CN105617837A - Treatment system and treatment method of acid waste gas in caprolactam production process - Google Patents
Treatment system and treatment method of acid waste gas in caprolactam production process Download PDFInfo
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- CN105617837A CN105617837A CN201410608366.7A CN201410608366A CN105617837A CN 105617837 A CN105617837 A CN 105617837A CN 201410608366 A CN201410608366 A CN 201410608366A CN 105617837 A CN105617837 A CN 105617837A
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- waste gas
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Abstract
The invention provides a treatment system of acid waste gas in caprolactam production process. The treatment system comprises an acid waste gas collecting tank used for collecting acid waste gas in caprolactam production process, a pressure reducing valve which is arranged on the top of the acid waste gas collecting tank and is used for maintaining the pressure in the acid waste gas collecting tank to be 30.0kPa or lower, and a scrubber tower which is communicated with the acid waste gas collecting tank, and is used for realizing reaction of the acid waste gas delivered into the scrubber tower with an alkali liquor and generating a solution containing SO4<2->. The invention also provides a treatment method of acid waste gas in caprolactam production process. The treatment system and treatment method of acid waste gas in caprolactam production process are capable of realizing reaction of the acid waste gas in caprolactam production process with the alkali liquor, generating a solution containing SO4<2->, preventing direct volatilization of the acid waste gas into the air and environmental pollution, and avoiding influences on health.
Description
Technical field
The present invention relates to chemical field, particularly relate to process device and the processing method of acid waste gas in preparing process of caprolactam.
Background technology
Sulfur trioxide is a kind of sulfur oxide, and molecular formula is SO3, have the abnormal smells from the patient of similar sulfur dioxide, be dissolved in water, react generation sulphuric acid with water. The gas form of sulfur trioxide is a kind of serious pollutant, is one of main source forming acid rain. The performance of its toxicity is same with sulfuric acid phase, and the tissue such as skin, mucosa is had strong impulse and corrosiveness. Conjunctivitis, edema can be caused; The corneal opacity, thus blind; Respiratory tract symptom, severe one generation dyspnea and pulmonary edema can also be caused; High concentration causes laryngospasm or glottic edema to die. Gastral burn is caused so that ulcer after oral. Severe patient is likely to have gastric perforation, peritonitis, laryngospasm and glottic edema, renal damage, shock etc. Chronic Effect has dental erosion, chronic bronchitis, emphysema and hepatitis interstitialis chronica etc. Environment there is is harm, air can be polluted.
Beckmann molecular rearrangement reaction is an important step in caprolactam production process, and its detailed process is as follows:
Cyclohexanone-oxime containing 10% SO3Oleum exist under, there is Beckmann molecular rearrangement reaction, form caprolactam sulfuric acid solution, and release big calorimetric. Primary response formula is as follows:
��
Above-mentioned reaction is undertaken in two steps:
The first step: cyclohexanone-oxime and nicotinic acid (oleum) react generation cyclohexanone-oxime sulfuric ester, and its reaction equation is as follows:
;
Second step: Beckmann rearrangement occurs cyclohexanone-oxime sulfuric ester under nicotinic acid effect, generates caprolactam, and its reaction equation is as follows:
��
In above-mentioned course of reaction, the raw material cyclohexanone-oxime come from upstream device divides three grades to enter rearrangement reactors, and another kind of raw material is containing 20%(wt) SO3Oleum first order pump inlet add, for ensure cyclohexanone-oxime fully react, containing 20%(wt) SO3Oleum need excessive, both mix mutually by certain proportioning, and rearrangement reaction carries out in rearrangement reactor, generate caprolactam sulfuric ester. Caprolactam sulfuric ester and the complete a small amount of oleum of unreacted enter surge tank. For guaranteeing equipment safety, surge tank need to uncovered can not seal. A small amount of SO that in surge tank, unreacted is complete3Evaporate in air from top manhole, formed " acid mist ", cause environmental pollution, have a strong impact on the physical and mental health of people.
In traditional production technology, the process system and method for acid waste gas mainly has following two:
The first acid waste gas processing unit, including two grades of packed towers, acid waste gas import it is provided with at the bottom of tower, tower top is provided with flue and Waste gas outlet, is externally provided with the first washing absorption mechanism, the second washing absorption mechanism, clear water atomization washing mechanism, gas-liquid separation mechanism and on-line checking mechanism in tower body. Clear water atomization washing mechanism is arranged on the top of the first washing absorption mechanism, and gas-liquid separation mechanism is arranged in flue, and on-line checking mechanism is also connected on the inlet pipeline of the second washing absorption mechanism. This device adopts clear water to wash, and need to set up and overlap washing facility more, the process not being suitable in preparing process of caprolactam acid waste gas.
