CN109621627B - Method for eliminating and recycling nitrogen oxides in combustion tail gas - Google Patents

Method for eliminating and recycling nitrogen oxides in combustion tail gas Download PDF

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CN109621627B
CN109621627B CN201811612546.7A CN201811612546A CN109621627B CN 109621627 B CN109621627 B CN 109621627B CN 201811612546 A CN201811612546 A CN 201811612546A CN 109621627 B CN109621627 B CN 109621627B
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CN109621627A (en
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沈美庆
王军
沈谷蓉
王建强
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Tianjin 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
    • 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
    • B01D53/86—Catalytic processes
    • B01D53/8621—Removing nitrogen compounds
    • B01D53/8625—Nitrogen oxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/40—Further details for adsorption processes and devices
    • B01D2259/40083—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption
    • B01D2259/40088—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption by heating
    • B01D2259/4009—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption by heating using hot gas

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  • Environmental & Geological Engineering (AREA)
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  • Exhaust Gas Treatment By Means Of Catalyst (AREA)

Abstract

The invention relates to a method for eliminating and recycling nitrogen oxides in combustion tail gas, which comprises the following steps: A. contacting the combustion exhaust gas comprising nitrogen oxides with an adsorbent at a temperature of less than 150 ℃ to adsorb the nitrogen oxides therein; the adsorbent comprises an active component loaded on a molecular sieve carrier, wherein the active component comprises a noble metal, a rare earth metal or a transition metal, and accounts for 0.1-20 wt% of the total mass of the adsorbent in terms of the content of a single substance; B. high-temperature air with the temperature higher than 250 ℃ is introduced into the adsorbent to desorb the adsorbed nitrogen oxides and the nitrogen oxides are sent into a combustion chamber along with the high-temperature air to be used as combustion air. The invention is suitable for various coal-fired, gas-fired and oil-fired boilers and automobile engines, not only eliminates NOx pollution, but also uses NOx as a combustion-supporting oxidant, and realizes resource utilization of pollutants.

