CN1087963C - Removing and recovering nitrogen oxide(s) by adsorption separation method from mixed gas contg. nitrogen oxide(s) - Google Patents
Removing and recovering nitrogen oxide(s) by adsorption separation method from mixed gas contg. nitrogen oxide(s) Download PDFInfo
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- CN1087963C CN1087963C CN99114941A CN99114941A CN1087963C CN 1087963 C CN1087963 C CN 1087963C CN 99114941 A CN99114941 A CN 99114941A CN 99114941 A CN99114941 A CN 99114941A CN 1087963 C CN1087963 C CN 1087963C
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Abstract
The present invention relates to a gas separation method, and the aim of the present invention is to solve the problem of low NOx elimination precision existing in the prior art. The method is carried out in circulation systems of at least two adsorption beds filled with adsorbing agents, each adsorption bed orderly achieves adsorption, reverse releasing, heating washing, cold blowing and pressurization, NOx is adsorbed by the adsorption agents, then the NOx is recovered through desorption elimination, and adsorbing agents are generated again. At least one of compounds containing potassium, sodium, iron, copper, magnesium and zinc is loaded on at least one of carriers such as activated carbon, aluminum oxide and silicon dioxide to form the adsorbing agents, and the metal content of the adsorbing agents is from 0.5 to 15%. The method can recycle NOx, and the minimum content of NOx in the clean gas can be less than 1 ppm, so that the clean gas can be directly discharged. The method has the advantages of simple process, etc.
Description
The present invention relates to gas separating method, particularly from gaseous mixture, remove and reclaim the method for NOx.
The method that existing industrialization removes NOx has following several:
(1) catalytic reduction method
This method is to add ammonia or methane and through cupric or platinum, palladium catalyst in the mist that contains NOx gas, is under 200～270 ℃ the condition in temperature.Be reduced into N
2And H
2O.This method will consume a large amount of catalyst and ammonia, and it is lower to remove the precision of NOx, is generally 200～500ppm.
(2) alkali absorb method
Be a kind of method commonly used, its shortcoming be NOx to remove precision very low, even follow-on alkali absorb method, its precision that removes NOx is still about 800ppm.
(3) pressurization water at low temperature absorption process
Also be a kind of method commonly used, its absorption pressure more than 1.1MPa, the NOx concentration of emission below 200ppm, when pressure at 2.0MPa, the temperature of washings is in the time of-5 ℃, NOx removes precision and can reach 40ppm.
Above several method exists all that NOx's remove that precision is not high, energy consumption is high, flow process is complicated, investment is big or secondary pollution is arranged.
Abroad also have in recent years to relate to the method that adopts the alternating temperature absorption method to remove the NOx in the gas, these class methods are to adopt NOx gas in the adsorbents adsorb gaseous mixture, adopt the thermal regeneration adsorbent then and remove NOx in the gaseous mixture.Method in Japanese patent laid-open 7-200283 adopts sharp iron ore type titanium dioxide adsorbent, must carry out drying to unstripped gas before absorption.Method in BP GB2124103, the adsorbent of employing are the modenites that contains the H ion, and the regeneration temperature of adsorbent is higher than 150 ℃.
Given this, the object of the present invention is to provide a kind ofly can from the gaseous mixture that contains NOx, remove and reclaim NOx, and remove the high adsorption separating method of precision.
The present invention adopts and selects optimum adsorbent and adopt transformation, alternating temperature reproducing adsorbent to realize its purpose on the basis of the method for existing alternating temperature adsorbing and removing NOx.
The adsorption method of separation (referring to accompanying drawing) that from the mist that contains NOx, removes and reclaim NOx of the present invention, have in the circular flow system of at least two adsorbent beds that are filled with adsorbent, the circular flow each time of system, each adsorbent bed adsorbs successively, reversely put pressure, add heat flush, cold blowing, pressurising step, unstripped gas is sent into from the feed end of adsorbent bed, and through adsorbents adsorb NOx, the purified gas of acquisition is discharged from discharge end, reproducing adsorbent then, desorb removes and reclaims NOx.Above-mentioned adsorbent is at least a carrier in active carbon, aluminium oxide, silica-gel carrier, support at least a compound in the compound that contains metallic element potassium, sodium, calcium, iron, copper, magnesium, zinc, its tenor is the adsorbent of 0.5%-15%.
Above-mentioned compound can be potassium hydroxide or cupric oxide or di-iron trioxide or potash.
