CN114042378A - Method for removing mercury in hazardous waste incineration flue gas - Google Patents
Method for removing mercury in hazardous waste incineration flue gas Download PDFInfo
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- CN114042378A CN114042378A CN202111381635.7A CN202111381635A CN114042378A CN 114042378 A CN114042378 A CN 114042378A CN 202111381635 A CN202111381635 A CN 202111381635A CN 114042378 A CN114042378 A CN 114042378A
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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
- B01D53/77—Liquid phase processes
- B01D53/79—Injecting reactants
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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
- 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
Abstract
The invention discloses a method for removing mercury in hazardous waste incineration flue gas, which is characterized by comprising the following steps: s1, obtaining the flue gas from which the mercury is to be removed, and measuring the content of the mercury in the flue gas; s2, calculating the dosage of calcium bromide by using a mercury bromide ratio calculation formula according to the measured mercury content; s3, preparing the calcium bromide into a solution, and spraying the solution into the flue gas at the temperature of 600-900 ℃ for reaction. The method can quantitatively calculate the using amount of the calcium bromide, and can effectively remove mercury in the flue gas without causing the concentration of bromide ions in the flue gas to rise.
Description
Technical Field
The invention belongs to the technical field of environmental protection, and particularly relates to a method for removing mercury in hazardous waste incineration flue gas.
Background
Mercury is an indispensable raw material in modern industrial and agricultural production, and the application of mercury is more than 3000. Mercury (Hg), commonly known as mercury, is the only liquid metal at room temperature, silvery white, and free-flowing. Heating of mercury in air oxidizes it to mercury oxide (HgO). The mercury compounds include mercuric chloride, mercurous chloride, mercuric sulfide, mercuric sulfate, and the like, in addition to oxidized mercury.
Mercury vapor is a highly toxic substance, and mercury can be largely evaporated even at normal temperature or below 0 ℃, and toxic reaction can occur after entering human bodies through respiratory tracts or gastrointestinal tracts. Such as attack on the digestive organs and kidneys of the human body, resulting in irritability, headaches, memory loss, or the like, or causing malnutrition, anemia, weight loss, and the like.
The removal of mercury in the industry currently relies primarily on the synergistic benefits of the flue gas Control systems (APCDs Air Pollution Control Devices). Particulate matter control device such as bag dust collector and electrostatic precipitator to HgpHas the advantage of betterDue to Hg2+Has good water solubility and can be easily removed by a wet desulphurization system, however, Hg0Is stable in chemical properties, low in boiling point, volatile and difficult to dissolve in water, and cannot be completely removed by the conventional APCDs.
Some studies have found that doping of a transition metal oxide in a catalyst of a Selective Catalytic Reduction device (SCR Selective Catalytic Reduction) is a promotion of Hg0An efficient route to oxidation. However, it should be noted that such modification operation may affect the NOx removal effect of the catalyst, and is also easily affected by other components in the flue gas, and in order to cooperatively control nitrogen oxides and mercury, it is necessary to comprehensively consider the catalytic efficiency, the coupling relationship of gas components, the catalyst poisoning prevention, and other factors, and these limitations make the modified catalyst temporarily unable to be widely applied as an effective means for mercury removal.
There have also been some studies discussing the halogen additive versus Hg0The promotion of oxidation, such as the incorporation of halogen additives such as calcium chloride into the coal. R Kleinarendt has studied the calcium bromide mercury removal process in detail. Research shows that the calcium bromide solution is added into hazardous waste incineration plants and coal-fired power plants to effectively reduce the concentration of elemental mercury in flue gas, and the influence of different flue gas components on the mercury oxidation rate is compared. But the research does not further explain the model of calcium bromide demercuration and the relation between the addition amount of calcium bromide and the mercury content in the smoke components.
The addition of excess halogen results in the production of reactive halogen products like hydrogen halides, elemental halogens, etc. during the reaction, which are not only highly toxic but also corrosive and difficult to handle.
Disclosure of Invention
Aiming at the problem that the bromine ion concentration in the flue gas is increased due to excessive addition of calcium bromide in the prior art, the invention adopts the following technical scheme:
a method for removing mercury in hazardous waste incineration flue gas comprises the following steps:
s1, obtaining the flue gas from which the mercury is to be removed, and measuring the content of the mercury in the flue gas;
s2, calculating the dosage of calcium bromide by using a mercury bromide ratio calculation formula according to the measured mercury content;
s3, preparing the calcium bromide into a solution, and spraying the solution into the flue gas at the temperature of 600-900 ℃ for reaction.
Wherein the formula for calculating the amount of bromine used for removing mercury from calcium bromide is R2=mBr/mHgX 100%, wherein R2The value range is 320-380 (m) for bromine-mercury ratioBrAnd mHgRespectively represent the mass of Br added to the reaction system and the total mass of Hg.
