CN103566608B - A kind of regenerative system of cracking c_5 separator solvent and renovation process - Google Patents
A kind of regenerative system of cracking c_5 separator solvent and renovation process Download PDFInfo
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- CN103566608B CN103566608B CN201210254374.7A CN201210254374A CN103566608B CN 103566608 B CN103566608 B CN 103566608B CN 201210254374 A CN201210254374 A CN 201210254374A CN 103566608 B CN103566608 B CN 103566608B
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Abstract
The invention discloses a kind of regenerative system and renovation process of cracking c_5 separator solvent.System comprises: thick solvent tank, solvent refining tower and return tank, and described thick solvent tank outlet at bottom connects solvent refining tower, and solvent refining top of tower returns solvent refining tower after connecting return tank, is provided with flash tank, reboiler before thick solvent tank; Described reboiler connects flash tank, and flash drum overhead connects thick solvent tank, connects waste residue tank bottom flash tank; Flash drum overhead is provided with solvent oil pipeline.Method comprises: circulating solvent enters flash tank after reboiler heating, and flash drum overhead extraction material enters solvent refining tower and refines after condensation, and solvent refining tower tower reactor obtains neat solvent; The extraction of flash tank bottoms interval is to waste residue tank.System and method of the present invention can make solvent better be separated with tar, decreases the possibility of tar accumulation simultaneously, improves the economic benefit of device, decrease manipulation strength.
Description
Technical field
The present invention relates to carbon five field, furtherly, relate to a kind of regenerative system and renovation process of cracking c_5 separator solvent.
Background technology
The C5 fraction of the quite a lot of quantity of by-product in petroleum cracking process of producing ethylene, the dienes such as isoprene, pentadiene and cyclopentadiene are rich in C5 fraction.These diolefin chemical property are active, are important industrial chemicals.By the difference on the raw material of petroleum hydrocarbon cracking, cracking severity and separation degree, the diolefin content in C5 fraction is different, but total amount is in the middle of 40 ~ 60%.Therefore, extraction and application C5 fraction for improve ethylene unit economic benefit, comprehensive utilization petroleum resources there is profound significance.
Cracked C 5 fraction is close by more than 20 kinds of boiling points, easily formed to each other azeotropic mixture component composition, therefrom isolate purity meet application require diolefin difficulty higher, technique is comparatively complicated, generally adopts extraction fractional distillation in prior art.Conventional selective solvent has dimethyl formamide (DMF), acetonitrile and 1-METHYLPYRROLIDONE, the process as patent JP63101338, JP74019245, US3510405, US3535260 etc. Suo Gongkai.Wherein DMF solvent has plurality of advantages such as selective good, the solubility of C 5 diene are large and carbon five is easily separated, corrosivity is low and toxicity is little.
In order to the isoprene product of high-purity, generally adopt two-section extraction rectificating method in prior art, main extractant is dimethyl formamide (DMF), acetonitrile etc.As in DMF method carbon five separation process by Beijing Chemical Research Institute and Beijing petrochemical industry project company (being now Sinopec Engineering Incorporation) joint development, first feed material preparation units is utilized to carry out pretreatment to carbon Wuyuan material, remove most carbon five alkynes, carbon four and part carbon five light component, then dipolymer reactor is entered, make most of cyclopentadiene become dicyclopentadiene, remove whole carbon six, dicyclo and the heavy constituent such as part pentadiene and cyclopentadiene at pre-weight-removing column; Pre-weight-removing column top material enters an extraction unit, adopts DMF as solvent, removes alkane in C5 fraction and monoolefine, obtain chemical grade isoprene in an extraction system; Remove alkynes wherein and cyclopentadiene in the second extraction cells, alkynes is crotonylene and pentone mainly, finally obtains polymerization grade isoprene product; Enter pentadiene and dicyclopentadiene unit by pre-de-heavy and weight-removing column still material to be separated by rectifying and to obtain pentadiene and dicyclopentadiene product respectively; Because the solvent of an extraction and two extraction systems recycles, and operating temperature is higher, the autopolymer of inevitable isoprene, pentadiene and copolymer generation between two, therefore need a small gangs of desolventizing regenerative system of the continuous extraction of circulating solvent by an extraction and two extraction systems.
