CN101450908B - Fractional condensation and regeneration method of dimethylformamide as extracting solvent for cracking carbon 5 - Google Patents
Fractional condensation and regeneration method of dimethylformamide as extracting solvent for cracking carbon 5 Download PDFInfo
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Abstract
The invention discloses a method for dephlegmation regeneration of extracting solvent dimethyl formamide for cracking C5 step by step, and belongs to the technical field of cracking C5 fraction separating method. In order to solve the problem that when solvent is regenerated, water is added to cause acceleration of hydrolysis of dimethylformamide in the prior art, the invention provides a regeneration method for removing C5 hydrocarbon, water, DCPD and colloid by rectification and step condensation methods, which comprises: a solvent regenerating kettle separates heavy components such as the colloid in the solvent to be regenerated; gas phase materials steamed out enter a decompression rectifying tower; and dimethylformamide carried by gas phase materials flowing out from the top of the tower is condensed firstly through a first condenser or a dephlegmator, and then C5 hydrocarbon and water in the gas phase materials are condensed and extracted in a second condenser; materials flowing out from the solvent regenerating kettle and the bottom of a refining column enter a residue releasing tank, undergo further solvent claim and are discharged. The solvent regeneration method does not have the problems of solvent hydrolysis, tower blockage, etc., and is easy to operate.
Description
Technical field
The present invention relates to a kind of renovation process of cracked, C 5 fraction extraction solvent dimethyl formamide, more particularly, the present invention relates to a kind of renovation process that utilizes the dimethyl formamide of fractional condensation.
Background technology
Diolefins such as isoprene, cyclopentadiene and m-pentadiene are rich in a considerable amount of C5 fractions of by-product in the C5 fraction in the process of petroleum cracking system ethene.These diolefin chemical property are active, are important chemical material.Because petroleum hydrocarbon cracking raw materials, cracking severity and separation degree is different, diolefin content is different in the cracked C 5 fraction, and total content is between 40～60%.Therefore, separate and utilize C5 fraction to improving the economic benefit of ethylene unit, the comprehensive utilization petroleum resources have far reaching significance.
Cracked C 5 fraction contain more than 20 kind of boiling point close, easily form the component of azeotrope each other, from wherein isolating the higher C 5 diene of comprehensive utilization value, technology is comparatively complicated.
In order to produce highly purified isoprene product, generally adopt the two-section extraction rectificating method in the prior art, the existing employed extraction solvent of industrialized cracked C 5 fraction separation method has dimethyl formamide (DMF), acetonitrile etc.For example in carbon five separation process of Beijing Chemical Research Institute's exploitation, at first utilize the raw materials pretreatment unit that carbon Wuyuan material is carried out pre-treatment, remove wherein carbon fourth class light constituent and most of alkynes, make the cyclopentadiene dimerization become dicyclopentadiene, in pre-weight-removing column, remove heavy constituent such as m-pentadiene; Use DMF to make extraction solvent then, in first extraction cells, remove alkane and monoolefine in the cracked C 5 fraction, make chemical grade isoprene; Remove wherein alkynes and cyclopentadiene in second extraction cells, alkynes mainly is crotonylene and valylene; In the another one unit, produce m-pentadiene product and dicyclopentadiene product by rectifying; Subsidiary at last solvent recovery unit.Obviously, this separation process is long, equipment is many, the energy consumption height, especially second extraction cells exists problems: (1) is in such two-section extraction rectificating method, operating equipment is more, the energy consumption of second extraction cells is very high, needs strict operation, and the simmer down to operation in some equipment of (2) alkynes brings unsafe factor, there is black bits latch up phenomenon in (3) second extraction cells, solvent recovery unit has a large amount of colloids, and is difficult to cleaning, and (4) solvent-oil ratio is big, increase production cost, had problem of environmental pollution simultaneously.In solvent recovery unit, adopt water azeotropic treating tower to reclaim solvent, at first will treat the heavy constituent such as pressure reducing and steaming colloid in the solvent reclamation jar of regenerated solvent, the formed logistics of gas phase enters water azeotropic treating tower, in this tower, add entry, make water and dicyclopentadiene form azeotrope, the azeotropic boiling point is 97 ℃, like this dicyclopentadiene and solvent DMF is separated.Owing to add entry, make the solvent DMF hydrolysis generate dimethylamine and formic acid, formic acid promotes solvent to quicken hydrolysis again, causes solvent loss and stops up tower and pipeline.
