CN104437028A - Method for removing alkyl nitrite and nitrous oxide from tail gas - Google Patents
Method for removing alkyl nitrite and nitrous oxide from tail gas Download PDFInfo
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Abstract
The invention relates to a method for removing alkyl nitrite and nitrous oxide from tail gas, and mainly solves the problems that an additional reducing agent is required to be added, the tail gas is difficult to reach the standard, a reduction catalyst is poor in stability and easy to deactivate, and the like in the prior art. According to the adopted technical scheme, he method comprises the following steps: (a) conveying industrial tail gas containing reducing gas into a deep freezer, cooling the tail gas to 10 DEG C below with freeze water, and recycling alkyl nitrite carried in the tail gas; (b) conveying the cooled tail gas into an absorption tower, and absorbing the alkyl nitrite in the tail gas with alkyl alcohol to obtain alkyl alcohol solution containing alkyl nitrite; and (c) conveying a gaseous discharge material from the top of the absorption tower into a reactor, reacting non-absorbed alkyl nitrite and nitrous oxide with the reducing gas in the industrial tail gas to generate nitrogen in the presence of a catalyst, so that the problems are well solved, and the method can be used for removing the alkyl nitrite and the nitrous oxide from the tail gas.
Description
Technical field
The present invention relates to a kind of method removing alkyl nitrite and nitrogen oxide in industrial tail gas.
Background technology
Normal, pernicious gas poisonous containing alkyl nitrite and nitrogen oxide etc. in industrial tail gas; if by these gases directly discharged to air; environmental pollution can be caused; the health of harm humans; therefore must process the alkyl nitrite in industrial tail gas and nitrogen oxide, the gas total content making alkyl nitrite and nitrogen oxygen in the gas after processing change thing reaches or lower than the permission discharge standard of national environmental protection regulations of rules.Such as, in carbon monoxide gas phase legal system in the technique of dialkyl oxalate, just containing certain density alkyl nitrite and oxides of nitrogen gas in the tail gas of discharge, must process.
In prior art, Japanese Patent Laid-Open 11-315053 uses methyl alcohol that nitric oxide reaction is generated methyl nitrite, use methanol absorption methyl nitrite pair again, reclaim methyl nitrite can be used as organic synthesis raw material use, the large usage quantity of this method methyl alcohol, and methyl nitrite is also difficult to be completely absorbed.US Patent No. 4879401 provides a kind of method removing nitrogen oxide in alkyl nitrite preparation process, it adds low alkyl group alcohol in oxides of nitrogen gas, as methyl alcohol, ethanol, and oxygen, most reaction of nitrogen oxides generates alkyl nitrite, remain the nitrogen oxide of small part, alkyl nitrite and other gas and adopt low alkyl group alcohol circulation preparation, be alkyl nitrite by residual nitrogen oxygenate conversion, and looping back reaction together with existing alkyl nitrite, low alkyl group alcohol can be used as washing agent removing foreign gas simultaneously.Chinese patent CN100493674C provides the removal methods of a kind of alkyl nitrite and oxides of nitrogen gas, tail gas containing alkyl nitrite and nitrogen oxide is absorbed by alkylol in alkyl nitrite recovery tower, nitrogen oxide and a small amount of unabsorbed alkyl nitrite are in catalytic reduction reactor, the temperature of 200 ~ 600 DEG C, under the pressure of 0.05 ~ 1Mpa, be reduced to nitrogen by the reducibility gas newly added.
The technology of existing process alkyl nitrite and nitrogen oxide tail gas exists needs additionally to add reducing agent, tail gas is difficult to up to standard, the problems such as reducing catalyst poor stability, easy in inactivation.
Summary of the invention
Technical problem to be solved by this invention is that the needs that prior art exists additionally add reducing agent, tail gas is difficult to up to standard, the problems such as reducing catalyst poor stability, easy in inactivation, there is provided a kind of method removing alkyl nitrite and nitrogen oxide in industrial tail gas newly, the method has that flow process is simple, the advantage of stable operation.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of method removing alkyl nitrite and nitrogen oxide in tail gas, comprises the following steps:
A) industrial tail gas containing reducibility gas is sent in deep freezer, uses chilled water that tail gas is being cooled to less than 10 degree;
B) send in absorption tower through cooled tail gas, use the alkyl nitrite in alkylol absorption tail gas, obtain the alkyl alcohol solution containing alkyl nitrite; The operating temperature on described absorption tower is-40 ~ 80 DEG C, and operating pressure is 0.1 ~ 20MPa;
C) the gas phase discharging of absorption tower tower top is sent in catalytic reduction reactor, and unabsorbed alkyl nitrite and nitrogen oxide react with the reducibility gas that carries in industrial tail gas and generate nitrogen under catalyst action.