Chinese patent CN1803764A discloses the renovation process of DMF after a kind of carbon five extraction desorption, and as shown in Figure 1, this is also the method that current industrialized unit generally adopts.Its basic procedure be solvent to be regenerated first in heavy constituents such as solvent reclamation still pressure reducing and steaming colloids, the logistics that gas phase is formed enters DMF surge tank after cooling.In surge tank, material sends into purification and recover tower through DMF purification and recover tower feeding pump, purification and recover tower is atmospheric operation, pass through azeotropic distillation, the hydrocarbon compounds such as removed overhead water, carbon five hydrocarbon and carbon five oligomer, tower reactor obtains the DMF solvent of more than 99% purity, returns extraction cells solvent as a supplement.
It is that solvent reclamation still constantly steams solvent DMF and carbon five hydro carbons that above-mentioned solvent regeneration system mainly has problems, colloid heavier in circulating solvent, black bits are constantly accumulated, when DMF is difficult to steam, again circulating solvent charging is switched in another regeneration still, due to colloid in regeneration still, comparatively viscous flow is slow, so heat-transfer effect is poor, the solids adhering formed after sticky material cooling is simultaneously in the heat exchanger tube of regeneration still, regeneration still is made to need frequent labor cleaning, on-the-spot foul odour is very serious, cleaning adds the labour intensity of workman frequently on the one hand, also impact regenerates the service life of still simultaneously, thus affect the economic benefit of device, the easy contaminated environment of polymer of stench on the other hand, affect workman healthy.
Chinese patent CN101397261A discloses a kind of renovation process of dimethylformamide as extracting solvent for cracking carbon 5, its key step is that the extractant dimethyl formamide that need regenerate enters solvent reclamation still, extract gaseous stream through decompression distillation out from regeneration still top, extract impure liquid phase stream out from lower end; Gaseous stream enters dehydrating tower, comprises the logistics of carbon five hydrocarbon and water through rectification under vacuum from overhead extraction, enters solvent refining tower from the water-free liquid stream of tower reactor extraction; Through the regenerated solvent of rectification under vacuum tower top extraction based on DMF in solvent refining tower, the dimeric liquid stream of tower reactor extraction carbon containing five enters solvent recovery tower with merging from the impure liquid stream regenerating still, through rectification under vacuum, recovered overhead solvent is merged into dehydrating tower charging, and kettle material is sent into residue release interval and discharged residue.This flow process can solve the problem such as solvent hydrolysis and blocking tower, but defect is that heat(ing) coil is in regeneration still, because liquid phase gravity flow is slower, heat-transfer effect is poor, extends tar simultaneously in time and is very easily accumulated in heat(ing) coil, need timing cleaning, and need the residue release of increase by two towers and belt stirrer, energy consumption and equipment investment higher, running cost increase, be not the flow process of very economical.
Chinese patent CN101450909A discloses a kind of segregation and fractionation regeneration method of dimethylformamide as extracting solvent for cracking carbon 5, its key step is that the extractant dimethyl formamide that need regenerate enters solvent reclamation still, extract gaseous stream through decompression distillation out from regeneration still top, extract impure liquid phase stream out from lower end; Gaseous stream enters segregation fractionating column middle and upper part, comprises the logistics of carbon five hydrocarbon and water through rectification under vacuum from overhead extraction; Extracting impure liquid phase stream out from regeneration still lower end enters with the residue toilet-cleaning jar stirred and heat, the gaseous stream steamed from residue toilet-cleaning jar top enters segregation fractionating column middle and lower part, discharges the logistics containing dicyclopentadiene, carbon five dimer and colloid bottom residue toilet-cleaning jar; Segregation fractionating column bottoms effluent flows to into residue toilet-cleaning jar, from the dimethyl formamide that the extraction of segregation fractionating column middle and lower part is regenerated.This flow process is on the one hand because heat(ing) coil is in regeneration still, heat-transfer effect is poor, extend tar in time to be very easily accumulated in heat(ing) coil simultaneously, need timing cleaning, on the other hand because the oligomer boiling point of DMF and carbon five is close, so the DMF purity of side take-off does not reach 99%, and CPD and DCPD can not meet the requirement being less than 1PPM and 0.2% respectively, therefore the needs of two extraction systemic circulation solvents can not be met, one-section abstraction flow process can only be used for, be of limited application.
