CN103566608A - Regeneration system and regeneration method for solvent of cracked C5 separation device - Google Patents
Regeneration system and regeneration method for solvent of cracked C5 separation device Download PDFInfo
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- CN103566608A CN103566608A CN201210254374.7A CN201210254374A CN103566608A CN 103566608 A CN103566608 A CN 103566608A CN 201210254374 A CN201210254374 A CN 201210254374A CN 103566608 A CN103566608 A CN 103566608A
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Abstract
The invention discloses a regeneration system and a regeneration method for the solvent of a cracked C5 separation device. The system comprises a crude solvent tank, a solvent refining tower and a reflux tank, wherein an outlet in the bottom of the crude solvent tank is connected with the solvent refining tower, the top of the solvent refining tower is connected with the reflux tank and then returns to the solvent refining tower, and a flash tank and a reboiler are arranged in front of the crude solvent tank; the reboiler is connected with the flash tank, the top of the flash tank is connected with the crude solvent tank, and the bottom of the flash tank is connected with a waste residue tank; and a solvent oil pipeline is arranged at the top of the flash tank. The method comprises the following steps that: a circulating solvent enters in the flash tank after being heated by the reboiler, materials extracted from the top of the flash tank enter in the solvent refining tower to be refined after being condensed, and a pure solvent is obtained in the tower kettle of the solvent refining tower; and a material flow at the bottom of the flash tank is intermittently extracted to the waste residue tank. According to the system and the method disclosed by the invention, the solvent can be separated from tar better, meanwhile, the possibility of tar accumulation is reduced, the economic benefits of the device are improved, and the operation strength is reduced.
Description
Technical field
The present invention relates to carbon five fields, 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 raw material, cracking severity and the separation degree of petroleum hydrocarbon cracking, the diolefin content in C5 fraction is different, but total amount is in the middle of 40～60%.Therefore, extraction and application C5 fraction has profound significance for the economic benefit, the comprehensive utilization petroleum resources that improve ethylene unit.
Cracked C 5 fraction is close by more than 20 kinds of boiling points, and the component that easily forms to each other azeotropic mixture forms, and therefrom isolating purity, to meet the diolefin difficulty of application requirements higher, and technique is comparatively complicated, generally adopts extraction fractional distillation in prior art.Conventional selective solvent has dimethyl formamide (DMF), acetonitrile and 1-METHYLPYRROLIDONE, as disclosed processes such as patent JP63101338, JP74019245, US3510405, US3535260.Wherein DMF solvent has the plurality of advantages such as large to selectively good, the solubility of C 5 diene, easily separated with carbon five, corrosivity is low and toxicity is little.
For the isoprene product of high-purity, in prior art, generally adopt two-section extraction rectificating method, main extractant is dimethyl formamide (DMF), acetonitrile etc.In DMF method carbon five separation process of Ru You Beijing Chemical Research Institute and Beijing petrochemical industry project company (Xian Wei Sinopec Engineering Incorporation) joint development, first utilize Dui Tan Wuyuan, pretreatment of raw material unit material to carry out pretreatment, remove most carbon five alkynes, carbon four and part carbon five light components, then enter dipolymer reactor, make most of cyclopentadiene two be polymerized to dicyclopentadiene, at pre-weight-removing column, remove the heavy constituents such as whole carbon six, dicyclo and part pentadiene and cyclopentadiene; Pre-weight-removing column top material enters an extraction unit, adopts DMF as solvent, in an extraction system, removes alkane and the monoolefine in C5 fraction, obtains chemical grade isoprene; In the second extraction cells, remove alkynes and cyclopentadiene wherein, alkynes is mainly crotonylene and pentone, finally obtains polymerization grade isoprene product; By pre-de-heavy and weight-removing column still material enter pentadiene with dicyclopentadiene unit by separated pentadiene and the dicyclopentadiene product of obtaining respectively of rectifying; Due to an extraction and two extraction systems solvents be to recycle, and operating temperature is higher, the inevitably autopolymer of isoprene, pentadiene and copolymer generation between two, therefore need to be by a small gangs of desolventizing regenerative system of the continuous extraction of circulating solvent of an extraction and two extraction systems.