Preferably, said R is2Has a value of 350.
Preferably, in S1, the specific method for obtaining the flue gas from which mercury is to be removed is to obtain the flue gas from which mercury is to be removed by sampling at a constant speed from the center of the flue gas flow by using an ontario sampling system; wherein the whole sampling system is kept at a constant temperature of 120 ℃ during the sampling process.
Preferably, in S1, the sampling position is sampling from a bag-type dust collector or a quenching tower.
Preferably, the step S3 is to prepare a saturated solution of calcium bromide, atomize the saturated solution of calcium bromide with an atomizer, control the flow rate, and spray the atomized solution of calcium bromide into flue gas at 800 ℃ at a constant speed to perform the reaction.
Preferably, the step of spraying the atomized calcium bromide solution into a boiler or a secondary combustion chamber for reaction is further included in the step of S3
Preferably, the rough sampling system comprises a constant-temperature quartz sampling tube, a filtering device, an ice bath absorption bottle group, a flowmeter and a flow pump.
The invention has the advantages of
Compared with the prior art, the invention has the following beneficial effects:
compared with the prior art that only halogen salt is added to remove mercury in the flue gas, and the relation between the addition amount of the halogen salt and the mercury content in the flue gas components is not explained, the method can quantitatively calculate the using amount of calcium bromide, and can effectively remove mercury in the flue gas without causing the concentration of bromide ions in the flue gas to rise.
Drawings
FIG. 1 shows the effect of calcium bromide on the appearance of mercury under different reaction conditions in example 1;
FIG. 2 shows the EPR detection signal of the reaction product of Hg and CaBr2 at 600 ℃; wherein the symbol (#) represents the spin adduct DMPO-M that interacts with the Br radical with the solvent, and DMPO-OH and DMPOX are represented by the symbols (#) and (+), respectively.
FIG. 3 shows CaBr2Experimental EPR signals for reactions with different ratios of bromine to mercury between Hg; wherein, A represents that the ratio of the bromine to the mercury is 350, B represents that the ratio of the bromine to the mercury is 700, and C represents that the ratio of the bromine to the mercury is 1200;
FIG. 4 shows an ampere rough sampling system;
FIG. 5 shows CaBr under the condition of hazardous waste combustion2For Hg0The oxidizing effect of (3); wherein A represents a blank group; b denotes CaBr injection under steady conditions2(ii) a C represents continuing to add mercury to the feed inlet; d represents the simultaneous addition of mercury and excess CaBr2(bromine to mercury ratio of 350); e represents the simultaneous addition of mercury and a small amount of CaBr2(the ratio of bromine to mercury is 150).
Detailed Description
Unless otherwise indicated, implied from the context, or customary in the art, all parts and percentages herein are by weight and the testing and characterization methods used are synchronized with the filing date of the present application. Where applicable, the contents of any patent, patent application, or publication referred to in this application are incorporated herein by reference in their entirety and their equivalent family patents are also incorporated by reference, especially as they disclose definitions relating to synthetic techniques, products and process designs, polymers, comonomers, initiators or catalysts, and the like, in the art. To the extent that a definition of a particular term disclosed in the prior art is inconsistent with any definitions provided herein, the definition of the term provided herein controls.
The numerical ranges in this application are approximations, and thus may include values outside of the ranges unless otherwise specified. A numerical range includes all numbers from the lower value to the upper value, in increments of 1 unit, provided that there is a separation of at least 2 units between any lower value and any higher value. For example, if a compositional, physical, or other property (e.g., molecular weight, melt index, etc.) is recited as 100 to 1000, it is intended that all individual values, e.g., 100, 101, 102, etc., and all subranges, e.g., 100 to 166, 155 to 170, 198 to 200, etc., are explicitly recited. For ranges containing a numerical value less than 1 or containing a fraction greater than 1 (e.g., 1.1, 1.5, etc.), then 1 unit is considered appropriate to be 0.0001, 0.001, 0.01, or 0.1. For ranges containing single digit numbers less than 10 (e.g., 1 to 5), 1 unit is typically considered 0.1. These are merely specific examples of what is intended to be expressed and all possible combinations of numerical values between the lowest value and the highest value enumerated are to be considered to be expressly stated in this application.
When used with respect to chemical compounds, the singular includes all isomeric forms and vice versa (e.g., "hexane" includes all isomers of hexane, individually or collectively) unless expressly specified otherwise. In addition, unless explicitly stated otherwise, the use of the terms "a", "an" or "the" are intended to include the plural forms thereof.