The second acid waste gas processing unit, adopt alkali liquor configuration and distribution system that the alkali liquor prepared is assigned in dedusting alkali liquor circulation absorption system, one-level alkali liquor circulation absorption system and two grades of alkali liquor circulation absorption systems, alkali liquor circulation in said system adopts the closed loop fluid path sprayed from top to bottom, alkali liquor can be sent into devil liquor recovery and process system, processes waste gas and adopts open loop gas circuit from bottom to top. Processing technique to adopt and allow process waste gas enter top from the bottom of dedusting absorption tower, one-level Alkali absorption tower and two grades of Alkali absorption towers and go out, alkali liquor sprays from top to bottom simultaneously. In ozone reactor, ozone makes the oxidation of nitric oxide in process waste gas become nitrogen dioxide, and last process waste gas up to standard is discharged from the floss hole on two grades of Alkali absorption tower tops. This device is mainly used in the process of nitrogen-containing oxide acid waste gas, need to set up multiple alkali liquor absorption tank, and acid waste gas also through spray drying treatment, not to be suitable in preparing process of caprolactam the process of acid waste gas equally.
In sum, process system and the processing method of finding a kind of acid waste gas suitable in preparing process of caprolactam are most important.
Summary of the invention
Based on this, it is necessary to in traditional production technology, the device and method that processes of acid waste gas is not all suitable in preparing process of caprolactam the process of acid waste gas, it is provided that the process system of acid waste gas in a kind of preparing process of caprolactam.
Additionally, the present invention also provides for the processing method of acid waste gas in a kind of preparing process of caprolactam.
The process system of acid waste gas in a kind of preparing process of caprolactam, including:
Acid waste gas houses tank, for housing the acid waste gas in preparing process of caprolactam;
It is arranged on described acid waste gas and houses the air relief valve of tank top, for the pressure that described acid waste gas houses in tank is maintained��30.0kPa; And
House, with described acid waste gas, the aeration tower that tank connects, for acid waste gas and the alkaline reaction of aeration tower will be passed into, generate containing SO4 2-Solution.
Wherein in an embodiment, in described aeration tower, it is provided with micro-spray device, for described alkali liquor being atomized into small drop, and to passing into the spent acidic gas blowout alkali liquor of aeration tower.
Wherein in an embodiment, described acid waste gas house tank top pass sequentially through be flexible coupling, pipeline connect be connected with the bottom of described aeration tower.
Wherein in an embodiment, the alkali liquor that in described preparing process of caprolactam, the process system of acid waste gas also includes connecting with described aeration tower houses tank, and described alkali liquor houses tank for housing the alkali liquor reacted with described acid waste gas.
Wherein in an embodiment, the bottom of described aeration tower passes sequentially through pipeline pump, the first rotor effusion meter houses tank with described alkali liquor and is connected; Tank passes sequentially through discharging pump to the collecting of described alkali liquor, the second spinner flowmeter is connected with described micro-spray device.
Wherein in an embodiment, the top of described aeration tower is provided with tail gas discharging pipe, for discharging the gas not absorbed by alkali liquor.
Wherein in an embodiment, the top of described aeration tower is provided with relief valve, is used for preventing aeration tower from building the pressure.
The processing method of acid waste gas in a kind of preparing process of caprolactam, comprises the following steps:
At below 30kPa, house the acid waste gas in preparing process of caprolactam; And
By described acid waste gas and alkaline reaction, generate containing SO4 2-Solution.
Wherein in an embodiment, described alkali liquor is sodium hydroxide solution, and the mass concentration of described alkali liquor is 0.05% ~ 5%, and pH value is 7.01 ~ 14.
Wherein in an embodiment, the flow of described alkali liquor is 0 ~ 10.0m3/hr��
The process system and method for acid waste gas in above-mentioned preparing process of caprolactam, by the acid waste gas in preparing process of caprolactam and alkaline reaction, generates containing SO4 2-Solution, it is prevented that acid waste gas directly evaporates in air, and contaminated environment is unhealthful.
Accompanying drawing explanation
Fig. 1 be an embodiment preparing process of caprolactam in the structural representation of process system of acid waste gas.
Fig. 2 be an embodiment preparing process of caprolactam in the process flow schematic diagram of acid waste gas.