Summary of the invention
Poor for solving solvent reclamation still heat-transfer effect in prior art, frequently switch and clear up, running cost and the larger problem of labour intensity.The invention provides a kind of regenerative system and method for cracking c_5 separator solvent.By heater and regeneration still are peeled off, increase flash tank agitator, enhance heat-transfer effect on the one hand, the flowing of material in flash tank is strengthened on the other hand by the stirring action of agitator, solvent is better separated with tar, decrease the possibility of tar accumulation simultaneously, improve the economic benefit of device, decrease manipulation strength.
An object of the present invention is to provide a kind of regenerative system of cracking c_5 separator solvent.
Comprise: thick solvent tank, solvent refining tower and return tank, described thick solvent tank outlet at bottom connects solvent refining tower, and solvent refining top of tower returns solvent refining tower after connecting return tank,
Flash tank, reboiler is provided with before described thick solvent tank; Described reboiler connects flash tank, and flash drum overhead connects thick solvent tank, connects waste residue tank bottom flash tank; Flash drum overhead is provided with solvent oil pipeline.
Described flash tank outer setting has heat(ing) coil or jacket pipe, passes into low-pressure steam and make flash tank inside holding 110 ~ 150 DEG C in coil pipe or chuck; Inside is provided with agitator, stirs continuously during normal operation.
Higher than flash tank charging aperture bottom described reboiler, in order to avoid heavy constituent accumulates in flash tank reboiler, namely reboiler outlet streams can flow in flash tank certainly.
Two of object of the present invention is to provide a kind of renovation process of cracking c_5 separator solvent.
Comprise: circulating solvent enters flash tank after reboiler heating, and flash drum overhead extraction material enters solvent refining tower and refines after condensation, and solvent refining tower tower reactor obtains neat solvent;
The extraction of flash tank bottoms interval is to waste residue tank.
Regenerated solvent enters flash tank after reboiler is heated to 115 ~ 160 DEG C.
The operating pressure of described flash tank is-0.06 ~-0.09MpaG;
The temperature of flash tank is 110 ~ 150 DEG C.
Flash drum overhead extraction material after being cooled to 80 ~ 120 DEG C material by being pumped into solvent refining tower.
When tar viscosity in flash tank comparatively large not easily discharge or flash distillation tank skin have tar residue, pass into solvent naphtha, continue to stir and pass into steam in coil pipe or jacket pipe all to dissolve to tar, then the solvent naphtha containing tar is drained into waste residue tank;
Described solvent naphtha to be boiling range the be C of 100 ~ 370 DEG C
6~ C
12hydrocarbon mixture, by can for the purpose of dissolved tar residue, as one of in carbon eight, carbon nine, carbon ten hydrocarbon mixture or they are whole, or the aromatic hydrocarbons such as toluene, dimethylbenzene or non-aromatics.
When liquid level in flash tank raises and flash tank temperature constantly raises, open pot bottom and be exported to waste residue tank pipeline valve, the while for the treatment of that in flash tank, liquid level falls after rise, flash tank temperature is reduced to 110 ~ 150 DEG C of stopping extraction.
Specifically can by the following technical solutions:
As shown in Figure 2, mainly comprise the following steps:
A) solvent come by carbon five device extraction cells stripping tower reactor enters flash tank reboiler, is warming up to 115 ~ 160 DEG C,
After heating, material enters solvent flashing tank, and this still is with agitator, and top is connected with solvent oil pipeline, and flash tank operating pressure is-0.06 ~-0.09MPaG, and top steams DMF steam, bottom interval extraction liquid phase stream.
