CN111644048A - Process method for removing nitrogen oxide and alkyl nitrite gas in tail gas - Google Patents
Process method for removing nitrogen oxide and alkyl nitrite gas in tail gas Download PDFInfo
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- B01D53/14—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 absorption
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Abstract
The invention relates to a process method for removing nitrogen oxide and alkyl nitrite gas in tail gas, which comprises the following steps: (1) mixing the process tail gas with the reducing gas, carrying out reduction reaction through a first-stage reactor and a second-stage reactor, and catalytically reducing nitrogen oxides and alkyl nitrite in the process tail gas into nitrogen, wherein the temperature of the first-stage reactor is 150-270 ℃, and the temperature of the second-stage reactor is 180-600 ℃; (2) feeding the reduced gas material into a washing tower for liquid absorption to remove NH3(ii) a (3) And (3) burning the gas material obtained in the step (2). Compared with the prior art, the method has the advantages of low consumption, good treatment effect, simple process flow and the like.
Description
Technical Field
The invention belongs to the field of tail gas treatment, and particularly relates to a process method for removing nitrogen oxides and alkyl nitrite gas in tail gas.
Background
In recent years, the industrialization of ethylene glycol prepared from coal has been advanced. Meanwhile, the national discharge standard for the three wastes is also increasingly strict. Therefore, the tail gas generated from the coal-to-ethylene glycol process route is also receiving more and more attention.
Process tail gas generated in the step of synthesizing oxalate in the process of preparing glycol from coal and containing nitrogen oxides (NO and NO)2、N2O, etc.), Methyl Nitrite (MN), etc. Wherein NO is a colorless, odorless, and water-insoluble toxic gas. When reacting with oxygen, red brown gas NO with pungent odor can be generated2。NO2After being inhaled into the lung tissue of a human body, the medicine has great corrosivity and seriously harms the health of the human body. N is a radical of2O itself is a greenhouse gas, causing a greenhouse effect about 310 times that of carbon dioxide. At the same time, N2O is commonly called laughing gas, and is often inhaled by contact, which can cause neurotoxicity and damage the brain. Therefore, the process off-gas must be cleaned to a level below the emission standards permitted by national legislation.
The invention mainly aims at nitrogen oxides (NO, NO) generated in the process of synthesizing oxalate2、N2O) and alkyl nitrite, provides an efficient and energy-saving treatment mode by catalytic reduction of a two-stage reactor, so that the content of nitrogen oxides and alkyl nitrite is less than 10mg/m3And the national emission standard is reached.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a process method for removing nitrogen oxides and alkyl nitrite gas in tail gas, which has the advantages of low energy consumption, good treatment effect and simple process flow.
The purpose of the invention can be realized by the following technical scheme:
a process method for removing nitrogen oxides and alkyl nitrite gases in tail gas comprises the following steps:
(1) mixing the process tail gas with the reducing gas, carrying out reduction reaction through a first-stage reactor and a second-stage reactor, and catalytically reducing nitrogen oxides and alkyl nitrite in the process tail gas into nitrogen, wherein the temperature of the first-stage reactor is 150-270 ℃, and the temperature of the second-stage reactor is 180-600 ℃;
(2) feeding the reduced gas material into a washing tower for liquid absorption to remove NH3;
(3) And (3) burning the gas material obtained in the step (2).
The invention mainly aims at nitrogen oxides (NO, NO) generated in the process of synthesizing oxalate2、N2O) and alkyl nitrite, provides an efficient and energy-saving treatment mode by catalytic reduction of a two-stage reactor, so that the content of nitrogen oxides and alkyl nitrite is less than 10mg/m3And the national emission standard is reached.
NO and NO in nitrogen oxide according to the composition of process tail gas2、N2O4Lower reduction temperatures corresponding to alkyl nitrite and the like, and N2The reduction temperature of O is higher and the two have larger difference, so the invention adopts the form of a two-stage reactor, firstly, the component which is easy to reduce is reduced at the relatively lower reduction temperature in the first-stage reactor, then, the temperature is increased to reduce N in the second-stage reactor2Reducing O to realize the total content of nitrogen oxide and alkyl nitrite at the outlet of the reactor to be less than 10mg/m3The denitrification effect is improved, and the high-temperature inactivation of the catalyst in the first-stage reactor is also avoided.
The first-stage reactor is a constant-temperature reactor, and the second-stage reactor is an adiabatic reactor.
