CN1242251A - Adsorption separation method for removing nitrogen oxide(s) and sulfer oxide(s) from gas coming from lime kiln - Google Patents
Adsorption separation method for removing nitrogen oxide(s) and sulfer oxide(s) from gas coming from lime kiln Download PDFInfo
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- CN1242251A CN1242251A CN 99114940 CN99114940A CN1242251A CN 1242251 A CN1242251 A CN 1242251A CN 99114940 CN99114940 CN 99114940 CN 99114940 A CN99114940 A CN 99114940A CN 1242251 A CN1242251 A CN 1242251A
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Abstract
The circulating system of present method has at least two adsorption beds packed with adsorbent, each of the adsorption beds proceeds adsorption, reverse relieving pressure, heating and flushing, cold blowing, pressurizing sequentially to adsorb NOx, SOx and obtain purified gas, then desorbs NOx, SOx and regenerates the adsorbent. Said adsorbent has at least one carrier of aluminium oxide, silica gel or active carbon, on the carrier, there is at least one compound of Na, K, Ca, Fe, Cu, Mg, Zn metallic elements, the metal content is 0.3-10% of the adsorbent. The NOx, SOx content in the purified gas is less than 1 ppm and CO2 content remains unchanged. The invented method is suitable for use to treat the lime kiln gas.
Description
The present invention relates to gas separation method, particularly from gaseous mixture, remove NOx, SOx method.
Lime industry can produce a large amount of limekiln gas in the calcination process of lime, its component and content thereof such as following table:
| Component | ??N 2 | ???O 2 | ??CO 2 | ????NOx | ??SOx | H 2O |
| ??V％ | 50～70 | ??5～15 | ?15～40 | ?20～1000ppm | 3～100ppm | Saturated |
This limekiln gas is put into atmosphere usually after dedusting, also can utilize this limekiln gas, and the pressure swing absorption process that adopts Chinese patent 2L 88 1 05938.2 to be introduced is with contained CO
2Gas extraction is come out, as useful product, for example as food-class CO
2, as the additive of beverage, steelwork converter bottom blowing gas etc.When the lime-kiln gas body is used for such use, must be removed to below the 1ppm at first with objectionable impurities such as wherein contained NOx, SOx, could further purify then and utilize CO
2The method that industrialization at present 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, in temperature is under 200～770 ℃ the condition, to 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, and institute's water generally will be below-5 ℃.
(3) pressurization water at low temperature absorption process
Also be a kind of method commonly used, absorption pressure is more than 1.1MPa, and the NOx concentration of emission is below 200ppm, and when pressure during at 2.0MPa, NOx removes precision and can reach 40ppm.
All there be removing that precision is not high, energy consumption is high, flow process is complicated, investment is big, can reducing CO of NOx in above several method
2Therefore the shortcoming of concentration is not suitable for removing of contained NOx in the gas of limekiln, SOx gas.
The external existing in recent years method that adopts the alternating temperature absorption method to remove the NOx in the gas, these class methods are the NOx gas that adopts 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 7-256054 adopts sharp iron ore type titanium dioxide to make adsorbent, and adopts the heating alternating temperature to carry out the regeneration of adsorbent.But when purification contains the gaseous mixture of NOx, SOx, must carry out in two steps, at first remove SOx, and then remove NOx, otherwise can cause adsorbent to poison and influence the absorption of NOx.And for example the method in Japanese patent laid-open 7-200283 also adopts sharp iron ore type titanium dioxide adsorbent, but also 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 this adsorbent is higher than 150 ℃.And because modenite is to CO
2Have very strong adsorptivity, therefore be not suitable for from sources of the gas such as limekiln gas, keep CO
2Content carries out the purified treatment that removes of NOx, SOx.
Given this, the object of the present invention is to provide a kind ofly can from the gas of limekiln, can remove NOx, SOx simultaneously, do not influence CO
2Content removes the high adsorption method of separation that removes NOx, SOx from the gas of limekiln of precision.
The present invention adopts and selects suitable adsorbent and adopt transformation, alternating temperature reproducing adsorbent to realize its purpose.