The terms "comprising," "including," "having," and derivatives thereof do not exclude the presence of any other component, step or procedure, and are not intended to exclude the presence of other elements, steps or procedures not expressly disclosed herein. To the extent that any doubt is eliminated, all compositions herein containing, including, or having the term "comprise" may contain any additional additive, adjuvant, or compound, unless expressly stated otherwise. Rather, the term "consisting essentially of … …" excludes any other components, steps or processes from the scope of any of the terms hereinafter recited, insofar as such terms are necessary for performance. The term "consisting of … …" does not include any components, steps or processes not specifically described or listed. Unless explicitly stated otherwise, the term "or" refers to the listed individual members or any combination thereof.
In order to make the technical problems, technical solutions and advantageous effects solved by the present invention more apparent, the present invention is further described in detail below with reference to the following embodiments.
Examples
The following examples are used herein to demonstrate preferred embodiments of the invention. It will be appreciated by those of skill in the art that the techniques disclosed in the examples which follow represent techniques discovered by the inventor to function in the invention, and thus can be considered to constitute preferred modes for its practice. Those of skill in the art should, in light of the present disclosure, appreciate that many changes can be made in the specific embodiments which are disclosed and still obtain a like or similar result without departing from the spirit or scope of the invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs and the disclosures and references cited herein and the materials to which they refer are incorporated by reference.
Those skilled in the art will recognize, or be able to ascertain using no more than routine experimentation, many equivalents to the specific embodiments of the invention described herein. Such equivalents are intended to be encompassed by the following claims.
Example 1 reaction under different conditions
(1) Under the condition of pure nitrogen, the change of the mercury concentration in the flue gas is observed in the temperature range of 300-1000 ℃, and the result is shown in figure 1;
(2) the change of the mercury concentration in the flue gas was observed in the temperature range of 300 ℃ to 1000 ℃ under the conditions of 80% nitrogen and 20% oxygen, and the results are shown in fig. 1;
(3) spraying a calcium bromide solution into the flue gas under the conditions of 80% nitrogen and 20% oxygen, and observing the change of the mercury concentration in the flue gas in the temperature range of 300-1000 ℃ respectively, wherein the result is shown in figure 1;
as can be seen from FIG. 1, Hg in flue gas is in the range of 300 ℃ to 1000 ℃ under pure nitrogen condition0The concentration is kept stable, which shows that mercury oxidation has no significant correlation with temperature change; in the second experimental group, 80% nitrogen and 20% oxygen were used as flue gas, Hg0The concentration of (2) does not vary much. When the temperature is lower than 500 ℃, the concentration of the elementary mercury in the flue gas is about 189 ug/m3When the temperature reaches 800 ℃, the concentration of the elementary mercury in the flue gasAbout 214 ug/m3. The reason is that mercury forms a gas-solid mixture of oxidized mercury at lower temperatures. When the temperature exceeds 500 ℃, the mercury oxide starts to decompose.
When CaBr is sprayed in2In solution, Hg0The concentration is obviously reduced, the conversion rate is obviously influenced by the temperature, and the Hg is Hg when the bromine-mercury ratio is 3500The removal rate of (a) was increased from 16.82% at 300 ℃ to 94.14% at 800 ℃ and then stabilized with further increase in temperature, the spike appearing in the figure being a mechanical error caused by fluctuations in the state of the detection instrument.
Example 2 calcium bromide demercuration oxidation mechanism experiment
Separately, A, B, C three microreactors were charged with distilled water (0.6 mL) and DMPO (100 mM), distilled water (0.6 mL), DMPO (100 mM) and Hg (1000 ug/mL), DMPO (100 mM) and CaBr2 (52% (w/w)), and heated in a 600 ℃ sand bath for 30s (MBr)2/MHg = 350) and recording the spectrum. The results are shown in fig. 2, from which it can be concluded that the calcium bromide demercuration oxidation mechanism is as follows:
example 3 radical trapping experiments at different ratio of bromine to mercury
Adding CaBr2(52% (w/w)) and Hg (1000 ug/ml) were placed in the reactor and heated to 600 deg.C for 30 seconds, after which time DMPO (100 mm) was added to the system and the spectra recorded. By reducing the mercury content, a ratio of mBr for bromine and mercury, respectively, was established2/mHg=350、 mBr2/mHg =700 and mBr2Control experiment of/mHg = 1200. The results are shown in FIG. 3, and the experimental results confirm that the addition of calcium bromide does generate some free radicals, which are halogen oxidized Hg0One of the effective substances of (1). The three curves represent a gradual decrease in total mercury. When the mass ratio reaches 350, the signal intensity of the free radicals DMPO-OH and DMPOX does not change with the increase of the mass ratio, which indicates that the two free radicals are excited by Br and reach a saturated state at the mass ratio of 350.