In order to improve above-mentioned carbon five separation process, the Beijing Chemical Research Institute has proposed the one-section abstraction separation process in Chinese patent the 01136383.5th and No. 02131463.2, wherein adopt and select hydrogenation and removing alkynes, has shortened flow process like this.Although this flow process has been omitted second section extraction cells, energy consumption and cost have been reduced.In this process, also need the solvent dimethyl formamide that recycles is regenerated.
Therefore, in order to overcome existing solvent reclamation existing problems, need a kind of renovation process that can avoid the hydrolysis of extraction solvent dimethyl formamide of exploitation.
Summary of the invention
The present invention utilizes water and dicyclopentadiene azeotropic separation dicyclopentadiene and adds the problem that the entry meeting impels the dimethyl formamide hydrolysis for what solve that prior art exists when the extraction solvent dimethyl formamide is regenerated, proposed a kind of renovation process that can avoid the hydrolysis of extraction solvent dimethyl formamide.
Concrete technical scheme is as follows.
The fractional condensation and regeneration method of the dimethylformamide as extracting solvent for cracking carbon 5 that the present invention proposes may further comprise the steps:
(1) needs regenerated extraction solvent dimethyl formamide to enter the solvent reclamation still, extract gaseous stream out from regeneration still top, extract impure liquid stream from the lower end out through underpressure distillation;
(2) gaseous stream from the solvent reclamation still enters solvent treatment tower middle and upper part, comprise carbon five hydrocarbon through rectification under vacuum from what cat head came out, the gaseous stream of water and dimethyl formamide at first through first condenser or segregative dephlegmator with the dimethyl formamide condensation, the stream portions of first condenser or segregative dephlegmator condensation refluxes, remainder turns back to the solvent reclamation still, or the logistics of first condenser or segregative dephlegmator condensation all refluxes, uncooled part enters carbon five hydrocarbon and the water of second condenser with carbon five hydrocarbon and water-cooled coalescence extraction condensation in first condenser or the segregative dephlegmator, and second condenser connects vacuum system;
(3) the impure liquid stream of extracting out from solvent reclamation still lower end enters and has the residue toilet-cleaning jar that stirs and heat, the gaseous stream that steams from residue toilet-cleaning jar top enters solvent treatment tower middle and lower part, and residue toilet-cleaning jar bottom is discharged and contained carbon five dimers and gelationus logistics;
(4) logistics of solvent treatment tower bottom extraction enters the residue toilet-cleaning jar, the dimethyl formamide of regenerating from the middle and lower part extraction of solvent treatment tower.
Preferably, the tower top pressure of described solvent treatment tower is 0.005MPa～0.015MPa, and tower top temperature is 70 ℃～90 ℃, and tower still pressure is 0.008MPa～0.025MPa, and tower still temperature is 85 ℃～110 ℃.
Theoretical plate number and reflux ratio for described solvent treatment tower are not particularly limited, and those skilled in the art know that number of theoretical plate is big more, reach identical separation purpose, and needed reflux ratio is more little, and is as the same on the contrary.And, need the composition of regenerated solvent also the separation and the recovery of solvent to be exerted an influence.When carbon five hydrocarbon, water, carbon five dimers and the colloid that contains in the need regenerated solvent was higher, needed number of theoretical plate of solvent treatment tower and/or reflux ratio were also higher.During for the logistics of partial reflux first condenser or segregative dephlegmator condensation, those skilled in the art can select reflux ratio and quantity of reflux according to industrial practical situation, and this is not had special requirement, can certainly adopt whole backflows.All refluxing makes separating effect better, but energy consumption is not necessarily best, therefore needs to weigh the factor of each side in practical condition.