Of the present inventionly from the gas of limekiln, remove NOx, the adsorption method of separation of SOx (referring to accompanying drawing), in the circular flow system that at least two adsorbent beds that are filled with adsorbent are arranged, each adsorbent bed of circular flow each time of system adsorbs successively, the reverse pressure of putting, add heat flush, cold blowing, the pressurising step, lime-kiln gas in service is sent into from the adsorbent bed feed end, through adsorbents adsorb NOx, SOx, the purified gas that obtains is discharged from discharge end, reproducing adsorbent then, desorb removes NOx, SOx, above-mentioned adsorbent is at aluminium oxide, silica gel, on at least a carrier in the absorbent charcoal carrier, supported sodium, potassium, calcium, iron, copper, magnesium, at least a compound in the compound of zinc metallic element, and tenor is the adsorbent of 0.3%-10%.
Above-mentioned compound can be selected di-iron trioxide or calcium oxide or potassium hydroxide or potash or NaOH or zinc chloride for use.
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 0.05～1.5Mpa, 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 can be with purified gas from discharge end or send into adsorbent bed with unstripped gas from feed end and carry out pressurising, also can send into adsorbent bed from discharge end and unstripped gas simultaneously from feed end with purified gas and carry out pressurising.
Above-mentioned add heat flush, cold blowing step to send into the gas of adsorbent bed can be purified gas, also can be air, or nitrogen, or the waste gas that produces of other commercial plant such as the pressure-swing absorption apparatus waste gas, the pressure-changed adsorption concentrating CO that produce
2The waste gas that device produces.
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, then the adsorbent in the adsorbent bed adsorbs NOx, SOx, be adsorbed back gained purified gas and discharge from the discharge end at adsorbent bed top, NOx, SOx are less than 1ppm in its purified gas.When the forward position of adsorption zone was moved upwards up near the adsorbent bed top, NOx, SOx ended unstripped gas and send into after reaching in discharging gas and setting concentration, stop absorption, 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, promptly gas is emitted and is reached atmospheric pressure state from adsorbent bed bottom feed end.
(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, the SOx desorb that are 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
The pressure purified gas is sent into adsorbent bed from discharge end, boost to adsorptive pressure 0.01～1.5MPa.For the adsorption step that enters circulation next time is 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 adding heat flush and cold blowing step, also can use the gas that does not contain NOx, SOx, the waste gas that produces as air, nitrogen, pressure-swing absorption apparatus etc. carries out.
Each adsorbent bed in the circulatory system of the present invention 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 selected adsorbent of the present invention to the adsorptivity of NOx, is not subjected to SOx and H
2The influence that O exists is compared with existing technology, need not to adopt to remove SOx and H in advance
2Remove the two-step method of NOx behind the O again.Adsorbent of the present invention has simultaneously NOx adsorption, SOx, and to the characteristics of the high adsorption capacity of NOx, SOx, NOx content is removed to from 20～1000ppm is lower than 1ppm, and the content of SOx is removed to from 3～100ppm and is lower than 1ppm.Moreover this adsorbent has and can not be higher than under 150 ℃ the regeneration temperature the thoroughly characteristics of desorption, and sorbent used to be higher than 150 ℃ regeneration temperature low than prior art, and reduced the regeneration energy consumption.Therefore, the present invention has can disposablely effectively remove contained NOx, SOx in the gas of limekiln simultaneously, and technological process is simpler, removes the precision height, advantage of low energy consumption.
Two, the selected adsorbent of the present invention has adsorbance to NOx, SOx much larger than CO
2Characteristics, as adsorbents adsorb CO
2When reaching capacity very soon, still far away can be saturated to the absorption of NOx, SOx, so it can not influence CO
2Concentration, when the NOx in removing limekiln gas, SOx, can in purified gas, keep CO
2Concentration, thereby be convenient to from purified gas to extract and utilize CO
2
Three, the selected adsorbent of the present invention is not subjected to the influence of moisture content, therefore as the water content in the limekiln gas of unstripped gas, can not influence the precision that removes of NOx of the present invention, SOx.Compared with the prior art, need not carry out drying to unstripped gas in advance and handle, thus the corresponding technology of having simplified.
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:
The adsorption method of separation that from the gas of limekiln, removes NOx, SOx of the present invention, employing is by 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.Unstripped gas is for containing CO
220%, O
211%, N
269%, the limekiln gas of NOx 655ppm, SOx 40ppm, flow is 15000Nm
3/ h is forced into 1.2MPa, after being cooled to 38 ℃, sends into this device.Adsorbent adopts the di-iron trioxide contain 0.5% iron and contains the active carbon of the sodium carbonate of 5% sodium.