B) there are heat(ing) coil or jacket pipe pattern in flash tank outside, passes into low-pressure steam and make flash tank inside holding 110 ~ 150 DEG C in coil pipe or chuck; There is agitator flash tank inside, stirs continuously during normal operation.
The top extraction of flash tank normal condition, stops charging in interval situation, opens outlet at bottom and start discharging, depending on material state in flash tank to waste residue tank (or waste residue pond) valve.When liquid level in flash tank raises and temperature constantly raises, show that tar accumulation is more, namely charging is stopped, start to concentrate, keep passing into quantity of steam in flash tank external heat coil pipe or jacket pipe constant, continue to be stirred to liquid phase bubble-free when emerging simultaneously, stop top extraction, pass into nitrogen vacuum breaker, liquid phase material in flash tank is expelled to waste residue tank or waste residue pond.Discharge the complete charging namely restarting regenerated solvent.To note in operating process observing tar situation in flash tank (avoid cause because of excessively concentrated discharge is smooth or solvent is more and increase solvent loss and contaminated environment) by visor.When tar viscosity comparatively large not easily discharge or flash distillation tank skin have tar residue, the valve can opening flash drum overhead connection solvent naphtha passes into solvent naphtha, continue stir and pass into steam in coil pipe or jacket pipe, all dissolve to tar, then the solvent naphtha containing tar is drained into waste residue tank (or waste residue pond).
C) first entered regeneration still condenser by solvent flashing tank top extraction gas phase, and be cooled to 80 ~ 120 DEG C, after cooling, material is by being pumped into solvent refining tower.
D) solvent refining tower is entered through the cooled material of solvent reclamation still condenser, pass through conventional distillation, tower top steams the hydrocarbon compounds such as water, carbon five hydrocarbon and carbon five oligomer, and tower reactor obtains the DMF solvent of more than 99% purity, returns extraction cells solvent as a supplement.
Above-described step c and d can adopt usual way in prior art.
Solvent in extractive distillation column is selected from least one in dimethyl formamide, dimethylacetylamide and the 1-METHYLPYRROLIDONE aqueous solution.
The present invention has the following advantages:
1. heater and regeneration still are peeled off, increase agitator, enhances heat-transfer effect, correspondingly decreases heat exchange area, decrease investment;
2. whole process can realize closed-loop operation, decreases the possibility of polymer exposure air, thus decreases the discharge of pollutant; Two regeneration stills when prior art is normally run, when a still liquid level height, just another still charging is switched to, still before keeps and steams until solvent major part is distilled out of, again by this still vacuum breaker batch turning, along with the operating time extends, due to tar accumulation, make manually regularly to open regeneration still cleaning tar, while contaminated environment, too increase labour intensity and the occupational hazards of workman.One aspect of the present invention heater is separated with regeneration still, and higher than flash tank charging aperture, so tar can not accumulate on heat exchanger tube, in flash tank, tar cleaning can closed-loop operation and do not need labor cleaning simultaneously;
3. strengthened the flowing of material in flash tank by the stirring action of agitator, solvent is better separated with tar, decrease the possibility of tar accumulation simultaneously, improve the economic benefit of device, decrease manipulation strength.
4. by increasing the pipeline of solvent naphtha, utilizing solvent naphtha to be dissolved by the tar of remnants, improving the mobility of tar, make whole operation can automation, add security and the hommization of device.
System and method of the present invention is not only applicable to DMF(dimethyl formamide), be also applicable to dimethylacetylamide, 1-METHYLPYRROLIDONE.
