating pyrolusite to 500 ℃, adding water to pulverize the pyrolusite to obtain pyrolusite powder; mixing pyrolusite powder with Li2MnTiO4And manganese titanate are uniformly mixed to obtain active ingredients, and the mixing mass percentage is that pyrolusite powder accounts for 20 percent, and Li2MnTiO457 percent of manganese titanate, 23 percent of manganese titanate, 15g of active component and water are added to prepare slurry, and the specific surface area is 290m2G, pore volume of 1.7cm385 g/g MCM-41 molecular sieve is added and soaked for 2.5h, the mixture is treated for 25min at the temperature of 80 ℃, and the mixture is dried to obtain the catalyst.
Example 5
Treating pyrolusite by microwave radiation for 10min, wherein the microwave radiation power is 300W, and crushing the pyrolusite into powder to obtain pyrolusite powder; mixing pyrolusite powder with Li2MnTiO4And manganese titanate are uniformly mixed to obtain active ingredients, and the mixing mass percentage is 50 percent of pyrolusite powder and Li2MnTiO426 percent of manganese titanate and 24 percent of manganese titanate, 30g of active component is taken, water is added to prepare slurry, and the specific surface area is 220m2G, pore volume of 1.3cm3Soaking 70 g/g of ZSM-5 molecular sieve for 2.3h, treating at 110 ℃ for 30min, and drying to obtain the finished product.
Example 6
Heating pyrolusite to 400 deg.C, adding water, pulverizing, and treating the pulverized pyrolusite powder with microwave radiation for 30min, the microwave radiation power is 100W, and pyrolusite powder is obtained; mixing pyrolusite powder with Li2MnTiO4And manganese titanate are uniformly mixed to obtain active ingredients, wherein the active ingredients comprise 70 percent of pyrolusite powder and Li in percentage by mass2MnTiO416 percent of manganese titanate and 14 percent of manganese titanate, 25g of active ingredients are taken, water is added to prepare slurry, 75g of silicon dioxide particles with the diameter of 0.01mm are added to be soaked for 2.7 hours, the mixture is treated for 24min at the temperature of 100 ℃, and the mixture is dried to obtain the silicon dioxide/manganese titanate composite material.
The activity evaluation of the flue gas desulfurization and mercury removal agent created by the invention is as follows:
the desulfurization and demercuration agents obtained in the above examples 1 to 6 were filled in a 5mL purification bed with an inner diameter of 12mm at normal temperature and pressure and a space velocity of 2000h-1The effect of desulfurization and demercuration is evaluated by passing nitrogen containing sulfur dioxide and mercury compound impurities with different concentrations through the purification bed, and the results are as follows:
therefore, the desulfurization and demercuration agent provided by the invention can remove a large amount of sulfur dioxide and mercury in flue gas, so that the desulfurization and demercuration rate reaches more than 98%; has high desulfurization and demercuration activity, and reduces the content of sulfur and mercury in the flue gas.
In addition, the raw materials adopted by the invention are easy to obtain, can be generally obtained in the prior art, and have lower treatment cost; can be widely applied to the treatment of various sulfur-containing and mercury-containing waste gases, reduces the content of sulfur and mercury components in the waste and reduces the environmental pollution rate.
The desulfurization and demercuration agent provided by the invention is soaked in warm water at the temperature of 20-30 ℃ after desulfurization and demercuration treatment is carried out on flue gas, so that the recovery and utilization of part of components in the desulfurization and demercuration agent can be realized, but the activity loss is serious.
Claims (8)
1. A flue gas desulfurization and mercury removal agent comprises active components and a carrier, and is characterized in that the mass percent of the active components is 1-30%; the active component is Li2MnTiO4A mixture of manganese titanate and pyrolusite; the active component comprises the raw material components with the mass percentage of Li2MnTiO41-6% of manganese titanate, 15-37% of manganese titanate and the balance of pyrolusite; the carrier has a specific surface area of 150-290m2A pore volume of 0.9 to 1.7 cm/g3/g。
2. The flue gas desulfurization and mercury removal agent of claim 1, wherein the active component comprises the raw material components in percentage by mass of Li2MnTiO43 percent of manganese titanate, 25 percent of manganese titanate and the balance of pyrolusite.
3. The flue gas desulfurization and mercury removal agent of claim 1, wherein the pyrolusite is treated by microwave radiation.
4. The flue gas desulfurization and mercury removal agent as claimed in claim 3, wherein the microwave radiation has a microwave power of 100-300W and a radiation time of 10-30 min.
5. The flue gas desulfurization and mercury removal agent as claimed in claim 1, wherein the pyrolusite is heated to 600 ℃ and then sprinkled with water on the surface of the pyrolusite to be pulverized, so as to obtain pyrolusite powder.
6. The flue gas desulfurization and mercury removal agent of claim 1, wherein the carrier is molecular sieve, silica or gamma-Al2O3。
7. The flue gas desulfurization and mercury removal agent of claim 1, wherein the carrier has a specific surface area of 220m2G, pore volume of 1.3cm3/g。
8. The method for preparing the flue gas desulfurization and mercury removal agent according to any one of claims 1 to 7, comprising the steps of:
(1) putting pyrolusite at the temperature of 300-600 ℃, heating, and spraying water on the surface of the pyrolusite to pulverize the pyrolusite to obtain pyrolusite powder;
(2) mixing pyrolusite powder with Li2MnTiO4Mixing the manganese titanate and the water uniformly to prepare slurry with the liquid-solid ratio of 3-5: 1;
(3) soaking the carrier in the slurry for 2-3h, treating at 70-130 deg.C for 20-30min, and molding.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102107113A (en) * | 2005-03-29 | 2011-06-29 | 洋马株式会社 | Exhaust gas purifying apparatus |
| CN105688647A (en) * | 2016-03-16 | 2016-06-22 | 贵州大学 | Method for dry desulfurization and demercuration of sintering flue gas containing mercury by means of low-grade pyrolusite |
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| CN1279121A (en) * | 1999-06-28 | 2001-01-10 | 陈银山 | Efficient clarifier for dust fume |
| CN100389172C (en) * | 2004-09-28 | 2008-05-21 | 中国石油化工股份有限公司 | Composition with desulfation function |
| CN101275096B (en) * | 2008-05-21 | 2011-11-02 | 宋云星 | Solid desulfuration incendiary agent for coal-burning boiler |
| CN104028218B (en) * | 2014-06-06 | 2016-05-25 | 四川大学 | A kind of low cost highly active catalytic type desulphurizing activated coke and preparation method thereof |
| CN105289645A (en) * | 2015-11-14 | 2016-02-03 | 华玉叶 | Catalyst composition used for fire coal flue gas purifying |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102107113A (en) * | 2005-03-29 | 2011-06-29 | 洋马株式会社 | Exhaust gas purifying apparatus |
| CN105688647A (en) * | 2016-03-16 | 2016-06-22 | 贵州大学 | Method for dry desulfurization and demercuration of sintering flue gas containing mercury by means of low-grade pyrolusite |
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