Detailed description of the invention
Understandable for enabling the above-mentioned purpose of the present invention, feature and advantage to become apparent from, below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in detail. Elaborate a lot of detail in the following description so that fully understanding the present invention. But the present invention can implement being much different from alternate manner described here, and those skilled in the art can do similar improvement when without prejudice to intension of the present invention, therefore the present invention is by the following public restriction being embodied as.
Refer to Fig. 1, the process system of acid waste gas in the preparing process of caprolactam of an embodiment, house tank 10 including acid waste gas, be arranged on acid waste gas and house the air relief valve 20 at tank 10 top, house, with acid waste gas, the aeration tower 30 that tank 10 connects.
Wherein, in acid waste gas collecting tank 10 i.e. preparing process of caprolactam, rearrangement buffering flow container is gentle rushes tank overflow pipe.
Acid waste gas houses tank 10, and for housing the acid waste gas in preparing process of caprolactam, namely this acid waste gas comprises from the sour gas reset in the sour gas and surge tank overflow pipe that volatilize buffering flow container.
Air relief valve 20, for by acid waste gas, the pressure housed in tank 10 maintains��30.0kPa.
Preferably, air relief valve 20 is nitrogen air relief valve.
Aeration tower 30, for passing into acid waste gas and the alkaline reaction of aeration tower 30, generates containing SO4 2-Solution.
In the present embodiment, acid waste gas house the top of tank 10 pass sequentially through be flexible coupling, pipeline connects and is connected with the bottom of aeration tower 30, the acid waste gas that acid waste gas houses in tank 10 collecting passes into the bottom of aeration tower 30.
Wherein, acid waste gas houses the top employing of tank 10 and is flexible coupling, and is to prevent acid waste gas collecting tank 10 from building the pressure, and makes its bearing capacity control at��50.0kPa.
Preferably, it is flexible coupling for metallic film.
Preferably, in aeration tower 30, it is provided with micro-spray device 32, for alkali liquor being atomized into small drop, and to passing into the spent acidic gas blowout alkali liquor of aeration tower 30.
In the present embodiment, the alkali liquor that in preparing process of caprolactam, the process system of acid waste gas also includes connecting with aeration tower 30 houses tank 40, and this alkali liquor houses tank for housing the alkali liquor reacted with acid waste gas.
Wherein, alkali liquor houses the oximes alkaline waste water storage tank in tank 40 i.e. preparing process of caprolactam.
Preferably, the bottom of aeration tower 30 passes sequentially through pipeline pump 42, the first rotor effusion meter 44 houses tank 40 with alkali liquor and is connected.
Alkali liquor collecting tank 40 passes sequentially through discharging pump the 46, second spinner flowmeter 48 and is connected with micro-spray device 32.
Concrete, the alkali liquor that alkali liquor houses in tank 40 introduces in aeration tower 30 under the effect of discharging pump 46, is reacted by micro-spray device 32 and the acid waste gas passing into aeration tower 30, generates containing SO4 2-Solution, under gravity, collect in the bottom of aeration tower 30, then again under the effect of pipeline pump 42, be back to alkali liquor and house in tank 40, alkali liquor forms closed loop balance, it is achieved recycle.
It is pointed out that micro-spray device 32 can omit, now can also directly alkali liquor be passed in aeration tower 30, from top drench, make alkali liquor with pass into aeration tower 30 acid waste gas react.
In the present embodiment, the top of aeration tower 30 is provided with tail gas discharging pipe 34, for discharging the gas not absorbed by alkali liquor.
Such as, what air relief valve 20 adopted is nitrogen air relief valve, then acid waste gas houses in tank 10 possibly together with nitrogen, and now nitrogen is not absorbed by alkali liquor, it is possible to discharged by tail gas discharging pipe 34, it is prevented that build the pressure.
In the present embodiment, the top of aeration tower 30 is additionally provided with relief valve 36, it is prevented that aeration tower 30 builds the pressure, cause reaction generate containing SO4 2-Solution and anti-the filling to acid waste gas of the complete alkali liquor of unreacted house in tank 10.
It is appreciated that to ensure equipment safety, tail gas discharging pipe 34 is provided with the 3rd effusion meter 342, for controlling not discharge by the gas of alkali liquor absorption; Acid waste gas houses the gas introduction tube (being connected with pipeline) of tank 10 equipped with pressure transmitter (not shown), and the uninterrupted of the second spinner flowmeter 48 is determined according to the pressure size of this pressure transmitter.