Accompanying drawing explanation
Fig. 1 tradition cracking c_5 separator circulating solvent regenerative system schematic diagram
Fig. 2 cracking c_5 separator of the present invention circulating solvent regenerative system schematic diagram
Description of reference numerals:
1-solvent reclamation still (A B is for subsequent use each other), 2-reboiler, 3-flash tank, 4-agitator, 5-waste residue tank, 6-condenser, the thick solvent tank of 7-, the thick solvent pump of 8-, 9-solvent refining tower, 10-solvent refining tower reboiler, 11-solvent refining tower condenser, 12-solvent refining tower return tank, 13-solvent refining tower reflux pump, 14-solvent refining tower reactor pump; 15-circulating solvent; 16-solvent naphtha
Detailed description of the invention
Below in conjunction with embodiment, further illustrate the present invention.
Embodiment:
As shown in Figure 2, a kind of cracking c_5 separator circulating solvent regenerative system.
Comprise: thick solvent tank 7, solvent refining tower 9 and return tank 12, described thick solvent tank 7 outlet at bottom connects solvent refining tower 9, and solvent refining tower 9 top returns solvent refining tower after connecting return tank 12,
Be provided with flash tank 3 and reboiler 2 before described thick solvent tank 7, in flash tank, be provided with agitator 4; Described reboiler 2 connects flash tank 3, and flash tank 3 top connects thick solvent tank 7, connects waste residue tank 5 bottom flash tank 3.
Described flash drum overhead is connected with solvent oil pipeline.
Described flash tank 3 is outside equipped with heat(ing) coil.
Higher than flash tank charging aperture bottom described reboiler 2.
A) solvent dimethylformamide (DMF) come by carbon five device extraction cells stripping tower reactor enters reboiler, be warming up to 120 DEG C, operating pressure is-0.011MPaG, after heating, material enters flash tank, the operating pressure of flash tank is-0.066MPaG, operating temperature is 116 DEG C, and top steams DMF steam, bottom interval extraction liquid phase stream.
B) flash tank outside has in heat(ing) coil coil pipe and passes into low-pressure steam and make flash tank inside holding 110 ~ 150 DEG C; There is agitator flash tank inside, stirs continuously during normal operation.
The top extraction of flash tank normal condition, stops charging in interval situation, opens outlet at bottom and start discharging to waste residue tank valve, depending on material state in flash tank.When liquid level in flash tank raises and temperature constantly raises, show that tar accumulation is more, namely charging is stopped, start to concentrate, keep flash tank external heat coil pipe to pass into quantity of steam constant, continue to be stirred to liquid phase bubble-free when emerging simultaneously, stop top extraction, pass into nitrogen vacuum breaker, liquid phase material in flash tank is expelled to waste residue tank or waste residue pond.Discharge the complete charging namely restarting regenerated solvent.To note in operating process observing tar situation in flash tank (avoid cause because of excessively concentrated discharge is smooth or solvent is more and increase solvent loss and contaminated environment) by visor.When tar viscosity comparatively large not easily discharge or flash distillation tank skin have tar residue, the valve can opening flash drum overhead connection solvent naphtha passes into solvent naphtha, continue stir and pass into steam in coil pipe, all dissolve to tar, then the solvent naphtha containing tar is drained into waste residue tank.The solvent naphtha adopted is the dish oil of ethylene unit, is C
9~ C
12hydrocarbon mixture.
C) first entered regeneration still condenser by solvent flashing tank top extraction gas phase, and be cooled to 100 DEG C, after cooling, material is by being pumped into solvent refining tower.
D) solvent refining tower is entered through the cooled material of solvent reclamation still condenser, pass through conventional distillation, tower top steams the hydrocarbon compounds such as water, carbon five hydrocarbon and carbon five oligomer, and tower reactor obtains the DMF solvent of more than 99% purity, returns extraction cells solvent as a supplement.
Claims (8)
1. the regenerative system of a cracking c_5 separator solvent, comprise: thick solvent tank, solvent refining tower and return tank, described thick solvent tank outlet at bottom connects solvent refining tower, and solvent refining top of tower returns solvent refining tower after connecting return tank, it is characterized in that:
Flash tank, reboiler is provided with before described thick solvent tank; Described reboiler connects flash tank, and flash drum overhead connects thick solvent tank, connects waste residue tank bottom flash tank; Flash drum overhead is provided with solvent oil pipeline;
Described flash tank outer setting has heat(ing) coil or jacket pipe, and inside is provided with agitator.