Description

Method for eliminating and recycling nitrogen oxides in combustion tail gas
Technical Field
The invention relates to the technical field of nitrogen oxide pollution treatment and resource recycling in combustion waste gas, in particular to a recycling method for recycling nitrogen oxide in combustion waste gas generated in the combustion process of coal, petroleum, natural gas and the like.
Background
There are a large number of combustion devices and power plants using coal, oil, and natural gas as fuels in industry, such as coal-fired/oil/natural gas power plants, building materials (cement, glass, ceramics, etc.), boilers and blast furnaces in industries such as steel, and motor vehicle engines. Combustion emits a large amount of nitrogen oxides (NOx), causing great harm to the ecological environment and human health. How to eliminate these NOx pollutants is the direction of efforts in industrial denitration technology.
At present, ammonia selective catalytic reduction (NH) technology is generally adopted to control the pollution of nitrogen oxides3-SCR)。NH3The SCR technology has the most mature mainstream denitration technology with high denitration efficiency. NH (NH)3The SCR technique is carried out by reacting NH with a catalytic material3Urea as reducing material reacts with nitrogen oxides to form nitrogen and water. Thus, NH3The SCR technology core components include catalytic materials, urea injection systems (urea tanks, nozzles, urea dosing units, control systems, etc.), nitrogen oxide sensors, etc.; the whole system is complex, the cost of equipment and raw materials is high, andthe catalytic material needs higher temperatures (greater than 200 ℃) to function. The requirement of zero emission of nitrogen oxides in industries such as motor vehicles, coal-fired/petroleum/natural gas power plants, building materials (cement, glass, ceramics and the like), steel and the like is difficult to meet.
NOx, while a pollutant, is also a valuable oxidizer resource from another perspective, such as liquid oxidizer that can be used as a rocket. NH (NH)3NH consumed in large quantities in SCR technology3And is also a valuable industrial raw material. NOx and NH3The two substances with precious value react to generate nitrogen without industrial value and are discharged, so that the method is practical and has a pitfalls.
Therefore, it is of great significance to find a method for recycling nitrogen oxides in combustion exhaust gas with simple process, low cost and high activity at low temperature (not more than 150 ℃).
Disclosure of Invention
The present invention has been made to solve the above problems.
The invention provides a method for eliminating and recycling nitrogen oxides in combustion tail gas, which comprises the following steps:
A. contacting the combustion exhaust gas comprising nitrogen oxides with an adsorbent at a temperature of less than 150 ℃ to adsorb the nitrogen oxides therein; the adsorbent comprises an active component loaded on a molecular sieve carrier, wherein the active component is selected from noble metals, rare earth metals or transition metals, and accounts for 0.1-20 wt% of the total mass of the adsorbent in terms of the content of a single substance; then, the user can use the device to perform the operation,
B. high-temperature air with the temperature higher than 250 ℃ is introduced into the adsorbent to desorb the adsorbed nitrogen oxides and the nitrogen oxides are sent into a combustion chamber along with the high-temperature air to be used as combustion air.
The combustion tail gas comprises various coal-fired/petroleum/natural gas boilers and engine combustion waste gas, such as waste gas containing nitrogen oxides after dust removal and desulfurization in the industries of motor vehicles, coal-fired power plants, gas turbines, cement, glass, ceramics, steel and the like.
Preferably, the active component is selected from silver, platinum, rhodium, palladium, yttrium, lanthanum, cerium, praseodymium, neodymium, manganese, iron, cobalt, nickel or copper; the molecular sieve carrier is selected from BEA, MFI or CHA type molecular sieves.
Preferably, the molecular sieve has a pore size range of 0.1nm-1nm and a specific surface area of 500-1000m2/g。
The preparation method of the adsorbent can be prepared by a hydrothermal crystallization method of an active metal source (usually soluble salts thereof) and a molecular sieve mother liquor together, or can be prepared by a method of impregnating a molecular sieve with the active metal source, and specific preparation methods can be found in another patent of a method which is simultaneously applied by the applicant and is entitled to adsorb nitric oxides and/or hydrocarbon compounds in the cold start process of a motor vehicle, and are not described again.
The adsorbent may also have some catalytic effect, e.g. it may convert a part of NO to NO2Thus, the adsorbent may also be referred to as a catalyst.
Preferably, the nitrogen oxides are brought to adsorption saturation or near saturation in step a. Wherein the near saturation means that the adsorption capacity reaches more than 70% of the saturated adsorption capacity.
Preferably, the adsorption process of step a is less than 30 seconds.
Preferably, the adsorption temperature in step a is from 50 to less than 150 ℃.
Preferably, a step of dedusting the combustion tail gas is further included before the step A.
Preferably, a step of desulfurizing the combustion exhaust gas is further included before the step A.
Preferably, step a is preceded by the step of cooling the combustion exhaust gas by a waste heat recovery device.
More preferably, the cooling medium in the waste heat recovery device is air, and the air is used as the high-temperature air in the step B after being heated by the waste heat of the combustion tail gas. In this case, the heat-exchanged combustion tail gas is further radiated to a temperature lower than 150 ℃ in a pipeline along the way, and then enters the adsorption device to contact with the adsorbent.