Pressure and temperature to the solvent reclamation still does not have special requirement, and is low more with pressure, and the temperature of regeneration still is low more, and high more with pressure, temperature is high more.This solvent reclamation still is also arranged in existing industrial installation, therefore it is not limited especially.For example pressure generally is controlled at 0.005MPa～0.015MPa, and temperature is generally 80 ℃～100 ℃.The residue toilet-cleaning jar is also arranged in the industrial installation, therefore it is not limited especially.
In the present invention, mentioned carbon five dimers mainly are meant isoprene and m-pentadiene dimer, isoprene, m-pentadiene and cyclopentadiene codimers between any two separately, these dimers can further generate polymers such as tripolymer, the tetramer again, thereby form described colloid.
The renovation process of dimethylformamide as extracting solvent for cracking carbon 5 of the present invention is applicable in the cracking c_5 separation process that the content to dicyclopentadiene in the regenerated solvent do not require.In the flow process of the two-section extraction separating cracked carbon 5 fraction that has industry now, the regenerated solvent at first adds in second extraction cells, therefore to the dicyclopentadiene content requirement in the regenerated solvent less than 0.2 quality %, otherwise regenerated solvent adds to the requirement that the cyclopentadiene content that can cause in the circulating solvent in the isoprene product can not be less than 1ppm.But, method for regenerating solvent of the present invention is applicable to one-section abstraction separation process that proposes in Chinese patent the 01136383.5th and No. 02131463.2 and the cracked, C 5 fraction separation method that proposes below, and described cracked, C 5 fraction separation method may further comprise the steps:
(1) the cracking c_5 raw material enters pre-lightness-removing column middle part, the light constituent that comprises carbon four and alkynes through reactive distillation processes from the extraction of pre-lightness-removing column cat head, the logistics of pre-lightness-removing column tower still extraction enters pre-weight-removing column middle part, comprise the logistics of isoprene through reactive distillation processes from the extraction of pre-weight-removing column cat head, comprise the logistics of m-pentadiene from the extraction of pre-weight-removing column tower still;
(2) the described logistics that comprises isoprene enters the extraction tower middle part, extraction solvent enters from extraction tower top, through the extracting rectifying process, the raffinate that comprises C 5 alkane and monoolefine from the extraction of extraction tower cat head, enter Analytic Tower from the logistics of tower still extraction, from the isoprene logistics of Analytic Tower cat head extraction based on isoprene, the logistics of resolving the extraction of Tata still loops back extraction tower through resolving;
(3) the isoprene logistics from the extraction of Analytic Tower cat head enters the weight-removing column middle part, from weight-removing column cat head extraction isoprene product, comprises the logistics of dicyclopentadiene through reactive distillation processes from the extraction of weight-removing column tower still;
Described reactive distillation processes is meant that in rectifying initial ring pentadiene dimerization becomes the reaction of dicyclopentadiene.
Described cracked, C 5 fraction separation method further comprises step:
(4) logistics of weight-removing column tower still extraction merges with the logistics of pre-weight-removing column tower still extraction, enter decarburization five towers, comprise the logistics of carbon five hydrocarbon from decarburization five column overhead extraction through reactive distillation processes, enter the dicyclopentadiene treating tower from the logistics of decarburization five Tata still extraction, make with extra care Tata still side line extraction dicyclopentadiene product through rectifying from dicyclopentadiene, the logistics that comprises carbon five hydrocarbon of decarburization five column overhead extraction enters the m-pentadiene treating tower, makes with extra care Tata still side line extraction m-pentadiene product through rectifying from m-pentadiene.