Chinese patent CN1803764A discloses the renovation process of DMF after a kind of carbon five extraction desorptions, 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 formed logistics of gas phase enters DMF surge tank after cooling.In surge tank, material is sent 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 99% above purity, returns to 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, heavier colloid in circulating solvent, black bits are constantly accumulated, when DMF is difficult to steam, again circulating solvent charging is switched in another regeneration still, because colloid in regeneration still is mobile slowly compared with thickness, so heat-transfer effect is poor, the solids adhering of the cooling rear formation of sticky material is in the heat exchanger tube of regeneration still simultaneously, the still that makes to regenerate needs frequent labor cleaning, on-the-spot foul odour is very serious, clear up frequently on the one hand the labour intensity that has increased workman, also affect the service life of regeneration still simultaneously, thereby affect the economic benefit of device, the easy contaminated environment of the 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 of need regeneration is entered to solvent reclamation still, through decompression distillation, from regeneration still top, extract gaseous stream out, from lower end, extract impure liquid phase stream out; Gaseous stream enters dehydrating tower, and the logistics that comprises carbon five hydrocarbon and water from overhead extraction through rectification under vacuum, enters solvent refining tower from the water-free liquid stream of tower reactor extraction; In solvent refining tower, through rectification under vacuum overhead extraction, take DMF as main regenerated solvent, tower reactor extraction carbon containing five dimeric liquid streams enter solvent recovery tower with the impure liquid stream merging from regeneration still, through rectification under vacuum, recovered overhead solvent merges to dehydrating tower charging, and tower reactor material is sent into residue release and intermittently discharged residue.This flow process can solve solvent hydrolysis and stop up the problems such as 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 in time tar and is very easily accumulated in heat(ing) coil simultaneously, needs regularly cleaning, and need to increase the residue release of two towers and belt stirrer, energy consumption and equipment investment are higher, and running cost increases, and is 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 of need regeneration is entered to solvent reclamation still, through decompression distillation, from regeneration still top, extract gaseous stream out, from lower end, extract impure liquid phase stream out; Gaseous stream enters segregation fractionating column middle and upper part, the logistics that comprises carbon five hydrocarbon and water from overhead extraction through rectification under vacuum; From regeneration still lower end, extracting impure liquid phase stream out enters with the residue toilet-cleaning jar that stirs and heat, the gaseous stream steaming from residue toilet-cleaning jar top enters segregation fractionating column middle and lower part, and the logistics that contains dicyclopentadiene, carbon five dimers and colloid is discharged in residue toilet-cleaning jar bottom; Segregation and fractionation tower bottom effluent stream enters residue toilet-cleaning jar, the dimethyl formamide of regenerating from the extraction of segregation fractionating column middle and lower part.This flow process is on the one hand because heat(ing) coil is in regeneration still, heat-transfer effect is poor, extend in time tar is very easily accumulated in heat(ing) coil simultaneously, need regularly cleaning, the oligomer boiling point due to DMF and carbon five approaches on the other hand, so the DMF purity of side line extraction does not reach 99%, and CPD and DCPD can not meet the requirement that is less than respectively 1PPM and 0.2%, therefore can not meet the needs of two extraction systemic circulation solvents, can only, for one-section abstraction flow process, be of limited application.
Summary of the invention
Poor for solvent reclamation still heat-transfer effect in solution prior art, frequently switch and clear up, the problem that running cost and labour intensity are larger.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, strengthened on the one hand heat-transfer effect, by the stirring action of agitator, strengthened flowing of material in flash tank on the other hand, make solvent better separated with tar, reduce the possibility of tar accumulation simultaneously, improved the economic benefit of device, reduced manipulation strength.
One of 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 to solvent refining tower after connecting return tank,
Before described thick solvent tank, be provided with flash tank, reboiler; Described reboiler connects flash tank, and flash drum overhead connects thick solvent tank, and flash tank bottom connects waste residue tank; Flash drum overhead is provided with solvent naphtha pipeline.
Described flash tank outer setting has heat(ing) coil or jacket pipe, passes into low-pressure steam and make to be incubated 110～150 ℃ in flash tank in coil pipe or chuck; Inside is provided with agitator, continuous stirring while normally moving.
Described reboiler bottom is higher than flash tank charging aperture, in order to avoid heavy constituent accumulates in flash tank reboiler, i.e. reboiler outlet logistics 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 it is refining that flash drum overhead extraction material enters solvent refining tower after condensation, and solvent refining tower tower reactor obtains neat solvent;
The extraction at intermittence of flash tank bottoms is to waste residue tank.
Regenerated solvent enters flash tank after reboiler is heated to 115～160 ℃.
The operating pressure of described flash tank is-0.06～-0.09MpaG;
The temperature of flash tank is 110～150 ℃.
Flash drum overhead extraction material after being cooled to 80～120 ℃ material by being pumped into solvent refining tower.