The quantity of the adsorbent bed in the adsorption method of separation of the invention described above is determined according to the treating capacity of gas, adopts two adsorbent beds when less treating capacity, adopts when bigger treating capacity more than two, as the circulatory system of the continuous running of 3～4 adsorbent beds.
The final pressure of the pressure of above-mentioned adsorption step and pressurising step is 0.05～2.0MPa, and the pressure of heating rinsing step, cold blowing step is 0.01～0.5MPa.
The temperature of above-mentioned heating rinsing step is 70～150 ℃.
Above-mentioned pressurising step, or is simultaneously sent into adsorbent bed from discharge end and unstripped gas from feed end with purified gas and is boosted from discharge end or send into adsorbent bed with unstripped gas from feed end and boost with purified gas.
Above-mentioned add heat flush, cold blowing step to send into the gas of adsorbent bed be purified gas or air.
Below, the step that the institute of circulation each time at each adsorbent bed of circular flow is experienced successively elaborates:
(1) absorption
The unstripped gas that with pressure is 0.05～1.5MPa is from the feed end of bottom sending in the adsorbent bed from bottom to top, and then the adsorbent in the adsorbent bed adsorbs NOx, is adsorbed back gained purified gas and discharges emptying from the discharge end at adsorbent bed top.When the forward position of adsorption zone was moved upwards up to appropriate location near the adsorbent bed top, NOx ended unstripped gas and sends into, stops absorption after reaching in discharging gas and setting concentration, and other adsorbent bed that this moment, unstripped gas was admitted to pressurising adsorbs.
(2) the reverse pressure of putting
Make adsorbent bed airflow direction against when absorption under adsorptive pressure put pressure, gas is emitted from the adsorbent bed bottom and is reached atmospheric pressure state.
(3) add heat flush
The band that other adsorbent bed is discharged is pressed the part in the cold air of purified gas, is decompressed to 0.01～0.5MPa, after heater via is heated to 70～150 ℃, from top to bottom by adsorbent bed, promptly enter from discharge end, feed end is discharged, make the NOx desorb that is adsorbed, adsorbent is reproduced.Stop heating then.
(4) cold blowing
Continue to be fed into band and press the cold air of purified gas, adsorbent bed is washed, cools off, to reaching normal temperature.
(5) pressurising
Pressure purified gas discharge end is sent into adsorbent bed, boost to adsorptive pressure 0.01～1.5Mpa.The gas of sending into adsorbent bed also can be other gas that does not contain NOx, as air etc.For the adsorption step that enters circulation is next time prepared.So far finish cycle operation one time.
From above step as can be known, reversely putting pressure, add heat flush, cold blowing, four steps of pressurising, all is to adsorb saturated adsorbent and can reuse the regeneration means of being taked for making.
In running, recycle the reverse stripping gas of putting the discharge gas of pressure and adding the heat flush discharge.
Each adsorbent bed in the circulatory system all experiences identical step, just diverges mutually on the sequential, carries out continuously to guarantee separation process.There is the sequential of the processing step of the present invention of two adsorbent beds to see Table 1, has the sequential of the processing step of the present invention of three adsorbent beds to see Table two.
Adsorption method of separation of the present invention has following obvious advantage and remarkable result.
One, the adsorbent selected for use of the present invention is the adsorbent that adaptable essence is taken off NOx, presents alkalescent and certain activity at adsorbent surface, has the ability that strengthens NOx adsorption, improves the characteristic of the precision that removes NOx.Can from the gaseous mixture that contains NOx, remove effectively and recycle NOx, the NOx content in the gaseous mixture is removed to below the 30ppm, the minimum 1ppm that reaches from 50～2000ppm.The content of NOx can reach environmental requirement in the purified gas that is obtained, thus directly emptying.
Two, the adsorbent selected for use of the present invention, with active carbon, aluminium oxide, silica gel is carrier, compare with the zeolite in the prior art, the carrier of molecular sieve adsorbent, adsorbent of the present invention has the performance characteristics a little less than the absorption affinity of H2O, can not produce H as prior art
2Therefore the common adsorption phenomena of O and NOx needn't dehydrate unstripped gas before purification in advance.Adsorbent of the present invention also has regeneration temperature and is lower than below 150 ℃, and just the NOx desorb that can will adsorb is complete, thereby has simplified flow process, has reduced energy consumption.
Adsorption separating method of the present invention is applicable to from nitric plant's tail gas or other contain the gaseous mixture of NOx to remove NOx, thereby recycles NOx.
Below, use embodiment and accompanying drawing thereof again, the present invention is elaborated.
