CN100386270C - Method for processing kettle-liquid of acrylonitrile quench tower lower portion - Google Patents
Method for processing kettle-liquid of acrylonitrile quench tower lower portion Download PDFInfo
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- CN100386270C CN100386270C CNB200610046845XA CN200610046845A CN100386270C CN 100386270 C CN100386270 C CN 100386270C CN B200610046845X A CNB200610046845X A CN B200610046845XA CN 200610046845 A CN200610046845 A CN 200610046845A CN 100386270 C CN100386270 C CN 100386270C
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Abstract
The present invention discloses the technological process of treating lower segment kettle liquid from acrylonitrile quenching tower, and relates to chemical waste water treating technology. The technological process includes flocculating the lower segment kettle liquid with flocculant, natural settling, centrifugal filtering, combined adsorption, and final decompression evaporating to concentrate. The water vapor from evaporation is used as the secondary heat source, the condensed water is used for replenishing technological water, the concentrated organic heavy components floating in the liquid surface is overflowed and burnt, and the residual concentrated ammonium sulfate solution is dewatered and washed with alcohol solution to obtain ammonium sulfate product, with the washed liquid being filtered and distilled to recover alcohol and the organic heavy residue being burnt or treated in other mode. The process can recover ammonium sulfate and water and reduce air pollution.
Description
The present invention proposes a kind of treatment process method to acrylonitrile quench tower lower portion still liquid, and it relates to carries out technical fields such as technology that physics and chemistry handles, equipment to wastewater from chemical industry.
Two, background technology
Prior art to the treatment process that acrylonitrile quench tower lower portion still liquid adopts is: burn through sending the waste water stove after the simple and easy granule foreign sedimentation.Though it is simple to handle method like this, consume a large amount of oil fuel, and throw away the sulphur ammonium that recovery value is arranged in this strand still liquid, cause certain sulphur and nitrogen oxide to pollute to atmosphere simultaneously, be a kind of less-than-ideal treatment process.
Acrylonitrile quench tower generally is divided into upper and lower two sections.Epimere still liquid contains the sulphur ammonium about 20%, and liquid impurity is less, is sent to ammonium sulfate device usually and removes to reclaim the sulphur ammonium.Hypomere still liquid then constitutes complexity, and all kinds of impurity are more.This strand hypomere still liquid measure that 80,000 tons of/year acrylonitrile installations are discharged be 7 tons/time about, wherein contain sulphur ammonium 10～15%, tens kinds of boiling points are higher than organic heavy component mixture about 20% of 100 ℃, nitrile thing about 1%, granule foreigns such as a small amount of spent catalyst powder and some organic polymers, all the other water of nearly 70%.Liquid appearance is a brownish black, to left standstill and some throw outs can be occurred.Because acrylonitrile quench tower lower portion still liquid water quality is abominable, all handles with burning method at present.80,000 tons of/year acrylonitrile installations only and are burnt 7000～9000 tons of pure sulphur ammoniums with regard to consume fuel oil more than 10,000 tons this every year.
Three, summary of the invention
The purpose of this invention is to provide a kind of new processing method, acrylonitrile quench tower lower portion still liquid is handled, separate granule foreign and the organic heavy component removed wherein, reclaim sulphur ammonium and water.Like this, avoid the direct burning of still liquid, save a large amount of oil fuel, also reduced atmospheric pollution.And sulphur ammonium that reclaims and water also have certain economic value.Though consume certain steam and electric power, 1/2 of the not enough burning method of its comprehensive cost.
Technical scheme of the present invention is: at first quench tower lower portion still liquid is introduced settlement separate facility and carry out dosing flocculation and natural subsidence.Utilize the centrifuging facility to do further processing then.The absorption facility that utilizes combination of materials such as carbon silicon to become again adsorbs.Afterwards, again the liquid of removing most of granule foreign is reduced pressure multiple-effect ground concentration and evaporation.After the water vapor that steams was made secondary heat source, water was sent to and is made the technology make up water with fixed attention.The organic heavy component that is concentrated in the liquid undergoes phase transition separates out oily matter and swims on the liquid level, with the drainage and collecting continuously of overflow mode.After sending to organic heavy component of dewatered and washed with the dissolve with ethanol wash residual, the sulphur ammonium liquid of remaining enrichment becomes ammonium sulfate products.Dissolve and wash away filtrate and go to distill the back and reclaim ethanol and reuse, do not take out organic heavy component that overflow is drawn when concentrating distillation and send the burning of igniting together and volatilize and condense in organic heavy component in the reboiler.The small collected thing of sedimentation, filtration, absorption reclaims, buried or burning disposal.