2. the regenerative system of cracking c_5 separator solvent as claimed in claim 1, is characterized in that:
Higher than flash tank charging aperture bottom described reboiler.
3. a renovation process for the regenerative system of the cracking c_5 separator solvent as described in one of claim 1 ~ 2, comprising:
Circulating solvent enters flash tank after reboiler heating, and flash drum overhead extraction material enters solvent refining tower and refines after condensation, and solvent refining tower tower reactor obtains neat solvent;
The extraction of flash tank bottoms interval is to waste residue tank.
4. renovation process as claimed in claim 3, is characterized in that:
Regenerated solvent enters flash tank after reboiler is heated to 115 ~ 160 DEG C.
5. renovation process as claimed in claim 3, is characterized in that:
The operating pressure of described flash tank is-0.06 ~-0.09MpaG;
The temperature of flash tank is 110 ~ 150 DEG C.
6. renovation process as claimed in claim 3, is characterized in that:
Flash drum overhead extraction material after being cooled to 80 ~ 120 DEG C material by being pumped into solvent refining tower.
7. the renovation process as described in one of claim 3 ~ 6, is characterized in that:
When tar viscosity in flash tank comparatively large not easily discharge or flash distillation tank skin have tar residue, pass into solvent naphtha, continue to stir and pass into steam in coil pipe or jacket pipe all to dissolve to tar, then the solvent naphtha containing tar is drained into waste residue tank;
Described solvent naphtha to be boiling range the be C of 100 ~ 370 DEG C
6~ C
12hydrocarbon mixture.
8. renovation process as claimed in claim 7, is characterized in that:
When liquid level in flash tank raises and flash tank temperature constantly raises, open pot bottom and be exported to waste residue tank pipeline valve, the while for the treatment of that in flash tank, liquid level falls after rise, flash tank temperature is reduced to 110 ~ 150 DEG C of stopping extraction.
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| CN103566608B true CN103566608B (en) | 2015-08-12 |
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| CN106811223A (en) * | 2017-03-22 | 2017-06-09 | 福建省环境工程有限公司 | A kind of tar processing method and processing unit |
| CN107875664B (en) * | 2017-12-21 | 2023-09-26 | 新疆工程学院 | Propylene-propane thermal coupling rectifying energy-saving device |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1803764A (en) * | 2005-12-26 | 2006-07-19 | 山东玉皇化工有限公司 | N, N-dimethylformamide regeneration method after C5 extraction desorption |
| CN101397261A (en) * | 2007-09-24 | 2009-04-01 | 中国石油化工股份有限公司 | Regeneration method of dimethylformamide as extracting solvent for cracking carbon 5 and use thereof |
| CN101759590A (en) * | 2009-05-16 | 2010-06-30 | 石狮龙祥制革有限公司 | DMF recycling method |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1803764A (en) * | 2005-12-26 | 2006-07-19 | 山东玉皇化工有限公司 | N, N-dimethylformamide regeneration method after C5 extraction desorption |
| CN101397261A (en) * | 2007-09-24 | 2009-04-01 | 中国石油化工股份有限公司 | Regeneration method of dimethylformamide as extracting solvent for cracking carbon 5 and use thereof |
| CN101759590A (en) * | 2009-05-16 | 2010-06-30 | 石狮龙祥制革有限公司 | DMF recycling method |
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Address after: No. 22, Chaoyangmen North Street, Chaoyang District, Beijing 100728 Patentee after: China Petrochemical Group Co., Ltd Patentee after: Sinopec Engineering Construction Co., Ltd Address before: No. 22, Chaoyangmen North Street, Chaoyang District, Beijing 100728 Patentee before: China Petrochemical Corporation Patentee before: Sinopec Engineering Construction Co., Ltd |