Brief description of drawings.
Fig. 1 is the process chart of a kind of adsorption method of separation of the present invention.Show the system of two adsorbent beds.
Fig. 2 is the process chart of another kind of adsorption method of separation of the present invention.Show the system of three adsorbent beds.
Embodiment 1:
A kind of adsorption method of separation that from the mist that contains NOx, removes and reclaim NOx of the present invention, employing has two common tower adsorbent bed A tower, B towers, common heater E, the pressure and temperature varying adsorption system device that corresponding pipeline, valve etc. constitute, its flow process is as shown in Figure 1.The nitric acid tail gas that unstripped gas selects for use the nitric acid production system to discharge contains NOx 2500ppm, and its flow is 5000Nm
3/ h under 0.45Mpa, sends into this device with unstripped gas after being cooled to 38 ℃.Adsorbent adopts the aluminium oxide that is loaded with 3% zinc chloride.
During the operation of this device, the A tower all experiences identical step with the B tower, just diverges mutually on the sequential, carries out continuously to guarantee operation.Be example with the A tower now, adsorption separation process is described, unstripped gas after compression, through pipeline 10, valve 1A sends into the A tower from bottom to top from the feed end of A tower bottom, carries out adsorption step, NOx in the unstripped gas is adsorbed by the adsorbent in the tower, be purified gas, from the discharge end of A top of tower, through valve 2A, pipeline 20 emptying, open with valve 1A, valve 2A that the A tower links this moment, and valve 3A, valve 4A then are in closed condition.Adsorbent in the A tower is inhaled saturated NOx, adsorbs at the end, and shut off valve 1A, valve 2A, open valve 3A carries out the reverse pressure step of putting, and with the pressed gas in the tower, at the bottom of the A tower, discharges outside the towers through valve 3A, pipeline 40.Open valve 4A then allows a part of purified gas heater via E, is heated to 150 ℃, and again through pipeline 30, valve 4A sends into the A tower from the top, carries out the heating rinsing step, adds heat-adsorbent, and along with adsorbent constantly is heated, NOx is also constantly by desorb.Behind the heating steps, connect the cold blowing step, stop heater E heating this moment, cold purified gas is still sent into tower through pipeline 30, valve 4A, by whole A tower, the heat that accumulates in the tower is taken away, till normal temperature from top to bottom.The discharge gas that reversely put pressure, adds heat flush, cooling step is regeneration gas, and all at the bottom of the A tower, through valve 3A, pipeline 40A discharges outside the tower.Shut off valve 4A, valve 3A then, open valve 2A enters the pressurising step, and purified gas is sent into the A tower from the discharge end of A top of tower, reaches till the adsorptive pressure, immediately shut off valve 2A.Finish a circular flow.Above-mentioned pressurising step also can be sent into the A tower from the feed end of A tower bottom with unstripped gas and carry out pressurising, can also be with purified gas from the discharge end of A top of tower with send into the A tower with unstripped gas simultaneously from the feed end of A tower bottom and carry out pressurising.Pressurising also can increase a binding pipeline 100 and valve 5AB by the discharge end at A tower, B tower, the purified gas of A tower discharge end is sent into from B tower discharge end carried out.Pressurising can also increase a binding pipeline 110 and valve 6AB by the feed end at A tower, B tower, the unstripped gas shunting of sending into B tower feed end is sent into from A tower feed end carried out.(dotted line among Fig. 1 shows pipeline 100, pipeline 110).
When the A tower is in adsorption step, the B tower then be in by reversely put pressure, add heat flush, the regenerative process of adsorbent bed that cold blowing, pressurising step constitute.The A tower be in by reversely put pressure, add heat flush, the regenerative process of adsorbent bed that cold blowing, pressurising constitute suddenly.The A tower be in by reversely put pressure, add heat flush, during the regenerative process of adsorbent bed that cold blowing, pressurising step constitute, the B tower then is in adsorption step, as shown in Table 1.The on off state of the valve 1B of B tower, valve 2B, valve 3B, valve 4B and the valve 1A of A tower, valve 2A, valve 3A, valve 4A are corresponding.
In the present embodiment, be the running time of each step, and the time of adsorption step is 6 hours, and reverse putting pressed 5 minutes, add heat flush 3 hours, cooling 2.5 hours, pressurising 25 minutes.Add heat flush and cold blowing and all carry out under 0.03Mpa pressure, the temperature that adds heat flush is controlled at 120 ℃,
Use the inventive method, remove NOx after, in the purified gas of acquisition, contain NOx＜30ppm, all the other are N
2And O
2, by directly emptying.Reverse discharge gas of pressing step and the stripping gas that heats the rinsing step discharge put returns the nitric acid production system after the pressurization cooling, reuptake and utilize NOx.The discharge pneumatic transmission of cooling step is gone into the tail gas blow-down pipe of nitric acid production system.