Four, description of drawings
Accompanying drawing is a process flow sheet of the present invention.
Five, embodiment
Acrylonitrile quench tower lower portion still liquid processing device comprises: fluid inlet 1, dosing mouth 2, dividing plate 3, slurry tank 4, slush pump 5, sedimentation strainer 6, overflow port 7, filtrate tank 8, water outlet 9, stirrer 10, centrifuging jar 11, centrifugal filter 12, adsorption tanks 13, upgrading tower fluid inlet 14, recovery tower reboiler steam inlet 15, upgrading tower 16, upgrading tower reboiler steam inlet 17, the upgrading tower reboiler coagulates water out 18, organic heavy component collector 19, concentrated ammonium sulfate solution outlet 20, drying bed 21, sulphur ammonium inlet 22, ethanol dissolves and washes away jar 23, recovery tower 24, ethanol steams mouth 25, ethanol is gone into tower mouth 26, finished product sulphur ammonium mouth 27, recovery tower reboiler 28, vacuum pump 29, vacuum pump outlet 30.
At first carry out natural subsidence introducing slurry tank 4 by fluid inlet 1 through the quench tower lower portion still liquid of simple and easy sedimentation of a few hours.Liquid has the dividing plate 3 of horizontal ripple to enter in the jar along the surface that is obliquely installed.Difference of altitude is generally more than 10mm between the crest of dividing plate ripple and trough.The design function of dividing plate has two: the one, fluid inlet 1 is separated in both sides with water outlet 9, and prevent liquid dispersion, reduce liquid and just walk the chance that short circuit is directly gone out from water outlet without sedimentation; The 2nd, make liquid drop to pot bottom and rise to water outlet from the dividing plate opposite side more later on, this has been equivalent to prolong the average stroke of liquid in slurry tank, helps improving the natural subsidence separation efficiency.Add an amount of amine flocculation agent by dosing mouth 2 and strengthen effect of settling.Flocculation agent pH value greater than 7 environment in better effects if, and alkaline environment can make in the liquid nitriles substance polymerization and settles down.Slush pump 5 is discharged into sedimentation strainer 6 to sediment discontinuously, and the filtrate that filtrate tank 8 is collected irregularly flows back in the slurry tank 4.Shorten filtration time in order to increase filtration area, sedimentation strainer 6 is designed to: shell is cylindrical, and liner is the filter screen identical shaped with shell, and filter screen vertically is divided into the little strainer that several volumes equate.The situation of arranging of each little strainer from cross section see be exactly an area of a circle by the figure of five equilibrium, they each other and periphery all leave certain space so that filtrate can flow out respectively simultaneously, and do not make a difference.The size in filter screen aperture determines that as required the residence time in the slurry tank should be not less than 8 hours.Strainer wants irregular switching to clean.Enter into centrifuging jar 11 through slurry tank water port 9 effusive liquid, do centrifugal rotatablely moving through stirrer 10.Tank skin is established some in the long and narrow slit of vertical openings as liquid exit, and jar inwall slit side that meets water is established the plate that meets water as liquid choked flow setting, makes the liquid of rotation go centrifugal filter 12 to filter through the plate interception back that meets water outside slit flows out jar.Every slit extension tube attached of tank wall such as fan-shaped as suddenly reducing to compile be a circular catheter, catheter connects with flange, valve with the outer tube of centrifugal filter 12, is convenient to switch, cleaning.Centrifugal linear velocity and the filter screen pore size of liquid in the centrifuging jar determined as required.
The liquid that is come out by centrifugal filter 12 enters in the adsorption tanks 13, and more tiny granule foreign and the metal ion that comes from the spent catalyst powder are adsorbed.The silica-gel sphere that activated carbon and specific surface area are very big is combined into the compound sorbent material.Activated carbon and silica-gel sphere are respectively with silk screen carrying, and layered and parallel is piled up, and require easy to loading and unloadingly, are beneficial to replacing.The residence time of absorption pot liquid is not less than 1 hour.Sorbent material can switch and regenerates according to the effluent quality situation.The specific surface area of silica-gel sphere is not less than 38m
2/ g.