Preferably, at least two sets of nitrogen oxide adsorption devices are arranged, wherein the first set executes the step A while the second set executes the step B, and the first set executes the step B while the second set executes the step A, so that the nitrogen oxides in the combustion tail gas can be continuously eliminated and recycled.
The invention has the beneficial effects that:
1. the adsorbent can quickly adsorb NOx at the temperature of less than 150 ℃, the saturated adsorption capacity of the adsorbent can reach 30mol/g, the NOx in combustion tail gas can be basically and completely removed, and zero NOx pollution emission is realized.
2. The invention completely avoids the reaction with NH3Disadvantages associated with SCR technology, in particular the elimination of the use of expensive NH3Reduce NOx, raw materials and equipment cost greatly reduced, for example the burning boiler owner needn't set up and spout the ammonia plant for the denitration again, greatly reduced equipment investment cost and maintenance cost, and avoided ammonia to reveal and the environmental protection pressure that ammonia escape brought.
3. The waste heat recovery device is used for preheating the ambient air, and the preheated high-temperature air is supplied to the boiler combustion chamber as combustion-supporting air after NOx is desorbed, so that the waste heat is recycled, the characteristic of NOx as a strong oxidant is fully utilized, the resource recycling of NOx is realized, the NOx pollution is eliminated, and the three aims are achieved.
Drawings
FIG. 1 is a schematic process flow diagram of the process of the present invention.
FIG. 2 is a graph showing the adsorption of NOx in the combustion exhaust gas of the glass industry at 100 ℃ by the adsorbent of the present invention. Wherein the abscissa is the contact time and the ordinate is the concentration of NOx in the exhaust gas in ppm by volume, the same applies hereinafter.
FIG. 3 is a NOx desorption curve diagram of the adsorbent of the invention after adsorbing tail gas in the glass industry and introducing high-temperature air after the tail gas is saturated.
FIG. 4 is a graph showing the adsorption of NOx in cement industry combustion exhaust gas at 150 ℃ by the adsorbent of the present invention.
FIG. 5 is a NOx desorption curve diagram of the adsorbent of the invention after adsorbing saturated tail gas in the cement industry and introducing high-temperature air.
FIG. 6 is a graph showing the adsorption of NOx in the combustion exhaust gas of a gas boiler at 80 ℃ by the adsorbent of the present invention.
FIG. 7 is a graph showing the NOx desorption curve of the adsorbent according to the present invention after adsorbing the exhaust gas of the gas boiler saturated and introducing high temperature air.
FIG. 8 is a graph showing the adsorption of NOx in the combustion exhaust gas of an oil-fueled engine at 80 ℃ by the adsorbent of the present invention.
Fig. 9 is a NOx desorption curve chart of the adsorbent according to the present invention after adsorbing the exhaust gas of the fuel engine and introducing high-temperature air.
FIG. 10 is a graph of the adsorption of NOx from the combustion exhaust of the glass industry at 50 ℃ by the Pd/Beta adsorbent of the present invention.
FIG. 11 is a graph showing the desorption of NOx by the Pd/Beta adsorbent of the present invention after adsorbing saturation of tail gas in the glass industry and introducing high temperature air.
Detailed Description
The following examples are given to illustrate the invention and are not intended to be limiting.
Example 1
Take the combustion tail gas discharged from a coal-fired boiler for smelting silica in a certain glass plant as an example.
After the combustion tail gas is subjected to dust removal and desulfurization treatment, the combustion tail gas contains 1500ppm of NOx and 16.5 percent of CO2、8％O2、11.5％H2O, the balance being N2. Taking the combustion tail gas sample for experiment, the dosage of the molecular sieve adsorbing material is 0.589g, the total gas flow is 900mL/min, the adsorption temperature is 100 ℃, and the space velocity is 11,000h-1. The adsorbent used was Ce/Beta indicating that Ce was supported on a Beta molecular sieve, and the composition of the remaining adsorbents is shown in the following description in a similar manner), wherein the percentage content of Ce was 2 wt%, and the NOx adsorption results are shown in FIG. 2, wherein adsorption saturation was achieved after about 41 seconds, and the saturated adsorption amount of NOx reached 32.8. mu. mol/g adsorbent.
After the adsorption saturation, the introduction of the combustion exhaust gas is stopped, the introduction of air into the adsorbent is changed, and a temperature-programmed desorption experiment is carried out, and as a result, as shown in fig. 3, it can be seen that when the air temperature is increased to 230 ℃, the NOx begins to be desorbed from the adsorbent, and the instantaneous concentration of the desorbed NOx reaches the maximum at about 285 ℃.
The detailed adsorption and desorption results are listed in table 1 below.
Industrially, after desorption, high-temperature air is introduced into the combustion chamber of the coal-fired boiler as combustion air, so that the desorbed NOx serves as a combustion improver.
Example 2
Take the combustion tail gas discharged from a coal-fired boiler of a cement plant as an example.