In technique scheme, the reducibility gas carried in industrial tail gas is selected from least one in carbon monoxide or hydrogen; In step a), the chilling temperature of deep freezer is preferably 0 ~ 10 DEG C; In step b), the mol ratio of alkylol and alkyl nitrite is preferably 2:1 ~ 10:1; In step b), the operating temperature of tail gas absorber is preferably-30 ~ 10 DEG C, and operating pressure is preferably 0.4 ~ 4.0MPa; Tail gas absorber in step b) is preferably selected from packed tower or plate column; Alkylol in step b) is preferably selected from least one in methyl alcohol, ethanol or butanols; In step c), the temperature of catalytic reduction reactor is preferably 100 ~ 300 DEG C, and pressure is preferably 0.1 ~ 0.5MPa; Catalyst in step c) in catalytic reduction reactor is preferably load type palladium catalyst, and carrier is aluminium oxide, and palladium content is 0.001 ~ 1.5%.
In technical scheme of the present invention, first utilize chilled water cooled exhaust gas, reclaim alkyl nitrite wherein, reduce the content of alkyl nitrite in tail gas, also reduce the load on absorption tower and the consumption of alkylol thereof; After two steps reclaim alkyl nitrite, substantially not containing alkyl nitrite in tail gas, also reduce further catalytic reduction reactor load; Adopt load type palladium catalyst, the reducibility gas carbon monoxide or hydrogen that carry in industrial tail gas can be utilized, under relatively low reaction temperature, nitrogen oxide in tail gas is removed to below 200ppm, meets environmental requirement, catalyst not easily coking, inactivation, can keep long-period stable operation.
Adopt technical scheme of the present invention, in tail gas, the concentration of alkyl nitrite and nitrogen oxide can be down to 0ppm, meets environmental requirement, and due to catalytic reduction operating temperature lower, catalyst stabilization, achieves good technique effect.
Accompanying drawing explanation
Fig. 1 is the process chart that the present invention removes alkyl nitrite and nitrogen oxide in tail gas.
In Fig. 1,1 is deep freezer, 2 is absorption tower, 3 is catalytic reduction reactor, and 4 is the industrial tail gas containing alkyl nitrite, nitrogen oxide and reducibility gas, and 5 is alkyl nitrite, 6 is alkylol, 7 is the alkyl alcohol solution containing alkyl nitrite, and 8 is the industrial tail gas after being separated alkyl nitrite, and 9 is qualified discharge gas.
Below by embodiment, the invention will be further elaborated, but these embodiments are in no case construed as limiting scope of the present invention.
Detailed description of the invention
[embodiment 1]
As shown in Figure 1, the industrial tail gas 4 containing alkyl nitrite and nitrogen oxide is sent into deep freezer 1, reclaim alkyl nitrite 5 wherein by condensing cooling.The discharge gas logistics be not condensed is sent in absorption tower 2, absorbs the alkyl nitrite in discharge gas, reclaim the alkyl alcohol solution 7 obtaining alkyl nitrite with alkylol 6.The tail gas 8 be separated after alkyl nitrite is admitted in catalytic reduction reactor 3, the reducibility gas that oxides of nitrogen gas and unabsorbed alkyl nitrite carry with tail gas itself under the effect of catalyst reacts and generates nitrogen, and industrial tail gas is converted into qualified discharge gas 9.
By flow chart 1, will containing carbon monoxide 15% (volume), the synthesizing dimethyl oxalate tail gas 0.1Nm of nitrogen oxide 1% (volume) and methyl nitrite 10% (volume)
3/ hr, deep freezer temperature is 0 DEG C, and tail gas absorption column overhead adds-40 DEG C of methanol solution 250ml/hr, operating pressure 3.0MPa, and the mol ratio of alkylol and alkyl nitrite is 2:1, and packed tower is selected on absorption tower.Catalytic reduction reactor controls 300 DEG C, and operating pressure 0.5MPa, selects load type palladium catalyst, and carrier is aluminium oxide, and palladium content is 0.5%, gas hourly space velocity (GHSV) 35000hr
-1, reacted gas is through gas chromatographic analysis: carbon monoxide 13% (volume), 0.0% (volume) of nitrogen oxide, methyl nitrite 0.0% (volume).