Table 1 liang tower time-scale
| The A tower | Absorption | The reverse pressure of putting | Add heat flush | Cold blowing | Pressurising | |||
| The B tower | The reverse pressure of putting | Add heat flush | Cold blowing | Pressurising | Absorption | |||
Embodiment 2
The adsorption method of separation that from the mist that contains NOx, removes and reclaim NOx of the present invention, employing has three common tower adsorbent bed A towers, the B tower, the C tower, common heater E, the pipeline 50 of input unstripped gas, carry the pipeline 60 of purified gas, pipeline 70, the pipeline 60 of heater is set, discharging regeneration gas is the pipeline 90 of stripping gas, and respectively with the A tower, the B tower, the valve 1A that the C tower is equipped, valve 2A, valve 3A, valve 4A, valve 5A, valve 6A, valve 1B, valve 2B, valve 3B, valve 4B, valve 5B, valve 6B, valve 1C, valve 2C, valve 3C, valve 4C, valve 5C, valve 6C, in the pressure and temperature varying adsorption system device that constitutes, its flow process as shown in Figure 2.The nitric acid tail gas that unstripped gas selects for use the nitric acid production system to discharge contains NOx 5000ppm, and its flow is 6000Nm
3/ h under 0.8Mpa pressure, sends into this device with unstripped gas after being cooled to 40 ℃.Adsorbent is selected the active carbon of the di-iron trioxide that is loaded with the sodium carbonate that contains sodium 6% and iron content 0.4% for use.
The running and the embodiment of present embodiment are similar.Because absorption, regeneration, the temporal needs of each step of pressurising adding between heat flush and the cold blowing step, are provided with isolation.
In the present embodiment, be the running time of each step, adsorbed 4 hours, and reverse putting pressed 5 minutes, add heat flush 3.5 hours, cold blowing 3.5 hours, pressurising 25 minutes.The pressure that regeneration pressure promptly adds heat flush, cooling step is 0.1MPa.The temperature that regeneration temperature promptly heats rinsing step is 105 ℃.Regeneration gas is an air.
Use the inventive method, remove NOx after, in the purified gas of acquisition, contain NOx＜30ppm, all the other are N
2And O
2, by directly emptying.Reverse discharge gas of pressing step and the stripping gas that heats the rinsing step discharge put returns the nitric acid production system after the pressurization cooling, reuptake and utilize NOx.The direct emptying of discharge gas of cooling step.
Table 2 three tower time-scales
| The A tower | Absorption | The reverse pressure of putting | Add heat flush | Isolate | Cold blowing | Pressurising | |||
| The B tower | Isolate | Cold blowing | Pressurising | Absorption | The reverse pressure of putting | Add heat flush | Isolate | ||
| The C tower | The reverse pressure of putting | Add heat flush | Isolate | Cold blowing | Pressurising | Absorption | |||
Claims (6)
1, from the mist that contains NOx, remove and reclaim the adsorption method of separation of NOx, it is characterized in that in the circular flow system that at least two adsorbent beds that are filled with adsorbent are arranged, the circular flow each time of system, each adsorbent bed adsorbs successively, the reverse pressure of putting, add heat flush, cold blowing, the pressurising step, unstripped gas is sent into from the feed end of adsorbent bed, through adsorbents adsorb NOx, the purified gas that obtains is discharged from discharge end, reproducing adsorbent then, desorb removes and reclaims NOx, the operational relation of each adsorbent bed is preceding adsorbent bed absorption back adsorbent bed absorption beginning at the end, above-mentioned adsorbent is at active carbon, aluminium oxide, on at least a carrier in the silica-gel carrier, support and contain metallic element potassium, sodium, calcium, iron, copper, magnesium, at least a compound in the compound of zinc, its tenor are the 0.5%-15% of adsorbent by weight.
2, adsorption method of separation according to claim 1 is characterized in that said compound is potassium hydroxide or cupric oxide or di-iron trioxide or potash.
3, adsorption method of separation according to claim 1 and 2 is characterized in that the pressure of said adsorption step and the final pressure of pressurising step are 0.05～2.0MPa, and the pressure of heating rinsing step, cold blowing step is 0.01～0.5MPa.