Further, the reactor at the lower reduction temperature is designed as a constant temperature reactor, because the reduction process of the nitrogen oxide and the alkyl nitrite is an exothermic process, and the reactor needs to be designed as a constant temperature in order to maintain the optimal reaction temperature and achieve the optimal reaction effect; the reaction temperature in the two-stage reactor is higher, if a heat-taking medium is adopted, the reaction temperature is higherThe temperature in the reactor is maintained at a high position, which increases the design difficulty of the reactor and increases the equipment investment, therefore, the adiabatic reactor is adopted, and N is utilized2The reaction heat of the O and reducing gas reaction process raises the temperature of the material, greatly simplifies the design of the reactor, has simple structure and low cost, reduces energy loss and has the effect of energy conservation.
The reaction pressure of the first-stage reactor and the second-stage reactor is 0.1-1 MPa in absolute pressure, and the gas airspeed is 50-10000 h-1。
The active component of the catalyst in the first-stage reactor comprises one or more of V, Mn, Fe, Co, Ni, Cu, Ag, Pt, Pd, Rh, Ru or Au; the active component of the catalyst in the two-stage reactor comprises one or more of V, Mn, Fe, Co, Ni, Cu, Ag, Pt, Pd, Rh, Ru or Au.
The washing liquid in the washing tower is water-containing liquid.
And the step (3) is to carry out combustion treatment on the gas material obtained in the step (2) to recover heat or send the gas material into a torch.
The process tail gas is esterification recycle gas or purge gas of esterification recycle gas after the esterification recycle gas passes through an alkyl nitrite regeneration absorption tower.
The nitrogen oxide component comprises NO and NO2、N2O4Or N2O, wherein the volume concentration of the nitrogen oxides in the process tail gas is less than 30%; the alkyl nitrite comprises one or more of methyl nitrite, ethyl nitrite and isopropyl nitrite, and the volume concentration of the alkyl nitrite in the process tail gas is less than 10%.
The reducing gas is selected from CO and H2、NH3Or one or more of hydrocarbons.
The volume ratio of the nitrogen oxides to the reducing gas in the process tail gas is 1: 1-1: 10.
Compared with the prior art, the invention has the following advantages:
(1) two reactors with different reaction temperatures are adopted to respectively reduce components with larger difference in reduction conditions in the tail gas, so that oxynitride in the tail gas can be effectively removed, and the content of oxynitride and alkyl nitrite is effectively reduced;
(2) the two reactors are respectively designed as a constant temperature reactor and an adiabatic reactor, so that the design difficulty of equipment is reduced, the high-temperature inactivation of a large amount of catalysts is avoided, and the treatment cost is reduced;
(3) the whole process flow is simple, the energy consumption is low, and the economic benefit and the environmental benefit are higher.
Drawings
FIG. 1 is a process flow diagram of the present invention;
in the figure, 1 is a process tail gas, 2 is a reducing gas, 3 is a process tail gas after primary reduction, 4 is a process tail gas after secondary reduction, 5 is a washing liquid, 6 is a washed gas material, 7 is a washing tower waste liquid, 8 is a standard exhaust gas, R1 is a constant temperature reactor, R2 is an adiabatic reactor, R3 is a combustion device, and C1 is a washing tower.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
Mixing a process tail gas 1 containing nitrogen oxides and methyl nitrite and a reducing gas 2 from esterification recycle gas, and feeding the mixture into a preheater for preheating, wherein the mixed gas comprises 8.9 volume percent of nitrogen oxides and CH3ONO 2.5 vol%, CO8.5 vol%, H244.5 vol%, the remainder N2、CO2、H2O; then introducing the two into a thermostatic reactor R1 containing Pt and Pd catalysts together for catalytic reduction, wherein the operating pressure of the thermostatic reactor R1 at the first section is 0.1Mpa, and the operating temperature is 230 ℃; the tail gas 3 of the process after the first-stage reduction enters a two-stage adiabatic reactor R2 for catalytic reduction, and the adiabatic reactorThe operation pressure of the thermal reactor R2 is 0.1Mpa, the operation temperature is 350 ℃, and the whole gas space velocity of the whole process is 200h-1. Through detection, the content of methyl nitrite in the gas from the adiabatic reactor R2 is 0mg/m3The NOx content is less than 10mg/m3. Introducing the process tail gas 4 after the two-stage reduction into the bottom of a washing tower C1, blending a washing liquid 5 into the top of the washing tower C1, wherein the washing liquid 5 is a water-containing liquid, and absorbing, washing and removing NH in the tail gas in a washing tower C13And (3) when alkaline gas is used, discharging a washing tower waste liquid 7 containing ammonia gas at the bottom of a washing tower C1, feeding a washed gas material 6 from the top of a washing tower C1 into a combustion device R3 for combustion treatment, and obtaining a standard exhaust gas 8 in a combustion device R3.