[embodiment 2]
As shown in Figure 1, the industrial tail gas 4 containing alkyl nitrite and nitrogen oxide is sent into deep freezer 1, reclaim alkyl nitrite 5 wherein by condensing cooling.The discharge gas logistics be not condensed is sent in absorption tower 2, absorbs the alkyl nitrite in discharge gas, reclaim the alkyl alcohol solution 7 obtaining alkyl nitrite with alkylol 6.The tail gas 8 be separated after alkyl nitrite is admitted in catalytic reduction reactor 3, the reducibility gas that oxides of nitrogen gas and unabsorbed alkyl nitrite carry with tail gas itself under the effect of catalyst reacts and generates nitrogen, and industrial tail gas is converted into qualified discharge gas 9.
By the carbon monoxide 13% (volume) contained, the synthesis of diethyl oxalate employing tail gas 0.2Nm of nitrogen oxide 0.8% (volume) and nitrous ether (ethyl nitrite) 12% (volume)
3/ hr, deep freezer temperature is 2 DEG C, and tail gas absorption column overhead adds-20 DEG C of ethanol 350ml/hr, operating pressure 1.0MPa, and the mol ratio of alkylol and alkyl nitrite is 2:1, and packed tower is selected on absorption tower.Catalytic reduction reactor controls 300 DEG C, and operating pressure 0.3MPa, selects load type palladium catalyst, and carrier is aluminium oxide, and palladium content is 0.8%, gas hourly space velocity (GHSV) 35000hr
-1, reacted gas is through gas chromatographic analysis: carbon monoxide 11.6% (volume), 0.0% (volume) of nitrogen oxide, nitrous ether (ethyl nitrite) 0.0% (volume).
[embodiment 3]
As shown in Figure 1, the industrial tail gas 4 containing alkyl nitrite and nitrogen oxide is sent into deep freezer 1, reclaim alkyl nitrite 5 wherein by condensing cooling.The discharge gas logistics be not condensed is sent in absorption tower 2, absorbs the alkyl nitrite in discharge gas, reclaim the alkyl alcohol solution 7 obtaining alkyl nitrite with alkylol 6.The tail gas 8 be separated after alkyl nitrite is admitted in catalytic reduction reactor 3, the reducibility gas that oxides of nitrogen gas and unabsorbed alkyl nitrite carry with tail gas itself under the effect of catalyst reacts and generates nitrogen, and industrial tail gas is converted into qualified discharge gas 9.
By the hydrogen 8% (volume) contained, the synthesis of diethyl oxalate employing tail gas 0.3Nm of nitrogen oxide 1.5% (volume) and nitrous ether (ethyl nitrite) 14% (volume)
3/ hr, deep freezer temperature is 5 DEG C, and tail gas absorption column overhead adds 6 DEG C of ethanol 400ml/hr, operating pressure 0.5MPa, and the mol ratio of alkylol and alkyl nitrite is 5:1, and packed tower is selected on absorption tower.Catalytic reduction reactor controls 200 DEG C, and operating pressure 0.2MPa, selects load type palladium catalyst, and carrier is aluminium oxide, and palladium content is 1.5%, gas hourly space velocity (GHSV) 40000hr
-1, reacted gas is through gas chromatographic analysis: carbon monoxide 5.8% (volume), 0.0% (volume) of nitrogen oxide, nitrous ether (ethyl nitrite) 0.0% (volume).
[embodiment 4]
As shown in Figure 1, the industrial tail gas 4 containing alkyl nitrite and nitrogen oxide is sent into deep freezer 1, reclaim alkyl nitrite 5 wherein by condensing cooling.The discharge gas logistics be not condensed is sent in absorption tower 2, absorbs the alkyl nitrite in discharge gas, reclaim the alkyl alcohol solution 7 obtaining alkyl nitrite with alkylol 6.The tail gas 8 be separated after alkyl nitrite is admitted in catalytic reduction reactor 3, the reducibility gas that oxides of nitrogen gas and unabsorbed alkyl nitrite carry with tail gas itself under the effect of catalyst reacts and generates nitrogen, and industrial tail gas is converted into qualified discharge gas 9.