Liquid after the absorption enters upgrading tower 16 to carry out reduction vaporization and concentrates, steam that most of moisture content can make sulphur ammonium and organic heavy component in the liquid be concentrated in the liquid, when they reach finite concentration respectively, organic heavy component undergoes phase transition, become oily matter and float on the liquid level by solubilised state, and flow in organic heavy component collector 19 from overflow port.It is that the container of making lining with the identical shaped filter screen of shell is arranged in cylindrical that organic heavy component collector 19 is designed to a shell, the aperture, lower surface of filter screen is less, periphery aperture ratio lower surface is big, and ascending gradually from bottom to top, and shell has the chuck of logical water coolant.Such structure is convenient to oily matter and is condensed that thereby to be beneficial to long-pending oil hydrophobic.The water of taking out of with organic heavy component returns after organic heavy component collector filters and carries out concentrating and separating in the upgrading tower again.The top of filter housing is provided with visor, will in time switch cleaning when seeing long-pending full gleanings.Bottom being discharged to by dense sulphur ammonium relief outlet 20, the remaining sulphur ammonium that is concentrated dehydrates on the drying bed 21 of the chain-plate type of heating, send into ethanol then and dissolve and wash away jar 23 usefulness ethanol and carry out thermosol and wash, a small amount of organic heavy component dissolving still remaining between sulphur ammonium solid particulate and filter out.Dissolve and wash away and jar be one and have heating and dissolve and wash away container with the filtering separation effect.Can be discharged by finished product sulphur ammonium mouth 27 through the sulphur ammonium after dissolveing and washing away, packing becomes product after the volatilization residual ethanol.Heating steam is introduced from upgrading tower reboiler steam inlet 17, and heat exchange is after the upgrading tower reboiler coagulates water out 18 discharges.The sulphur ammonium concentration that upgrading tower is discharged is controlled at 80～90%, and the working pressure of cat head is 0.4kg/cm
2(A), Dui Ying temperature is about 78 ℃.Drying bed 21 Heating temperatures are less than 100 ℃.
The ethanol filtrate of containing the organic heavy component of dissolved is admitted to evaporates recovery ethanol in the recovery tower 24.Steam mouthful 25 ethanol that steam by cat head ethanol and reclaim the back repeated use.The water vapor that concentrated cat head steams enters reboiler 28 from recovery tower reboiler steam inlet 15, and lime set is extracted out through vacuum pump outlet 30 discharges by vacuum pump 29 and made the technology make up water after the heat exchange.Multiple-effect evaporation under the decompression can make full use of steam source, energy efficient.Recovery tower reboiler 28 is designed to: the peripheral hardware chuck is for heating steam circulation, in the wire filler is arranged for condense cylindrical heat exchanger on it of the organic heavy component after concentrating.The two end cap up and down of interchanger is the plane face flange form.When switching cleaning, open two end cap and take out the wire filler, together send the burning of igniting together with organic heavy component collector 19 gleanings.
Example:
Certain acrylonitrile quench tower lower portion still liquid phase related parameter is: 7 tons of flows/time, wherein the sulphur ammonium 10～15%, tens kinds of boiling points are higher than organic heavy component mixture about 20% of 100 ℃, nitrile thing about 1%, granule foreign such as spent catalyst powder and some organic polymers tens of kilogram/times, all the other water of nearly 70%.Liquid appearance is muddy brownish black, pH value 6.8,70 ℃ of temperature.
Liquid is added in the slurry tank 4 by fluid inlet 1, adds an amount of amine flocculation agent by dosing mouth 2 simultaneously.Liquid flows into a jar bottom along the dividing plate 3 that is obliquely installed in the jar, is overflowed by water outlet 9 after the sedimentation through the residence time more than 8 hours.Remaining impurities particle footpath is less than sedimentation strainer screen aperture in this moment liquid.The settling that falls to tank base is irregularly squeezed in the sedimentation strainer 6 by slush pump 5, when strainer is full of back termination of pumping and begin to filter during by overflow port 7 overflows.The filtrate that filtrate tank 8 is collected is returned in the slurry tank.To clear up filter residue after the each filtration of sedimentation strainer.The filter residue that goes out clearly can reclaim, buried or burning.
Liquid enters in the centrifuging jar 11 under the counterclockwise stirring of agitator 10 and rotates.Liquid is under centrifugal action, and granule foreign wherein gets rid of to tank skin and along long and narrow slit water outlet and enters centrifugal filter 12.Granule foreign particle footpath after filtering in the liquid is less than the strainer screen aperture.Because the amount of this part granule foreign still less, so the cleaning cycle of strainer 12 is longer.To can take off strainer easily behind the valve closes of reducing place during cleaning.After liquid enters the adsorbents adsorb of adsorption tanks 13 through activated carbon and silica-gel sphere composition, granule foreign particle diameter in the water outlet should be in tens micrometer ranges, even can be less than 20 microns, some metal ion also can be absorbed by silica-gel sphere in the liquid, and what have can recycle.Because this part granule foreign seldom, so the switching of the sorbent material regeneration frequency can be seldom.