In the present invention, there is no particular limitation to each Rectification Column's Theoretical Plate Number and concrete operations condition, those skilled in the art can select suitable number of theoretical plate and operational condition according to practical situation, can be by changing the purpose of separating that number of theoretical plate, feed rate and backflow recently reach each tower.Form for given logistics, the boiling point of this logistics is determined under the certain pressure, therefore can change temperature by changing pressure, and for example tower top temperature and tower still temperature etc. are to satisfy demand of practical production.For reactive distillation processes, in order to help the generation of cyclopentadiene dimerization reaction, the determining of parameter will help carrying out as much as possible dimerization reaction, for example selects higher reflux ratio, long dwell time in the tower and helps temperature that dimerization reaction takes place etc.Determining for a person skilled in the art of these parameters is easily.
Preferably, but be not limited to, described pre-lightness-removing column has 80～140 number of theoretical plates, and reflux ratio is 5～20, and tower top temperature is 40～60 ℃.Described pre-weight-removing column has 80～180 number of theoretical plates, and reflux ratio is 10～30, and tower top temperature is 40～60 ℃.Described weight-removing column has 80～180 number of theoretical plates, and reflux ratio is 10～30, and tower top temperature is 40～60 ℃.Described decarburization five towers have 40～100 number of theoretical plates, and reflux ratio is 5～20, and tower top temperature is 40～60 ℃.
In described cracked, C 5 fraction separation method, can from the extraction pipeline of resolving the Tata still, extract out continuously or off and on partly and need go regeneration by the regenerated extraction solvent, the solvent after the regeneration adds in the extraction solvent continuously or off and on.
In existing two-section extraction separating cracked carbon 5 fraction flow process, because the regenerated solvent at first circulates and adds in second extraction cells, utilize method of extraction that the cyclopentadiene in the isoprene is removed less than 1ppm (quality), so just require cyclopentadiene and dicyclopentadiene content in the regenerated solvent very low, for example respectively less than 1ppm (quality) and 0.2%, otherwise can not make cyclopentadiene in the product isoprene less than 1ppm (quality) through second extraction process.In the one-section abstraction sepn process, because weight-removing column has the effect that reactive distillation removes cyclopentadiene, therefore cyclopentadiene in the regenerated solvent and dicyclopentadiene content are not required, can contain them.
Because extraction solvent dimethyl formamide fractional condensation and regeneration method of the present invention does not make water and dicyclopentadiene azeotropic principle, does not need deliberately to add entry to regenerative process, can not increase the disadvantageous effect of solvent loss and obstruction tower.And easier by contrast operation, operator do not need to consider that azeotropic is formed and the add-on of water.Thereby the advantage of method for regenerating solvent of the present invention is conspicuous.
Description of drawings
Fig. 1 is the synoptic diagram of expression cracked, C 5 fraction extraction solvent dimethyl formamide fractional condensation and regeneration method of the present invention.
Nomenclature:
1, solvent reclamation still; 2, residue toilet-cleaning jar; 3, solvent treatment tower; 4, first condenser or segregative dephlegmator; 5, second condenser; 6, return tank.