After the combustion tail gas is subjected to dust removal and desulfurization treatment, the combustion tail gas contains 1000ppm of NOx and 12.5 percent of CO2、9.2％O2、6％H2O, the balance being N2. Taking the combustion tail gas sample for experiment, the dosage of the molecular sieve adsorbing material is 0.288g, the total gas flow is 1000mL/min, the adsorption temperature is 150 ℃, and the airspeed is 25,000h-1. The adsorbent used was La/Beta, in which the percentage content of La was 5 wt%, and the NOx adsorption results are shown in FIG. 4, in which adsorption saturation was achieved after about 34 seconds, and the saturated adsorption amount of NOx reached 33.4. mu. mol/g adsorbent.
After the adsorption saturation, the introduction of the combustion exhaust gas is stopped, the introduction of air into the adsorbent is changed, and a temperature-programmed desorption experiment is carried out, and as a result, as shown in fig. 5, it can be seen that when the air temperature is increased to 220 ℃, the NOx begins to be desorbed from the adsorbent, and the instantaneous concentration of the desorbed NOx reaches the maximum at about 280 ℃.
The detailed adsorption and desorption results are listed in table 1 below.
Industrially, after desorption, high-temperature air is introduced into the combustion chamber of the coal-fired boiler as combustion air, so that the desorbed NOx serves as a combustion improver.
Example 3
Take the combustion tail gas discharged from the gas boiler of a power plant as an example.
After the combustion tail gas is subjected to dust removal and desulfurization treatment, the combustion tail gas contains 500ppm of NOx and 5 percent of CO2、8％O2、5％H2O, the balance being N2. Taking the combustion tail gas sample for experiment, the dosage of the molecular sieve adsorbing material is 0.144g, the total gas flow is 1000mL/min, the adsorption temperature is 80 ℃, and the airspeed is 50,000h-1. The adsorbent used was Cu/ZSM-5 with a Cu content of 10 wt%, and the NOx adsorption results are shown in FIG. 6, which is a graph ofThe adsorption saturation was reached in about 47 seconds, and the saturated adsorption amount of NOx reached 33.6. mu. mol/g adsorbent.
After the adsorption saturation, the introduction of the combustion exhaust gas is stopped, the introduction of air into the adsorbent is changed, and a temperature-programmed desorption experiment is carried out, and as a result, as shown in fig. 7, it can be seen that when the air temperature is increased to 220 ℃, the NOx begins to be desorbed from the adsorbent, and the instantaneous concentration of the desorbed NOx reaches the maximum at about 280 ℃.
The detailed adsorption and desorption results are listed in table 1 below.
Industrially, after desorption, high-temperature air is introduced into the combustion chamber of the gas boiler as combustion air, so that the desorbed NOx is used as a combustion improver.
Example 4
Take the combustion exhaust gas discharged from a certain automobile fuel engine as an example.
After the combustion tail gas is subjected to dust removal and desulfurization treatment, the combustion tail gas contains 200ppm of NOx and 5 percent of CO2、10％O2、5％H2O, the balance being N2. Taking the combustion tail gas sample for experiment, the dosage of the molecular sieve adsorbing material is 0.144g, the total gas flow is 1000mL/min, the adsorption temperature is 80 ℃, and the airspeed is 50,000h-1. The adsorbent used was Co/SSZ-13, in which the percentage content of Co was 20 wt%, and the NOx adsorption results are shown in FIG. 8, in which adsorption saturation was achieved after about 121 seconds, and the saturated adsorption amount of NOx reached 29.8. mu. mol/g adsorbent.
After saturation of adsorption, the combustion exhaust gas was stopped and the adsorbent was redirected to introduce air and a temperature programmed desorption experiment was carried out, and as a result, as shown in fig. 9, it can be seen that when the air temperature increased to 230 ℃, NOx began to desorb from the adsorbent and the instantaneous concentration of desorbed NOx reached a maximum at about 283 ℃.
The detailed adsorption and desorption results are listed in table 1 below.
Industrially, after desorption, high-temperature air is introduced into a combustion chamber of the fuel engine to be used as combustion-supporting air, so that the desorbed NOx is used as a combustion improver.
Example 5
Take the combustion tail gas discharged from a coal-fired boiler for smelting silica in a certain glass plant as an example.
After the combustion tail gas is subjected to dust removal and desulfurization treatment, the combustion tail gas contains 1500ppm of NOx and 16.5 percent of CO2、8％O2、11.5％H2O, the balance being N2. Taking the combustion tail gas sample for experiment, the dosage of the molecular sieve adsorbing material is 0.589g, the total gas flow is 900mL/min, the adsorption temperature is 50 ℃, and the airspeed is 11,000h-1. The adsorbent used is PdCe/Beta, wherein Pd and Ce are loaded on a Beta molecular sieve, the composition of the rest of the adsorbents shows that the method is similar to the method), the percentage content of Pd is 0.1 wt%, the percentage content of Ce is 2 wt%, the NOx adsorption result is shown in figure 10, the adsorption saturation is achieved after about 42 seconds, and the saturated adsorption capacity of NOx reaches 40.4 mu mol/g of the adsorbent.
After the adsorption saturation, the combustion exhaust gas is stopped and the air is introduced into the adsorbent again and the temperature programmed desorption experiment is carried out, and as a result, as shown in fig. 11, it can be seen that when the air temperature is increased to 220 ℃, the NOx begins to be desorbed from the adsorbent, and the instantaneous concentration of the desorbed NOx reaches the maximum at about 285 ℃.
The detailed adsorption and desorption results are listed in table 1 below.
Industrially, after desorption, high-temperature air is introduced into the combustion chamber of the coal-fired boiler as combustion air, so that the desorbed NOx serves as a combustion improver.
TABLE 1
Figure GDA0003011971810000071