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 now with the A tower, adsorption separation process is described, unstripped gas after compression, through pipeline 10, valve 1A, send into the A tower from bottom to top from the feed end of A tower bottom, carry out adsorption step, the NOx in the unstripped gas, SOx are adsorbed by the adsorbent in the tower, are purified gas, from the discharge end of A top of tower, send through valve 2A, pipeline 20.At this moment, the valve 1A, the valve 2A that link with the A tower open, and valve 3A, valve 4A then are in closed condition.Adsorbent in the A tower is inhaled saturated NOx, SOx, 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, allow a part of purified gas be the heater E of electricity or steam through heating source, be heated to 150 ℃ with indirect mode, again through pipeline 30, valve 4A sends into the A tower from the top, carry out the heating rinsing step, adds heat-adsorbent, along with adsorbent constantly is heated, adsorbate NOx, SOx are 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 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.Through reversely putting pressure, adding heat flush and cooled stripping gas is regeneration gas.Regeneration gas is at the bottom of the A tower, and through valve 3A, pipeline 40 is discharged outside the towers, can send into limekiln gas chimney, in alkali lye and the back discharge.Shut off valve 4A, valve 3A then, open valve 2A enters the pressurising step, and purified gas is sent 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 be by increasing a binding pipeline 110 and valve 6AB at the feed end of A tower, B tower, will send into the shunting of B tower feed end unstripped gas and send into from A tower feed end and carry 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, 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, adsorbed 6 hours, and reverse putting pressed 5 minutes, add heat flush 3 hours, cold blowing flushing 2.5 hours, pressurising 25 minutes.The pressure of heating rinsing step is 0.05MPa.The temperature of heating rinsing step is 130 ℃.
Use the inventive method, remove NOx, SOx after, in the purified gas of acquisition, contain CO
220%, NOx＜1ppm, SOx＜1ppm, all the other are N
2And O
2CO wherein
2Content identical with content in the gas of limekiln.
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:
Of the present inventionly from the gas of limekiln, remove NOx, the adsorption method of separation of SOx, 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, the pipeline 60 of output purified gas, pipeline 70, the pipeline 80 of heater E 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 mutually, 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, the pressure and temperature varying adsorption system device that valve 6C etc. constitute, its flow process as shown in Figure 2.Unstripped gas is for containing CO
225%, O
28%, N
267%, the limekiln gas of NOx 310ppm, SOx 84ppm, its flow is 36000Nm
3/ h is forced into 0.3Mpa, sends into this device after being cooled to 40 ℃, and adsorbent adopts the silica gel of the potash contain 5% metallic potassium.
The running of present embodiment and embodiment 1 are similar.Because absorption, reversely put pressure, add heat flush, cold blowing, the temporal needs of each step of pressurising, adding between heat flush and the cold blowing step, isolation step is set.
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 of heating rinsing step is 0.05MPa.The temperature of heating rinsing step is 100 ℃.The used regeneration gas of heating rinsing step adopts pressure-changed adsorption concentrating CO
2The waste gas that device produces.
Use the inventive method, remove NOx, SOx after, in the purified gas of acquisition, contain CO
2, NOx＜1ppm, SOx＜1ppm, all the other are N
2And O
2CO wherein
2Content identical with content in the gas of limekiln.
Table 2 three tower time-scales
| The A tower | Absorption | Reverse bleeding off pressure | Add heat flush | Isolation | Cold blowing | Pressurising | |||
| The B tower | Isolation | Cold blowing | Pressurising | Absorption | Reverse bleeding off pressure | Add heat flush | Isolation | ||
| The C tower | Reverse bleeding off pressure | Add heat flush | Isolation | Cold blowing | Pressurising | Absorption | |||
Claims (6)
1, from the gas of limekiln, remove NOx, the adsorption method of separation of SOx, it is characterized in that in the circular flow system that at least two adsorbent beds that are filled with adsorbent are arranged, each adsorbent bed of circular flow each time of system adsorbs successively, the reverse pressure of putting, add heat flush, cold blowing, the pressurising step, lime-kiln gas in service is sent into from the adsorbent bed feed end, through adsorbents adsorb NOx, SOx, the purified gas that obtains is discharged from discharge end, reproducing adsorbent then, desorb removes NOx, SOx, above-mentioned adsorbent is at aluminium oxide, silica gel, on at least a carrier in the absorbent charcoal carrier, supported sodium, potassium, calcium, iron, copper, magnesium, at least a compound in the compound of zinc metallic element, and tenor is the adsorbent of 0.3%-10%.