By the carbon monoxide 12% (volume) contained, the synthesis of oxalic acid dibutyl ester tail gas 0.3Nm of nitrogen oxide 1.2% (volume) and butyl nitrite 10% (volume)
3/ hr, deep freezer temperature is 10 DEG C, and tail gas absorption column overhead adds 80 DEG C of butanols liquid 400ml/hr, operating pressure 4.0MPa, and the mol ratio of alkylol and alkyl nitrite is 8:1, and plate column is selected on absorption tower.Catalytic reduction reactor controls 100 DEG C, and operating pressure 0.4MPa, selects load type palladium catalyst, and carrier is aluminium oxide, and palladium content is 1.2%, gas hourly space velocity (GHSV) 35000hr
-1, reacted gas is through gas chromatographic analysis: carbon monoxide 10.1% (volume), 0.0% (volume) of nitrogen oxide, butyl nitrite 0.001% (volume).
[embodiment 5]
As shown in Figure 1, the industrial tail gas 4 containing alkyl nitrite and nitrogen oxide is sent into deep freezer 1, reclaim alkyl nitrite 5 wherein by condensing cooling.The discharge gas logistics be not condensed is sent in absorption tower 2, absorbs the alkyl nitrite in discharge gas, reclaim the alkyl alcohol solution 7 obtaining alkyl nitrite with alkylol 6.The tail gas 8 be separated after alkyl nitrite is admitted in catalytic reduction reactor 3, the reducibility gas that oxides of nitrogen gas and unabsorbed alkyl nitrite carry with tail gas itself under the effect of catalyst reacts and generates nitrogen, and industrial tail gas is converted into qualified discharge gas 9.
Will containing carbon monoxide 15% (volume), the synthesizing dimethyl oxalate tail gas 0.1Nm of nitrogen oxide 1% (volume) and methyl nitrite 10% (volume)
3/ hr, deep freezer temperature is 8 DEG C, and tail gas absorption column overhead adds 10 DEG C of methanol solution 200ml/hr, operating pressure 2.0MPa, and the mol ratio of alkylol and alkyl nitrite is 10:1, and packed tower is selected on absorption tower.Catalytic reduction reactor controls 150 DEG C, and operating pressure 0.1MPa, selects load type palladium catalyst, and carrier is aluminium oxide, and palladium content is 0.1%, gas hourly space velocity (GHSV) 40000hr
-1, reacted gas is through gas chromatographic analysis: carbon monoxide 13.0% (volume), 0.001% (volume) of nitrogen oxide, methyl nitrite 0.002% (volume).
[comparative example 1]
The nitrogen oxide in tail gas is removed with method identical in embodiment 1, but it is 100 DEG C that the temperature of catalytic reduction reactor controls, reacted gas is through gas chromatographic analysis: carbon monoxide 14% (volume), 0.1% (volume) of nitrogen oxide, methyl nitrite 0.2% (volume), can not meet the requirement of environmental protection.
[comparative example 2]
The nitrogen oxide in tail gas is removed with method identical in embodiment 1, but it is 400 DEG C that the temperature of catalytic reduction reactor controls, reacted gas is through gas chromatographic analysis: carbon monoxide 13% (volume), 0% (volume) of nitrogen oxide, methyl nitrite 0% (volume).Too high reaction temperature makes the life-span of catalyst by original >1, shortens to 2 months, affects the long period of whole device, stable operation.
Claims (10)
1. remove a method for alkyl nitrite and nitrogen oxide in tail gas, comprise the following steps:
A) industrial tail gas containing reducibility gas is sent in deep freezer, uses chilled water that tail gas is being cooled to less than 10 degree;
B) send in absorption tower through cooled tail gas, use the alkyl nitrite in alkylol absorption tail gas, obtain the alkyl alcohol solution containing alkyl nitrite; The operating temperature on described absorption tower is-40 ~ 80 DEG C, and operating pressure is 0.1 ~ 20MPa;
C) the gas phase discharging of absorption tower tower top is sent in catalytic reduction reactor, and unabsorbed alkyl nitrite and nitrogen oxide react with the reducibility gas that carries in industrial tail gas and generate nitrogen under catalyst action.
2. the method removing alkyl nitrite and nitrogen oxide in tail gas according to claim 1, is characterized in that the reducibility gas carried in industrial tail gas is selected from least one in carbon monoxide or hydrogen.
3. the method removing alkyl nitrite and nitrogen oxide in tail gas according to claim 1, is characterized in that the chilling temperature of deep freezer in step a) is 0 ~ 10 DEG C.
4. the method removing alkyl nitrite and nitrogen oxide in tail gas according to claim 1, is characterized in that the mol ratio of alkylol and alkyl nitrite in step b) is 2:1 ~ 10:1.