4, adsorption method of separation according to claim 1 and 2, the temperature that it is characterized in that said heating rinsing step is 70～150 ℃.
5, adsorption method of separation according to claim 1 and 2, it is characterized in that said pressurising step with purified gas from discharge end or send into adsorbent bed with unstripped gas from feed end and boost, or simultaneously send into adsorbent bed from discharge end and unstripped gas from feed end with purified gas and boost.
6, adsorption method of separation according to claim 1 and 2 is characterized in that saidly adding heat flush, cold blowing step to send into the gas of adsorbent bed being purified gas or air.
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| CN99114941A CN1087963C (en) | 1999-06-18 | 1999-06-18 | Removing and recovering nitrogen oxide(s) by adsorption separation method from mixed gas contg. nitrogen oxide(s) |
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| CN99114941A CN1087963C (en) | 1999-06-18 | 1999-06-18 | Removing and recovering nitrogen oxide(s) by adsorption separation method from mixed gas contg. nitrogen oxide(s) |
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| CN1087963C true CN1087963C (en) | 2002-07-24 |
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| CN102491292A (en) * | 2011-12-06 | 2012-06-13 | 中国成达工程有限公司 | Low-consumption and low-emission nitric acid production method and production equipment thereof |
| CN104248941B (en) * | 2013-06-27 | 2016-08-17 | 中国石油化工股份有限公司 | For adsorbing cleanser of volatile oxidn and preparation method thereof in MTO tail gas |
| CN106311134B (en) * | 2015-06-24 | 2019-03-26 | 中国石油化工股份有限公司 | Solid purificant and preparation method thereof |
| DE102018211819A1 (en) * | 2018-07-17 | 2020-01-23 | Audi Ag | Utilization of nitrogen oxides from the ambient air |
| CN110152606B (en) * | 2019-01-21 | 2022-03-29 | 北京工业大学 | Adsorbent for adsorbing NOx at low temperature and loading Mg/Dy or Na/Sm on ordered mesoporous C-FDU-15 and preparation method thereof |
| CN109966860A (en) * | 2019-04-16 | 2019-07-05 | 北京科技大学 | More temperature swing adsorption gas purification systems of one kind and technique |
| CN110639473A (en) * | 2019-10-22 | 2020-01-03 | 北京工业大学 | Modified activated carbon adsorbent for adsorbing NOx at high temperature and preparation method thereof |
| CN110940752B (en) * | 2019-12-17 | 2022-08-05 | 陕西延长石油（集团）有限责任公司 | Multi-element low-carbon hydrocarbon adsorption and desorption evaluation device and method |
| CN111437696A (en) * | 2020-05-09 | 2020-07-24 | 中国成达工程有限公司 | Containing NOxExhaust gas treatment system |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2124103A (en) * | 1982-07-17 | 1984-02-15 | Kernforschungsanlage Juelich | Process for separating and recycling nox gas components by adsorption and desorption on a molecular sieve |
| DE4129166A1 (en) * | 1991-09-03 | 1993-03-04 | Nymic Anstalt | METHOD FOR PURIFYING SMOKE GAS |
| FR2714301A1 (en) * | 1993-12-24 | 1995-06-30 | Bellini Jacques | Gas purificn. appts. with efficient regeneration of filter materials |
| JPH07200283A (en) * | 1993-12-29 | 1995-08-04 | Toshiba Corp | Exchange system for resident load module |
| JPH07256054A (en) * | 1994-03-22 | 1995-10-09 | Hitachi Zosen Corp | Apparatus and method for adsorbing and removing nox |
-
1999
- 1999-06-18 CN CN99114941A patent/CN1087963C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2124103A (en) * | 1982-07-17 | 1984-02-15 | Kernforschungsanlage Juelich | Process for separating and recycling nox gas components by adsorption and desorption on a molecular sieve |
| DE4129166A1 (en) * | 1991-09-03 | 1993-03-04 | Nymic Anstalt | METHOD FOR PURIFYING SMOKE GAS |
| FR2714301A1 (en) * | 1993-12-24 | 1995-06-30 | Bellini Jacques | Gas purificn. appts. with efficient regeneration of filter materials |
| JPH07200283A (en) * | 1993-12-29 | 1995-08-04 | Toshiba Corp | Exchange system for resident load module |
| JPH07256054A (en) * | 1994-03-22 | 1995-10-09 | Hitachi Zosen Corp | Apparatus and method for adsorbing and removing nox |
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