When the more difficult discharge of tar viscosity or flash distillation tank skin have tar residue in flash tank, pass into solvent naphtha, continue to stir and in coil pipe or jacket pipe, pass into steam to tar all to dissolve, then the solvent naphtha containing tar is drained into waste residue tank;
Described solvent naphtha is that boiling range is the C of 100～370 ℃
6～C
12hydrocarbon mixture, take can dissolved tar residue be object, as one of in carbon eight, carbon nine, carbon ten hydrocarbon mixtures or they are whole, or aromatic hydrocarbons or the non-aromatics such as toluene, dimethylbenzene.
When liquid level rising and flash tank temperature constantly raise in flash tank, open pot bottom and be exported to waste residue tank pipeline valve, treat that the interior liquid level falling while flash tank temperature of flash tank is reduced to 110～150 ℃ and stops extraction.
Specifically can be by the following technical solutions:
As shown in Figure 2, mainly comprise the following steps:
A) solvent being come by carbon five device extraction cells stripping tower reactors enters flash tank reboiler, is warming up to 115～160 ℃,
After heating, material enters solvent flashing tank, and this still is with agitator, and top is connected with solvent naphtha pipeline, and flash tank operating pressure is-0.06～-0.09MPaG, and top steams DMF steam, and bottom is extraction liquid phase stream intermittently.
B) there are heat(ing) coil or jacket pipe pattern in flash tank outside, passes into low-pressure steam and make to be incubated 110～150 ℃ in flash tank in coil pipe or chuck; There is agitator flash tank inside, continuous stirring while normally moving.
The top extraction of flash tank normal condition, intermittently stops charging in situation, opens outlet at bottom to waste residue tank (or waste residue pond) valve and starts discharging, depending on material state in flash tank.When in flash tank, liquid level rising and temperature constantly raise, show that tar accumulation is more, stop charging, start to concentrate, keep passing into quantity of steam in flash tank external heat coil pipe or jacket pipe constant, when continuing to be stirred to liquid phase simultaneously and emerging without bubble, 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 that restarts regenerated solvent.In operating process, to note observing tar situation in flash tank (avoiding because of concentrated smooth or more solvent loss and the contaminated environment of increasing of solvent of discharge that excessively cause) by visor.When tar viscosity be difficult for to be discharged more greatly or when flash distillation tank skin has tar residue, the valve that can open 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) by solvent flashing tank top extraction gas phase, first entered regeneration still condenser, and be cooled to 80～120 ℃, cooling rear material is by being pumped into solvent refining tower.
D) through the cooled material of solvent reclamation still condenser, enter solvent refining tower, 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 99% above purity, returns to 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, increased agitator, strengthened heat-transfer effect, the corresponding heat exchange area that reduced, has reduced investment;
2. whole process can realize closed-loop operation, has reduced the possibility of polymer exposure air, thereby has reduced the discharge of pollutant; Two regeneration stills when prior art is normally moved, when a still liquid level is high, just switch to another still charging, 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 must regularly open regeneration still cleaning tar, in the time of contaminated environment, also increased workman's labour intensity and occupational hazards.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. by the stirring action of agitator, strengthen flowing of material in flash tank, made the solvent better separated with tar, reduced possibility of tar accumulation simultaneously, improved the economic benefit of installing, reduced manipulation strength.
4. by increasing the pipeline of solvent naphtha, utilize solvent naphtha that remaining tar is dissolved, improved the mobility of tar, make the whole operation can automation, increased 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 standby 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
The specific embodiment
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 bottoms connect solvent refining tower 9, after solvent refining tower 9 tops connect return tank 12, return to solvent refining tower,
Before described thick solvent tank 7, be provided with flash tank 3 and reboiler 2, in flash tank, be provided with agitator 4; Described reboiler 2 connects flash tank 3, and flash tank 3 tops connect thick solvent tank 7, and flash tank 3 bottoms connect waste residue tank 5.
Described flash drum overhead is connected with solvent naphtha pipeline.
Described flash tank 3 is outside equipped with heat(ing) coil.
Described reboiler 2 bottoms are higher than flash tank charging aperture.
A) the solvent dimethyl formamide (DMF) being come by carbon five device extraction cells stripping tower reactors enters reboiler, be warming up to 120 ℃, operating pressure is-0.011MPaG, after heating, material enters flash tank, the operating pressure of flash tank is-0.066MPaG, operating temperature is 116 ℃, and top steams DMF steam, and bottom is extraction liquid phase stream intermittently.