Example 4 determination of Mercury content in hazardous waste incineration flue gas
Tests for removing mercury in flue gas by calcium bromide in certain hazardous waste incineration plant in Shandong
The flue gas to be mercury removed was obtained by sampling at a constant speed from the center of the flue gas flow after the quench tower using an ampere-rough sampling system as shown in fig. 4, wherein the entire sampling system was kept at a constant temperature of 120 ℃.
As shown in FIG. 5, the mercury content in the flue gas after the quenching tower was sampled and tested under the steady operation condition (A). Collecting flue gas by adopting an Ontario-Hygro method, and determining the content of mercury in the flue gas as shown in table 1;
TABLE 1 elemental analysis in hazardous waste incineration flue gas
a ad refers to a dry base in industrial analysis of hazardous waste
Example 5 removal of Mercury from hazardous waste incineration waste flue gas
As shown in FIG. 5, CaBr under the condition of dangerous waste combustion2For Hg0Shows Hg under different working conditions0About 70-85% of mercury in hazardous waste as Hg0Is released. The mercury content was about 0.015 mg/m3From this, the mass of calcium bromide injected per cubic meter was calculated to be 13.1 mg. When the combustion chamber injects CaBr under the stable working condition2In the case of (B), Hg0The removal rate reaches 90 percent. We added mercury to the feed to simulate a high mercury content waste incineration environment, with a mercury concentration in the flue gas of about 0.213 mg/m3 under high mercury content flue gas (C) conditions. Excessive calcium bromide (mass ratio of 350) is added on the basis of simulating the incineration working condition of the high-mercury-content garbage, and the mercury removal rate reaches over 95 percent and is almost completely removed.
Comparative example 1 removal of mercury from hazardous waste incineration waste flue gas
As shown in FIG. 5, CaBr under the condition of dangerous waste combustion2For Hg0Shows Hg under different working conditions0Is released fromAmount of about 70-85% of mercury in hazardous waste as Hg0Is released. The mercury content was about 0.015 mg/m3When the ratio of bromine to mercury is 150 and the amount of calcium bromide is reduced, the removal rate of mercury is about 65%.
As can be seen in fig. 5, the line graphs show the bromide ion concentrations in five samples of flue gas, with lower bromide ion concentrations as the mercury concentration in the flue gas increases, indicating that mercury will react with hydrogen bromide and consume bromide ions.
All documents referred to herein are incorporated by reference into this application as if each were individually incorporated by reference. Furthermore, it should be understood that various changes and modifications of the present invention can be made by those skilled in the art after reading the above teachings of the present invention, and these equivalents also fall within the scope of the present invention as defined by the appended claims.
Claims (6)
1. A method for removing mercury in hazardous waste incineration flue gas is characterized by comprising the following steps:
s1, obtaining the flue gas from which the mercury is to be removed, and measuring the content of the mercury in the flue gas;
s2, calculating the dosage of calcium bromide by using a mercury bromide ratio calculation formula according to the measured mercury content;
s3, preparing calcium bromide into a solution, and spraying the solution into flue gas at the temperature of 600-900 ℃ for reaction;
wherein, the calculation formula of the ratio of bromine and mercury is as follows R2=mBr/mHg×100%，R2The ratio of bromine to mercury is 320-380 mBrAnd mHgRespectively representing the mass of Br and the total mass of Hg in the reaction system.
2. The method for removing mercury in hazardous waste incineration flue gas according to claim 1, wherein the ratio of bromine to mercury R is2Has a value of 350.
3. The method for removing mercury from hazardous waste incineration flue gas according to claim 1, wherein in the step S1, the method for obtaining the flue gas from which mercury is to be removed specifically comprises: sampling at constant speed from the center of the flue gas flow by using an Ontario sampling system to obtain the flue gas from which mercury is to be removed; wherein the whole sampling system is kept at a constant temperature of 120 ℃ during the sampling process.
4. The method for removing mercury from hazardous waste incineration flue gas according to claim 1, wherein S3 is specifically that calcium bromide is prepared into a saturated solution, the saturated solution of calcium bromide is atomized by an atomizer, and then the saturated solution of calcium bromide is sprayed into flue gas at 800 ℃ at a constant speed to react under a controlled flow rate.
5. The method for removing mercury in hazardous waste incineration flue gas according to claim 1, wherein the step of atomizing the calcium bromide solution and spraying the atomized calcium bromide solution into a boiler or a secondary combustion chamber for reaction is further included in the step of S3.
6. The method for removing mercury in hazardous waste incineration flue gas according to claim 1, wherein in the S1, a sampling position is a bag-type dust remover or a quenching tower.
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