Embodiment
Further describe the present invention with reference to the accompanying drawings, the fractional condensation and regeneration method of the dimethylformamide as extracting solvent for cracking carbon 5 that the present invention proposes may further comprise the steps:
(1) needs regenerated extraction solvent dimethyl formamide to enter solvent reclamation still 1, extract gaseous stream out from solvent reclamation still 1 top, extract impure liquid stream from the lower end out through underpressure distillation; The temperature of solvent reclamation still 1 generally is controlled at 80 ℃～100 ℃, and pressure generally is controlled at 0.005MPa～0.015MPa; Whole solvent regeneration system is communicated with and is communicated with vacuum system by second condenser;
(2) gaseous stream from solvent reclamation still 1 enters solvent treatment tower 3 middle and upper parts, for example 1/3 enter solvent treatment tower 3 from top, above this opening for feed, stay some column plates to help with dimethyl formamide and carbon five, water separately, the tower top pressure of described solvent treatment tower is 0.005MPa～0.015MPa, tower top temperature is 70 ℃～90 ℃, tower still pressure is 0.008MPa～0.025MPa, tower still temperature is 85 ℃～110 ℃, the gaseous stream that comes out from cat head through rectification under vacuum comprises carbon five hydrocarbon, water and dimethyl formamide and a spot of dicyclopentadiene of carrying, because the boiling point of dimethyl formamide and dicyclopentadiene is more much higher than the boiling point of carbon five hydrocarbon and water, therefore this gaseous stream can be at first through first condenser or segregative dephlegmator 4 with dimethyl formamide and dicyclopentadiene condensation, the stream portions of first condenser or segregative dephlegmator 4 condensations refluxes, remainder turns back to further recovery dimethyl formamide wherein of solvent reclamation still 1, or the logistics of first condenser or segregative dephlegmator 4 condensations all refluxes, uncooled part in first condenser or the segregative dephlegmator 4, mainly be carbon five hydrocarbon and water, enter carbon five hydrocarbon and the water of second condenser 5 with carbon five hydrocarbon and water-cooled coalescence extraction condensation, carbon five hydrocarbon and water stratification can separate, second condenser 5 connects vacuum system, and the pressure of vacuum system is determining the pressure of total system; Because system pressure is lower with carbon five hydrocarbon boiling points than low,, can partly be extracted into vacuum pump and discharge, but the content of carbon five hydrocarbon in solvent is lower, can not produce big influence so the condensation of carbon five hydrocarbon possibility is incomplete;
(3) extract impure liquid stream out from solvent reclamation still 1 lower end and enter the residue toilet-cleaning jar 2 that has stirring and heating, the gaseous stream that steams from residue toilet-cleaning jar 2 tops enters solvent treatment tower 3 middle and lower parts with further recovery dimethyl formamide wherein, and residue toilet-cleaning jar 2 bottoms are discharged and contained dicyclopentadiene, carbon five dimers and gelationus logistics; The dimer that described carbon five dimers for example are dimer, m-pentadiene and the cyclopentadiene of isoprene and cyclopentadiene, the dimer of isoprene self etc., described colloid is meant the polymkeric substance that molecular weight is higher, polymer of carbon five diolefine etc. for example, a small amount of polymerization takes place and produces in carbon five hydrocarbon inevitably in carbon five separation production process;
(4) logistics of solvent treatment tower 3 bottom extraction enters residue toilet-cleaning jar 2, the dimethyl formamide of regenerating from the 3 middle and lower part extraction of solvent treatment tower, for example, below the side line extraction mouth of dimethyl formamide, stay some column plates to help dimethyl formamide and colloid are separated from 1/3 or 1/4 place of solvent treatment tower bottom.
Embodiment 1
Utilizing renovation process of the present invention to handle needs regenerated cracked, C 5 fraction extraction solvent dimethyl formamide, needs the regenerated dimethyl formamide mainly composed as follows:
| Component | Form weight % |
| Carbon five hydrocarbon | 0.4 |
| Water | 0.30 |
| Dimethyl formamide DMF | 89.66 |
?