Preferably, it is additionally provided with repid cut-off valve 482 between the second spinner flowmeter 48 and micro-spray device 32, passes into the alkali liquor in aeration tower 30 for fast shut-off.
The process system of acid waste gas in above-mentioned preparing process of caprolactam, acid waste gas is housed the sour gas volatilized in tank 10 pass sequentially through be flexible coupling, pipeline connects and passes into the bottom of aeration tower 30, and the alkaline reaction in aeration tower 30, generate containing SO4 2-Solution, it is prevented that acid waste gas directly evaporates in air, and contaminated environment is unhealthful.
Additionally, alkali liquor introduces in aeration tower 30 under the effect of material pump 46, reacted by micro-spray device 32 and the acid waste gas passing into aeration tower 30, generate containing SO4 2-Solution, under gravity, collect in the bottom of aeration tower 30, then again under the effect of pipeline pump 42, be back to alkali liquor and house in tank 40, alkali liquor forms closed loop balance, it is achieved recycle.
Fig. 2 be an embodiment preparing process of caprolactam in the processing method of acid waste gas, comprise the following steps:
S210, at below 30kPa, house the acid waste gas in preparing process of caprolactam.
In present embodiment, adopt and house tank top installation air relief valve at acid waste gas so that the pressure that acid waste gas houses in tank maintains below 30kPa.
Wherein, acid waste gas houses and resets in tank and preparing process of caprolactam that buffering flow container is gentle rushes tank overflow pipe.
Acid waste gas is namely containing from resetting the sour gas cushioned in the sour gas and surge tank overflow pipe volatilized in flow container.
SO in acid waste gas3Content is at 10mg/L ~ 100mg/L.
S220, by acid waste gas and alkaline reaction, generate containing SO4 2-Solution.
In the present embodiment, alkali liquor is sodium hydroxide solution. Preferably, the mass concentration of alkali liquor is 0.05% ~ 5%, and pH value is 7.01 ~ 14.
In the present embodiment, acid waste gas and alkali liquor react in aeration tower, generate containing SO4 2-Solution.
Preferably, acid waste gas is 10 DEG C ~ 50 DEG C with the reaction temperature of alkali liquor.
In order to make alkali liquor fully absorb acid waste gas, micro-spray device is set in aeration tower, alkali liquor is atomized into small drop, and to passing into the spent acidic gas blowout alkali liquor of aeration tower.
Preferably, the flow of alkali liquor is 0 ~ 10.0m3/hr��
Being appreciated that in preparing process of caprolactam, above-mentioned alkali liquor is oximes operation waste water.
Concrete, alkali liquor is contained in alkali liquor and houses in tank. In preparing process of caprolactam, alkali liquor houses tank and oximes alkaline waste water storage tank.
The alkali liquor that alkali liquor houses in tank introduces in aeration tower under the effect of discharging pump, is reacted by micro-spray device and the acid waste gas passing into aeration tower, generates containing SO4 2-Solution, under gravity, collect in the bottom of aeration tower, then again under the effect of pipeline pump, be back to alkali liquor and house in tank, alkali liquor forms closed loop balance, it is achieved recycle.
In above-mentioned preparing process of caprolactam, the processing method of acid waste gas is simple, quick, by the acid waste gas in preparing process of caprolactam and alkaline reaction, generates containing SO4 2-Solution, after testing, SO in the gas after process3Concentration be 0mg/L.
It it is below specific embodiment.
Embodiment 1
At below 30kPa, house the acid waste gas in preparing process of caprolactam, SO in acid waste gas3Content be 10mg/L. Being the alkaline reaction of 0.05% at 10 DEG C by acid waste gas and mass concentration, the flow of alkali liquor is 2000L/hr. After testing, SO in the gas after process3Concentration be 0mg/L.
Embodiment 2
At below 30kPa, house the acid waste gas in preparing process of caprolactam, SO in acid waste gas3Content be 100mg/L. Being the alkaline reaction of 5% at 50 DEG C by acid waste gas and mass concentration, the flow of alkali liquor is 10000L/hr. After testing, SO in the gas after process3Concentration be 0mg/L.
Embodiment 3
At below 30kPa, house the acid waste gas in preparing process of caprolactam, SO in acid waste gas3Content be 50mg/L. Being the alkaline reaction of 3.0% at 30 DEG C by acid waste gas and mass concentration, the flow of alkali liquor is 5000L/hr. After testing, SO in the gas after process3Concentration be 0mg/L.