5. the method removing alkyl nitrite and nitrogen oxide in tail gas according to claim 1, it is characterized in that in step b), the operating temperature of tail gas absorber is-30 ~ 10 DEG C, operating pressure is 0.4 ~ 4.0MPa.
6. the method removing alkyl nitrite and nitrogen oxide in tail gas according to claim 1, is characterized in that the tail gas absorber in step b) is selected from packed tower or plate column.
7. the method removing alkyl nitrite and nitrogen oxide in tail gas according to claim 1, the alkylol that it is characterized in that in step b) is selected from least one in methyl alcohol, ethanol or butanols.
8. the method removing alkyl nitrite and nitrogen oxide in tail gas according to claim 1, is characterized in that the temperature of catalytic reduction reactor in step c) is 100 ~ 300 DEG C.
9. the method removing alkyl nitrite and nitrogen oxide in tail gas according to claim 1, is characterized in that the pressure of catalytic reduction reactor in step c) is 0.1 ~ 0.5MPa.
10. the method removing alkyl nitrite and nitrogen oxide in tail gas according to claim 1, it is characterized in that the catalyst in step c) in catalytic reduction reactor is load type palladium catalyst, carrier is aluminium oxide, and palladium content is 0.001 ~ 1.5%.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106139898A (en) * | 2015-04-14 | 2016-11-23 | 高化学株式会社 | The method of the NO in regeneration, absorption and removing CO carbonyl coupling synthesis of oxalate process tail gas, alkyl nitrite and CO and N2O |
| CN106268226A (en) * | 2015-06-12 | 2017-01-04 | 中国石油化工股份有限公司 | Containing NO in coal ethyl glycol commercial productionxthe processing method of tail gas |
| CN106268227A (en) * | 2015-06-12 | 2017-01-04 | 中国石油化工股份有限公司 | Containing NO in coal ethyl glycol commercial productionxthe processing means of tail gas |
| CN109107345A (en) * | 2018-09-17 | 2019-01-01 | 河南新邦化工技术有限公司 | CO is coupled synthesis of oxalate technique discharge gas and its treating tail gas technique and system |
| CN109796345A (en) * | 2019-01-30 | 2019-05-24 | 青岛科技大学 | A kind of tail gas method of comprehensive utilization of nitrite displacement method production nitromethane |
| CN111408238A (en) * | 2020-03-18 | 2020-07-14 | 中国神华煤制油化工有限公司 | Material recycling device and method for preparing ethylene glycol from synthesis gas |
| CN112973406A (en) * | 2019-12-13 | 2021-06-18 | 湖北富博化工有限责任公司 | Resource utilization and treatment method for nitromethane waste gas |
| CN114602311A (en) * | 2020-12-08 | 2022-06-10 | 湖北远大富驰医药化工股份有限公司 | Method for circularly preparing nitromethane |
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Cited By (12)
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|---|---|---|---|---|
| CN106139898A (en) * | 2015-04-14 | 2016-11-23 | 高化学株式会社 | The method of the NO in regeneration, absorption and removing CO carbonyl coupling synthesis of oxalate process tail gas, alkyl nitrite and CO and N2O |
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| CN106268226A (en) * | 2015-06-12 | 2017-01-04 | 中国石油化工股份有限公司 | Containing NO in coal ethyl glycol commercial productionxthe processing method of tail gas |
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| CN109796345B (en) * | 2019-01-30 | 2022-02-22 | 青岛科技大学 | Comprehensive utilization method of tail gas generated in nitromethane production by nitrite displacement method |
| CN112973406A (en) * | 2019-12-13 | 2021-06-18 | 湖北富博化工有限责任公司 | Resource utilization and treatment method for nitromethane waste gas |
| CN112973406B (en) * | 2019-12-13 | 2022-10-21 | 湖北富博化工有限责任公司 | Resource utilization and treatment method for nitromethane waste gas |
| CN111408238A (en) * | 2020-03-18 | 2020-07-14 | 中国神华煤制油化工有限公司 | Material recycling device and method for preparing ethylene glycol from synthesis gas |
| CN114602311A (en) * | 2020-12-08 | 2022-06-10 | 湖北远大富驰医药化工股份有限公司 | Method for circularly preparing nitromethane |
| CN114602311B (en) * | 2020-12-08 | 2023-11-07 | 湖北远大富驰医药化工股份有限公司 | Method for circularly preparing nitromethane |
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Application publication date: 20150325 |