Claims (7)

1. A method for eliminating and recycling nitrogen oxides in combustion exhaust gas is characterized by comprising the following steps:
A. contacting the combustion exhaust gas comprising nitrogen oxides with an adsorbent at a temperature of less than 150 ℃ to adsorb the nitrogen oxides therein; the adsorbent comprises an active component loaded on a molecular sieve carrier, wherein the active component is selected from noble metals, rare earth metals or transition metals, and accounts for 0.1-20 wt% of the total mass of the adsorbent in terms of the content of a single substance; then, the user can use the device to perform the operation,
B. introducing high-temperature air with the temperature of more than 250 ℃ into the adsorbent to desorb the adsorbed nitrogen oxides and sending the nitrogen oxides into a combustion chamber along with the high-temperature air to be used as combustion-supporting air;
the adsorption temperature in the step A is 50 to less than 150 ℃, and the adsorption process is less than 30 seconds.
2. The method of claim 1, wherein the active component is selected from silver, platinum, rhodium, palladium, yttrium, lanthanum, cerium, praseodymium, neodymium, manganese, iron, cobalt, nickel, or copper; the molecular sieve carrier is selected from BEA, MFI or CHA type molecular sieves.
3. The method of claim 1, wherein nitrogen oxides are saturated and/or nearly saturated in step a.
4. The method according to claim 1, characterized by further comprising the step of cooling the combustion exhaust gas by passing the combustion exhaust gas through a waste heat recovery device before step a.
5. The method according to claim 4, wherein the cooling medium in the waste heat recovery device is air, and the air is heated by the waste heat of the combustion exhaust gas and is used as the high-temperature air in the step B.
6. The method of claim 1, wherein at least two sets of nitrogen oxide adsorption units are provided, wherein the first set performs step A while the second set performs step B, and the first set performs step B while the second set performs step A, thereby continuously eliminating and recycling nitrogen oxides in the combustion exhaust.
7. The method as claimed in claim 1, wherein the molecular sieve has a pore size in the range of 0.1nm-1nm and a specific surface area of 500-1000m2/g。
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