Embodiment described above only have expressed the several embodiments of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention. It should be pointed out that, for the person of ordinary skill of the art, without departing from the inventive concept of the premise, it is also possible to making some deformation and improvement, these broadly fall into protection scope of the present invention. Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. the process system of acid waste gas in a preparing process of caprolactam, it is characterised in that including:
Acid waste gas houses tank, for housing the acid waste gas in preparing process of caprolactam;
It is arranged on described acid waste gas and houses the air relief valve of tank top, for the pressure that described acid waste gas houses in tank is maintained��30.0kPa; And
House, with described acid waste gas, the aeration tower that tank connects, for acid waste gas and the alkaline reaction of aeration tower will be passed into, generate containing SO4 2-Solution.
2. the process system of acid waste gas in preparing process of caprolactam according to claim 1, it is characterised in that be provided with micro-spray device in described aeration tower, for being atomized into small drop, and to passing into the spent acidic gas blowout alkali liquor of aeration tower by described alkali liquor.
3. the process system of acid waste gas in preparing process of caprolactam according to claim 1, it is characterised in that described acid waste gas house tank top pass sequentially through be flexible coupling, pipeline connect be connected with the bottom of described aeration tower.
4. the process system of acid waste gas in preparing process of caprolactam according to claim 2, it is characterized in that, the alkali liquor that in described preparing process of caprolactam, the process system of acid waste gas also includes connecting with described aeration tower houses tank, and described alkali liquor houses tank for housing the alkali liquor reacted with described acid waste gas.
5. the process system of acid waste gas in preparing process of caprolactam according to claim 4, it is characterised in that the bottom of described aeration tower passes sequentially through pipeline pump, the first rotor effusion meter houses tank with described alkali liquor and is connected; Tank passes sequentially through discharging pump to the collecting of described alkali liquor, the second spinner flowmeter is connected with described micro-spray device.
6. the process system of acid waste gas in preparing process of caprolactam according to claim 1, it is characterised in that the top of described aeration tower is provided with tail gas discharging pipe, for discharging the gas not absorbed by alkali liquor.
7. the process system of acid waste gas in preparing process of caprolactam according to claim 1, it is characterised in that the top of described aeration tower is provided with relief valve, is used for preventing aeration tower from building the pressure.
8. the processing method of acid waste gas in a preparing process of caprolactam, it is characterised in that comprise the following steps:
At below 30kPa, house the acid waste gas in preparing process of caprolactam; And
By described acid waste gas and alkaline reaction, generate containing SO4 2-Solution.
9. the processing method of acid waste gas in preparing process of caprolactam according to claim 8, it is characterised in that described alkali liquor is sodium hydroxide solution, and the mass concentration of described alkali liquor is 0.05% ~ 5%, and pH value is 7.01 ~ 14.
10. the processing method of acid waste gas in preparing process of caprolactam according to claim 8, it is characterised in that the flow of described alkali liquor is 0 ~ 10.0m3/hr��
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| CN201410608366.7A CN105617837A (en) | 2014-11-04 | 2014-11-04 | Treatment system and treatment method of acid waste gas in caprolactam production process |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090226364A1 (en) * | 2008-03-07 | 2009-09-10 | E. I. Du Pont De Nemours And Company | Process for treating acid gas in staged furnaces with inter-stage heat recovery and inter-stage sulfur production |
| CN202876580U (en) * | 2012-09-28 | 2013-04-17 | 长乐力恒锦纶科技有限公司 | Caprolactam exhaust gas/dust recovery system |
| CN103463936A (en) * | 2013-09-07 | 2013-12-25 | 中北大学 | Device and method for removing sulfur dioxide contained in waste gas |
| CN103768918A (en) * | 2012-10-26 | 2014-05-07 | 中国石油化工股份有限公司 | Purification method and device for tail gas of caprolactam device |
-
2014
- 2014-11-04 CN CN201410608366.7A patent/CN105617837A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090226364A1 (en) * | 2008-03-07 | 2009-09-10 | E. I. Du Pont De Nemours And Company | Process for treating acid gas in staged furnaces with inter-stage heat recovery and inter-stage sulfur production |
| CN202876580U (en) * | 2012-09-28 | 2013-04-17 | 长乐力恒锦纶科技有限公司 | Caprolactam exhaust gas/dust recovery system |
| CN103768918A (en) * | 2012-10-26 | 2014-05-07 | 中国石油化工股份有限公司 | Purification method and device for tail gas of caprolactam device |
| CN103463936A (en) * | 2013-09-07 | 2013-12-25 | 中北大学 | Device and method for removing sulfur dioxide contained in waste gas |
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Application publication date: 20160601 |