Example 2
Mixing a process tail gas 1 containing nitrogen oxides and methyl nitrite and a reducing gas 2 from esterification recycle gas, and feeding the mixture into a preheater for preheating, wherein the mixed gas comprises 12.2 volume percent of nitrogen oxides and CH3CH2ONO 3.4 vol%, CO 12.0 vol%, H223.5 vol%, the remainder N2、CO2、H2O; then introducing the two into a thermostatic reactor R1 containing Au and Pd catalysts together for catalytic reduction, wherein the operating pressure of the thermostatic reactor R1 at the first section is 0.1Mpa, and the operating temperature is 260 ℃; the tail gas 3 of the first-stage reduction process enters a second-stage adiabatic reactor R2 for catalytic reduction, the operating pressure of the adiabatic reactor R2 is 0.1Mpa, the operating temperature is 320 ℃, and the whole gas space velocity of the whole process is 180h-1. Through detection, the content of ethyl nitrite in the gas from the adiabatic reactor R2 is 0mg/m3The NOx content is less than 10mg/m3. Introducing the process tail gas 4 after the two-stage reduction into the bottom of a washing tower C1, blending a washing liquid 5 into the top of the washing tower C1, wherein the washing liquid 5 is a water-containing liquid, and absorbing, washing and removing NH in the tail gas in a washing tower C13And (3) when alkaline gas is used, discharging a washing tower waste liquid 7 containing ammonia gas at the bottom of a washing tower C1, feeding a washed gas material 6 from the top of a washing tower C1 into a combustion device R3 for combustion treatment, and obtaining a standard exhaust gas 8 in a combustion device R3.
Examples 3 to 5
The processes of examples 3 to 5 are the same as those of example 1, except that the compositions of the process off-gas 1 and the reducing gas 2, and specific process parameters and stream parameters are shown in table 1.
Examples 6 to 7
The process procedures of the embodiments 6 to 7 are the same as those of the embodiment 1, except that the composition of the process tail gas 1 and the reducing gas 2, and the process tail gas 1 is purge gas after an alkyl nitrite regeneration absorption tower, and specific process parameters and stream parameters are shown in table 1.
TABLE 1 examples 3-7 Process parameters
aThe rest is N2、CO2、H2O。
As can be seen from Table 1, for process off-gases of different compositions, the process of the present invention can achieve a RONO content of 0 after reaction in the final exhaust gas up to standard, NOxThe content is less than 10mg/m3And the national emission standard is reached.
Example 8
Mixing a process tail gas 1 containing nitrogen oxides and methyl nitrite and a reducing gas 2 from esterification recycle gas according to the volume ratio of 1:10, and entering the mixture into a preheater for preheating, wherein the finally mixed gas comprises 6.2 volume percent of nitrogen oxides and CH3ONO1.8 vol%, CO 6.2 vol%, H261.5 vol%, the remainder N2、CO2、H2O; then introducing the two into a thermostatic reactor R1 containing Pt and Pd catalysts together for catalytic reduction, wherein the operating pressure of the thermostatic reactor R1 at the first section is 1.0Mpa, and the operating temperature is 270 ℃; the tail gas 3 of the first-stage reduction process enters a second-stage adiabatic reactor R2 for catalytic reduction, the operating pressure of the adiabatic reactor R2 is 1Mpa, the operating temperature is 600 ℃, and the whole gas space velocity of the whole process is 50h-1. Through detection, the content of methyl nitrite in the gas from the adiabatic reactor R2 is 0mg/m3The NOx content is less than 10mg/m3. Returning the two sections toIntroducing the original process tail gas 4 into the bottom of a washing tower C1, blending a washing solution 5 into the top of the washing tower C1, wherein the washing solution 5 is a water-containing liquid, and absorbing, washing and removing NH in the tail gas in a washing tower C13And (3) when alkaline gas is used, discharging a washing tower waste liquid 7 containing ammonia gas at the bottom of a washing tower C1, feeding a washed gas material 6 from the top of a washing tower C1 into a combustion device R3 for combustion treatment, and obtaining a standard exhaust gas 8 in a combustion device R3.