The liquid of having removed most granule foreigns is entered in the upgrading tower 16 by upgrading tower fluid inlet 14, and this tower is operated under negative pressure, so the service temperature of tower is lower than liquid normal boiling point temperature.The water vapor that cat head steams goes recovery tower 24 to make the heating thermal source, and energy consumption is reduced.Concentrate the organic heavy component of viscous crude shape of separating out in the tower on the liquid level adrift and constantly flow into collection in organic heavy component collector 19, the water that overflow is taken out of then can return in the tower after filtering.The sulphur ammonium of having removed behind most of moisture content and the organic heavy component then enters drying bed 21 by concentrated ammonium sulfate solution outlet 20 at the bottom of the tower, and this moment, the sulphur ammonium concentration about 80～90%.The remaining moisture content of evaporate to dryness is after sulphur ammonium inlet 22 enters ethanol dissolves and washes away in jars 23 and carry out the dissolve with ethanol washing, dissolve and wash away out after organic heavy component remaining between sulphur ammonium particle, after filtration separately, be packaged as product by 27 discharges of finished product sulphur ammonium mouth behind the sulphur ammonium volatilization ethanol with sulphur ammonium particle.Ethanol filtrate is squeezed into recovery tower 24 by ethanol tower inlet 26, coagulates water out 18 by upgrading tower reboiler steam inlet 17 admission heating back by the upgrading tower reboiler and discharges.Flow into because per hour have the gleanings of nearly metric ton, so the cleaning frequency of organic heavy component collector 19 can be higher.The sulphur ammonium product per hour also has the hundreds of kilogram.
Ethanol filtrate through evaporation, steams mouthful 25 ethanol that steam by cat head ethanol and reuses in recovery tower 24.Organic heavy component is concentrated to be stayed in the tower still reboiler 28, will in time switch, clear up according to the heat exchange efficiency situation.The water vapor that upgrading tower steams is entered in the reboiler 28 by recovery tower reboiler steam inlet 15 and provides thermal source for recovery tower.After the heat exchange, lime set is extracted out by vacuum pump 29, discharges acrylonitrile installation through vacuum pump outlet 30 and makes the technology make up water.This technology make up water per hour has nearly about 5 tons.Because bringing organic heavy component of recovery tower into filtrate is not a lot, so the cleaning frequency of recovery tower reboiler 28 does not have the height of organic heavy component collector 19.
Compare with existing pure incinerating method, advantage of the present invention is: with 80,000 ton/years of propylene The nitrile device is example, but every year 1～1.2 ten thousand ton of fuel saving oil, reclaim 7000～9000 tons of sulphur ammoniums, Recycle 40,000 tons in water, and reduced sulphur, nitrogen oxide to the pollution of atmosphere. Although consume Certain steam and power, but the not enough burning method of its integrated cost 1/2, economic benefit and society The meeting benefit is fairly obvious.
Claims (10)
1. method for processing kettle-liquid of acrylonitrile quench tower lower portion is characterized in that: liquid reduces pressure, the multi-purpose concentration and evaporation after flocculation natural subsidence, centrifuging, compound adsorbent adsorption treatment again; After the water vapor that steams is made secondary heat source, coagulate water as the technology make up water; The organic heavy component phase transformation that is concentrated in the liquid is separated out oily matter and is floated on the liquid level, sends the burning of igniting after drawing collection; Become ammonium sulfate products behind remaining organic heavy component of sulphur ammonium liquid dewatered and washed with the dissolve with ethanol wash residual that thickens, dissolve and wash away filtrate and go distillation to reclaim the ethanol repeated use, the organic heavy component that condenses in the reboiler takes out the burning of igniting; Recyclable, the buried or burning of the gleanings of sedimentation, filtration, absorption.
2. method for processing kettle-liquid of acrylonitrile quench tower lower portion according to claim 1, it is characterized in that: acrylonitrile quench tower lower portion still liquid is introduced slurry tank (4) sedimentation by fluid inlet 1, establish in the slurry tank (4) inclination, there is the dividing plate (3) of horizontal ripple on the surface, the liquid that adds flocculation agent flows into a jar end from fluid inlet (1) along dividing plate (3), being turned back by dividing plate (3) opposite side rises to water outlet (9) and overflow again.