| Dicyclopentadiene DCPD | 5.21 |
| Carbon five dimer X3 | 1.89 |
| Colloid | 2.54 |
(1) needs regenerated extraction solvent dimethyl formamide to enter solvent reclamation still 1, extract gaseous stream out from solvent reclamation still 1 top, extract impure liquid stream from the lower end out through underpressure distillation; The temperature of solvent reclamation still 1 is controlled at 90 ℃, and pressure-controlling is at 0.008MPa;
(2) the solvent treatment tower has 50 blocks of column plates, enter the 16th block of column plate of solvent treatment tower 3 from the gaseous stream of solvent reclamation still 1, the tower top pressure of described solvent treatment tower is 0.008MPa, tower top temperature is 70 ℃, tower still pressure is 0.015MPa, tower still temperature is 95 ℃, the gaseous stream that comes out from cat head through rectification under vacuum through first condenser or segregative dephlegmator 4 with heavy constituent condensations such as dimethyl formamides, the temperature of first condenser or segregative dephlegmator 4 is 25 ℃, the logistics of first condenser or segregative dephlegmator 4 condensations all refluxes, uncooled part in first condenser or the segregative dephlegmator 4, mainly be carbon five hydrocarbon and water, enter second condenser 5, with the part of carbon five hydrocarbon and water-cooled coalescence extraction condensation, second condenser 5 connects vacuum system under about 0 ℃;
(3) extract impure liquid stream out from solvent reclamation still 1 lower end and enter the residue toilet-cleaning jar 2 that has stirring and heating, the gaseous stream that steams from residue toilet-cleaning jar 2 tops enters the 45th block of column plate of solvent treatment tower 3 with further recovery dimethyl formamide wherein, and residue toilet-cleaning jar 2 bottoms are discharged and contained dicyclopentadiene, carbon five dimers and gelationus logistics;
(4) logistics of solvent treatment tower 3 bottoms extraction enters residue toilet-cleaning jar 2, from the 40th dimethyl formamide that the column plate extraction was regenerated of solvent treatment tower 3.
Claims (2)
1. the fractional condensation and regeneration method of a dimethylformamide as extracting solvent for cracking carbon 5 is characterized in that, described fractional condensation and regeneration method may further comprise the steps:
(1) needs regenerated extraction solvent dimethyl formamide to enter the solvent reclamation still, extract gaseous stream out from regeneration still top, extract impure liquid stream from the lower end out through underpressure distillation;
(2) gaseous stream from the solvent reclamation still enters solvent treatment tower middle and upper part, comprise carbon five hydrocarbon through rectification under vacuum from what cat head came out, the gaseous stream of water and dimethyl formamide at first through first condenser or segregative dephlegmator with the dimethyl formamide condensation, the stream portions of first condenser or segregative dephlegmator condensation refluxes, remainder turns back to the solvent reclamation still, or the logistics of first condenser or segregative dephlegmator condensation all refluxes, uncooled part enters carbon five hydrocarbon and the water of second condenser with carbon five hydrocarbon and water-cooled coalescence extraction condensation in first condenser or the segregative dephlegmator, and second condenser connects vacuum system;
(3) the impure liquid stream of extracting out from solvent reclamation still lower end enters and has the residue toilet-cleaning jar that stirs and heat, the gaseous stream that steams from residue toilet-cleaning jar top enters solvent treatment tower middle and lower part, and residue toilet-cleaning jar bottom is discharged and contained carbon five dimers and gelationus logistics;
(4) logistics of solvent treatment tower bottom extraction enters the residue toilet-cleaning jar, the dimethyl formamide of regenerating from the middle and lower part extraction of solvent treatment tower.
2. the fractional condensation and regeneration method of dimethylformamide as extracting solvent for cracking carbon 5 as claimed in claim 1, it is characterized in that, the tower top pressure of described solvent treatment tower is 0.005MPa～0.015MPa, tower top temperature is 70 ℃～90 ℃, tower still pressure is 0.008MPa～0.025MPa, and tower still temperature is 85 ℃～110 ℃.
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| CN102021015B (en) * | 2009-09-10 | 2013-05-01 | 中国石油化工集团公司 | Tar dissolving method for extracting C4 hydrocarbon and C5 hydrocarbon by using dimethylformamide as solvent |
| CN102040533B (en) * | 2009-10-20 | 2014-08-06 | 中国石油化工股份有限公司 | Regeneration method for N,N-dimethyl formamide and application thereof |
| CN103570576B (en) * | 2012-07-20 | 2016-06-15 | 中国石油化工集团公司 | A kind of cracking c_5 tripping device circulating solvent regeneration system rapidly and method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3510405A (en) * | 1967-11-11 | 1970-05-05 | Nippon Zeon Co | Isoprene purification process |
| 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 |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3510405A (en) * | 1967-11-11 | 1970-05-05 | Nippon Zeon Co | Isoprene purification process |
| 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 |
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