Example 9
Mixing a process tail gas 1 containing nitrogen oxides and methyl nitrite from esterification recycle gas and a reducing gas 2 according to the volume ratio of 1:1, and entering the mixture into a preheater for preheating, wherein the finally mixed gas comprises 13.8 volume percent of nitrogen oxides and CH3CH2ONO 3.88 vol%, CO 13.8 vol%, H213.8 vol%, the remainder N2、CO2、H2O; then introducing the two into a thermostatic reactor R1 containing Pt and Pd catalysts together for catalytic reduction, wherein the operating pressure of the thermostatic reactor R1 at the first section is 0.1Mpa, and the operating temperature is 150 ℃; the tail gas 3 of the first-stage reduction process enters a second-stage adiabatic reactor R2 for catalytic reduction, the operating pressure of the adiabatic reactor R2 is 0.1Mpa, the operating temperature is 180 ℃, and the whole gas space velocity of the whole process is 1000h-1. Through detection, the content of methyl nitrite in the gas from the adiabatic reactor R2 is 0mg/m3,NOxThe content is less than 10mg/m3. Introducing the process tail gas 4 after the two-stage reduction into the bottom of a washing tower C1, blending a washing liquid 5 into the top of the washing tower C1, wherein the washing liquid 5 is a water-containing liquid, and absorbing, washing and removing NH in the tail gas in a washing tower C13And (3) when alkaline gas is used, discharging a washing tower waste liquid 7 containing ammonia gas at the bottom of a washing tower C1, feeding a washed gas material 6 from the top of a washing tower C1 into a combustion device R3 for combustion treatment, and obtaining a standard exhaust gas 8 in a combustion device R3.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (10)
1. A process method for removing nitrogen oxides and alkyl nitrite gases in tail gas is characterized by comprising the following steps:
(1) mixing the process tail gas with the reducing gas, carrying out reduction reaction through a first-stage reactor and a second-stage reactor, and catalytically reducing nitrogen oxides and alkyl nitrite in the process tail gas into nitrogen, wherein the temperature of the first-stage reactor is 150-270 ℃, and the temperature of the second-stage reactor is 180-600 ℃;
(2) feeding the reduced gas material into a washing tower for liquid absorption to remove NH3;
(3) And (3) burning the gas material obtained in the step (2).
2. The process for removing nitrogen oxides and alkyl nitrite in tail gas as claimed in claim 1, wherein the first-stage reactor is a constant temperature reactor, and the second-stage reactor is an adiabatic reactor.
3. The process method for removing nitrogen oxide and alkyl nitrite in tail gas as claimed in claim 1, wherein the reaction pressure of the first stage reactor and the second stage reactor is 0.1-1 MPa in terms of absolute pressure, and the gas space velocity is 50-10000 h-1。
4. The process for removing nitrogen oxides and alkyl nitrite gas in tail gas according to claim 1, wherein the active component of the catalyst in the primary reactor comprises one or more of V, Mn, Fe, Co, Ni, Cu, Ag, Pt, Pd, Rh, Ru or Au; the active component of the catalyst in the two-stage reactor comprises one or more of V, Mn, Fe, Co, Ni, Cu, Ag, Pt, Pd, Rh, Ru or Au.
5. The process for removing nitrogen oxides and alkyl nitrite gases in tail gas as claimed in claim 1, wherein the washing liquid in the washing tower is an aqueous liquid.
6. The process method for removing nitrogen oxides and alkyl nitrite gases in tail gas as claimed in claim 1, wherein the step (3) is specifically to perform combustion treatment on the gas material obtained in the step (2) to recover heat or send the gas material into a torch.
7. The process method for removing nitrogen oxide and alkyl nitrite in tail gas as claimed in claim 1, wherein the tail gas is esterification recycle gas or purge gas of esterification recycle gas after passing through alkyl nitrite regeneration absorption tower.
8. The process for removing nitrogen oxides and alkyl nitrite gases in tail gas as claimed in claim 1, wherein the components of nitrogen oxides comprise NO and NO2、N2O4Or N2O, wherein the volume concentration of the nitrogen oxides in the process tail gas is less than 30%; the alkyl nitrite comprises one or more of methyl nitrite, ethyl nitrite and isopropyl nitrite, and the volume concentration of the alkyl nitrite in the process tail gas is less than 10%.
9. The process for removing nitrogen oxides and alkyl nitrite in tail gas as claimed in claim 1, wherein said reducing gas is selected from CO and H2、NH3Or one or more of hydrocarbons.
10. The process method for removing nitrogen oxides and alkyl nitrite gases in tail gas as claimed in claim 1, wherein the volume ratio of nitrogen oxides to reducing gases in the tail gas is 1: 1-1: 10.
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DE3145331C1 (en) * | 1981-11-14 | 1983-06-09 | Nukem Gmbh, 6450 Hanau | A process for removing nitrous gases from gas mixtures |
SE8405665D0 (en) * | 1984-11-13 | 1984-11-13 | Bruno Stefan Javorsky | PROCEDURE AND PROCEDURE TO CONTAIN NITROGEN OXIDES |
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CN108136329A (en) * | 2015-10-28 | 2018-06-08 | 卡萨尔公司 | The method and apparatus that NOx and N2O is removed from gas |
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