3. method for processing kettle-liquid of acrylonitrile quench tower lower portion according to claim 1, it is characterized in that: the flocculating settling thing is entered in the sedimentation strainer (6) aperiodically by slush pump (5), sedimentation strainer (6) shell is cylindrical, liner is the filter screen identical shaped with shell, filter screen vertically is divided into the little strainer that several volumes equate, reaches periphery between each little strainer and all leaves for the effusive space of filtrate.
4. method for processing kettle-liquid of acrylonitrile quench tower lower portion according to claim 1, it is characterized in that: enter into centrifuging jar (11) through the effusive liquid of slurry tank water port (9), centrifuging jar (11) tank skin is vertically opened some in long and narrow slit, the long and narrow slit of jar inwall side that meets water has water eliminator, the extension tube attached reducing of the long and narrow slit of tank wall is a circular catheter, and this catheter and centrifugal filter (12) outer tube links with flange, valve.
5. method for processing kettle-liquid of acrylonitrile quench tower lower portion according to claim 1, it is characterized in that: the liquid that is come out by centrifugal filter (12) enters in the adsorption tanks (13), sorbent material in the adsorption tanks (13) is activated carbon and silica-gel sphere, they are piled up with silk screen carrying layered and parallel, and the silica-gel sphere specific surface area is not less than 38m
2/ gram.
6. method for processing kettle-liquid of acrylonitrile quench tower lower portion according to claim 1, it is characterized in that: the liquid after the absorption enters upgrading tower (16) to carry out reduction vaporization and concentrates, upgrading tower (16) is operated under negative pressure, and the water vapor that cat head steams goes recovery tower reboiler (28) to make to coagulate after the secondary heat source water and makes the technology make up water; Concentrate the organic heavy component continuous overflow of oily of separating out and enter organic heavy component collector (19), the water of taking out of returns in the upgrading tower (16) after organic heavy component collector (19) is hydrophobic; Go to dissolve and wash away behind the further dewatered and washed of sulphur ammonium of the concentration 80～90% that the tower still is discharged with ethanol.
7. method for processing kettle-liquid of acrylonitrile quench tower lower portion according to claim 1, it is characterized in that: organic heavy component collector (19) be a shell be cylindrical, in have the filter screen identical to make the container of lining with shell shape, the aperture of filter screen periphery aperture ratio lower surface is big, and the aperture is ascending gradually from bottom to top, filter housing is provided with the chuck of logical water coolant, and shell upper is provided with visor.
8. method for processing kettle-liquid of acrylonitrile quench tower lower portion according to claim 1 is characterized in that: organic heavy component remaining between sulphur ammonium particle dissolves washing with ethanol, and then, the liquid filtering separation that dissolves and washes away that will contain organic heavy component from the sulphur ammonium is gone out.
9. method for processing kettle-liquid of acrylonitrile quench tower lower portion according to claim 1 is characterized in that: the ethanol that contains organic heavy component dissolves and washes away liquid and steams the repeated use of recovery ethanol by recovery tower (24) cat head, and organic heavy component is condensed in the reboiler (28).
10. method for processing kettle-liquid of acrylonitrile quench tower lower portion according to claim 1 is characterized in that: recovery tower reboiler (28) is a jacketed type, circulates for heating steam in the chuck; The wire filler is arranged in the reboiler, and the two end cap up and down of reboiler is the plane face flange formula.
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| CNB200610046845XA CN100386270C (en) | 2006-06-06 | 2006-06-06 | Method for processing kettle-liquid of acrylonitrile quench tower lower portion |
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| CN100386270C true CN100386270C (en) | 2008-05-07 |
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| CN102311179A (en) * | 2010-07-09 | 2012-01-11 | 中国石油化工股份有限公司 | Centrifugal sedimentation method for treating catalyst-containing waste liquid in acrylonitrile industries |
| CN102452756B (en) * | 2010-10-22 | 2013-04-24 | 中国石油化工股份有限公司 | Treatment method of wastewater from acrylonitrile production device by propylene ammoxidation |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1413980A (en) * | 2001-10-22 | 2003-04-30 | 中国石油化工股份有限公司 | Quench process of acrylonitrile |
| CN1508121A (en) * | 2002-12-17 | 2004-06-30 | 中国石油化工股份有限公司 | Acrylonitrile quench method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1413980A (en) * | 2001-10-22 | 2003-04-30 | 中国石油化工股份有限公司 | Quench process of acrylonitrile |
| CN1508121A (en) * | 2002-12-17 | 2004-06-30 | 中国石油化工股份有限公司 | Acrylonitrile quench method |
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