B) flash tank outside has and in heat(ing) coil coil pipe, passes into low-pressure steam and make in flash tank 110～150 ℃ of insulations; There is agitator flash tank inside, continuous stirring while normally moving.
The top extraction of flash tank normal condition, intermittently stops charging in situation, opens outlet at bottom to waste residue tank valve and starts discharging, depending on material state in flash tank.When in flash tank, liquid level rising and temperature constantly raise, show that tar accumulation is more, stop charging, start to concentrate, keep flash tank external heat coil pipe to pass into quantity of steam constant, when continuing to be stirred to liquid phase simultaneously and emerging without bubble, 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 that restarts regenerated solvent.In operating process, to note observing tar situation in flash tank (avoiding because of concentrated smooth or more solvent loss and the contaminated environment of increasing of solvent of discharge that excessively cause) by visor.When tar viscosity be difficult for to be discharged more greatly or when flash distillation tank skin has tar residue, the valve that can open flash drum overhead connection solvent naphtha passes into solvent naphtha, continue to stir and also in coil pipe, to pass into steam, all dissolve to tar, then the solvent naphtha containing tar is drained into waste residue tank.The solvent naphtha adopting is the dish oil of ethylene unit, is C
9～C
12hydrocarbon mixture.
C) by solvent flashing tank top extraction gas phase, first entered regeneration still condenser, and be cooled to 100 ℃, cooling rear material is by being pumped into solvent refining tower.
D) through the cooled material of solvent reclamation still condenser, enter solvent refining tower, 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 99% above purity, returns to extraction cells solvent as a supplement.
Claims (9)
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 to solvent refining tower after connecting return tank, it is characterized in that:
Before described thick solvent tank, be provided with flash tank, reboiler; Described reboiler connects flash tank, and flash drum overhead connects thick solvent tank, and flash tank bottom connects waste residue tank; Flash drum overhead is provided with solvent naphtha pipeline.
2. the regenerative system of cracking c_5 separator solvent as claimed in claim 1, is characterized in that:
Described flash tank outer setting has heat(ing) coil or jacket pipe, and inside is provided with agitator.
3. the regenerative system of cracking c_5 separator solvent as claimed in claim 1, is characterized in that:
Described reboiler bottom is higher than flash tank charging aperture.
4. a renovation process for the regenerative system of the cracking c_5 separator solvent as described in one of claim 1 ~ 3, comprising:
Circulating solvent enters flash tank after reboiler heating, and it is refining that flash drum overhead extraction material enters solvent refining tower after condensation, and solvent refining tower tower reactor obtains neat solvent;
The extraction at intermittence of flash tank bottoms is to waste residue tank.
5. renovation process as claimed in claim 4, is characterized in that:
Regenerated solvent enters flash tank after reboiler is heated to 115～160 ℃.
6. renovation process as claimed in claim 4, is characterized in that:
The operating pressure of described flash tank is-0.06～-0.09MpaG;
The temperature of flash tank is 110～150 ℃.
7. renovation process as claimed in claim 4, is characterized in that:
Flash drum overhead extraction material after being cooled to 80～120 ℃ material by being pumped into solvent refining tower.
8. the renovation process as described in one of claim 4 ~ 7, is characterized in that:
When the more difficult discharge of tar viscosity or flash distillation tank skin have tar residue in flash tank, pass into solvent naphtha, continue to stir and in coil pipe or jacket pipe, pass into steam to tar all to dissolve, then the solvent naphtha containing tar is drained into waste residue tank;
Described solvent naphtha is that boiling range is the hydrocarbon mixture of the C6～C12 of 100～370 ℃.
9. renovation process as claimed in claim 8, is characterized in that:
When liquid level rising and flash tank temperature constantly raise in flash tank, open pot bottom and be exported to waste residue tank pipeline valve, treat that the interior liquid level falling while flash tank temperature of flash tank is reduced to 110～150 ℃ and stops extraction.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107875664A (en) * | 2017-12-21 | 2018-04-06 | 新疆工程学院 | Propylene propane thermal coupling Finestill energy-saving apparatus |
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 |
-
2012
- 2012-07-20 CN CN201210254374.7A patent/CN103566608B/en active Active
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 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107875664A (en) * | 2017-12-21 | 2018-04-06 | 新疆工程学院 | Propylene propane thermal coupling Finestill energy-saving apparatus |
| CN107875664B (en) * | 2017-12-21 | 2023-09-26 | 新疆工程学院 | Propylene-propane thermal coupling rectifying energy-saving device |
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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 |