2, adsorption method of separation according to claim 1 is characterized in that said compound is ferric oxide or calcium oxide or potassium hydroxide or potash or NaOH or zinc chloride.
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 0.05～1.5Mpa, 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 carry out pressurising, or simultaneously send into adsorbent bed from discharge end and unstripped gas from feed end with purified gas and carry out pressurising.
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 the waste gas that purified gas or air or nitrogen or pressure-swing absorption apparatus produce.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99114940A CN1087962C (en) | 1999-06-18 | 1999-06-18 | Adsorption separation method for removing nitrogen oxide(s) and sulfer oxide(s) from gas coming from lime kiln |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99114940A CN1087962C (en) | 1999-06-18 | 1999-06-18 | Adsorption separation method for removing nitrogen oxide(s) and sulfer oxide(s) from gas coming from lime kiln |
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| CN1087962C CN1087962C (en) | 2002-07-24 |
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| CN102380281A (en) * | 2010-07-08 | 2012-03-21 | 气体产品与化学公司 | Recycle TSA regen gas to boiler for oxyfuel operations |
| CN101822929B (en) * | 2010-02-02 | 2012-06-06 | 华东理工大学 | Method for capturing carbon dioxide by utilizing electrical desorption technology |
| CN104248941A (en) * | 2013-06-27 | 2014-12-31 | 中国石油化工股份有限公司 | Purifying agent for adsorbing volatile oxides in MTO tail gas and preparation method thereof |
| CN105664705A (en) * | 2016-01-12 | 2016-06-15 | 宁夏宁东诚鑫环保新材料科技有限公司 | Limestone and attapulgite mixed desulfurizing agent |
| CN106237821A (en) * | 2016-07-21 | 2016-12-21 | 石家庄新华能源环保科技股份有限公司 | A kind of limekiln denitrating system |
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| CN106345393A (en) * | 2016-08-26 | 2017-01-25 | 苏州金宏气体股份有限公司 | Nitrogen dioxide adsorbent, nitrogen dioxide absorbing device and manufacturing method of nitrogen dioxide absorbing device |
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| CN105597488B (en) * | 2015-12-25 | 2019-01-15 | 杨皓 | A method of nitrogen and rich sour gas are produced from flue gas using pressure swing adsorption technique |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3226840A1 (en) * | 1982-07-17 | 1984-02-16 | Kernforschungsanlage Jülich GmbH, 5170 Jülich | METHOD FOR SEPARATING AND RECYCLING NO (DOWN ARROW) X (DOWN ARROW) GAS SHARES BY ADDING AND DESORPING MOLSIEB |
| DE4129166A1 (en) * | 1991-09-03 | 1993-03-04 | Nymic Anstalt | METHOD FOR PURIFYING SMOKE GAS |
| FR2714301B1 (en) * | 1993-12-24 | 1996-03-15 | Jacques Bellini | Device and method for purifying a gas, in particular for producing pure air. |
| JPH07256054A (en) * | 1994-03-22 | 1995-10-09 | Hitachi Zosen Corp | Apparatus and method for adsorbing and removing nox |
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1999
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| CN101822929B (en) * | 2010-02-02 | 2012-06-06 | 华东理工大学 | Method for capturing carbon dioxide by utilizing electrical desorption technology |
| CN102380281A (en) * | 2010-07-08 | 2012-03-21 | 气体产品与化学公司 | Recycle TSA regen gas to boiler for oxyfuel operations |
| CN102380281B (en) * | 2010-07-08 | 2014-07-09 | 气体产品与化学公司 | Recycle TSA regen gas to boiler for oxyfuel operations |
| CN104248941A (en) * | 2013-06-27 | 2014-12-31 | 中国石油化工股份有限公司 | Purifying agent for adsorbing volatile oxides in MTO tail gas and preparation method 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 |
| CN105664705A (en) * | 2016-01-12 | 2016-06-15 | 宁夏宁东诚鑫环保新材料科技有限公司 | Limestone and attapulgite mixed desulfurizing agent |
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| CN106345393A (en) * | 2016-08-26 | 2017-01-25 | 苏州金宏气体股份有限公司 | Nitrogen dioxide adsorbent, nitrogen dioxide absorbing device and manufacturing method of nitrogen dioxide absorbing device |
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