CN104311740B - A kind of Petropols device removes the method for total chlorine in the most poly-carbon five - Google Patents
A kind of Petropols device removes the method for total chlorine in the most poly-carbon five Download PDFInfo
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- CN104311740B CN104311740B CN201410474456.1A CN201410474456A CN104311740B CN 104311740 B CN104311740 B CN 104311740B CN 201410474456 A CN201410474456 A CN 201410474456A CN 104311740 B CN104311740 B CN 104311740B
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Abstract
A kind of Petropols device removes the method for total chlorine in the most poly-carbon five, belongs to Petropols processing technique field.It is characterized in that, concrete technology step is: utilizes resin flash column (1) to obtain the most poly-carbon five mixed vapour containing organochlorine and delivers to the feed(raw material)inlet at dechlorination rectifying column (2) middle part；Carrying out rectification in dechlorination rectifying column (2), controlling dechlorination rectifying column (2) interior technological parameter is: dechlorination rectifying column (2) top pressure 25KPa ~ 35KPa, tower top temperature 40 DEG C ~ 55 DEG C, temperature 50 C ~ 60 DEG C, tower side, bottom temperature are at 60 DEG C ~ 90 DEG C；Tower top utilizes the most poly-carbon five collection assembly condensing reflux；Residual heavy constituent in tower reactor is carried out secondary flash by heavy constituent flash vaporization components.The present invention utilizes top gaseous phase as the charging of dechlorination rectifying column, decreases the steam consumption of tower reactor；Heavy constituent is carried out secondary flash, decreases the consumption of the most poly-carbon five, ensure that the recovery that the most poly-carbon five consumes to greatest extent.
Description
Technical field
A kind of Petropols device removes the method for total chlorine in the most poly-carbon five, belongs to Petropols processing technique field.
Background technology
At present, C 5 petroleum resin device is in addition to producing hard resin, and the most poly-carbon five of its by-product is mainly used in mediation vapour
Oil, this most poly-carbon five light oil is white clear liquid, octane number about 94, density (20 DEG C) 0.62 ~ 0.69, isopentane content: 50%
~ 66%, can be as special blended gasoline raw material.
Proving through using, automobile-used carbon five lighter hydrocarbons oil is compared with gasoline, and power does not declines and gasoline is suitable, and unit consumption compares gasoline
Declining 3% ~ 5%, tail gas declines more than 90%, and discharge reaches Europe II, Eu III standard.Finished product Vehicular light hydrocarbon oil retail price is more cheap than gasoline
More than 0.50 yuan/liter, suitable with liquefied gas price.There is economic benefit and environmental benefit, petroleum resources can be made to be able to abundant profit
With, there is wide market prospect.
The most poly-carbon five of its by-product of process units of some domestic C 5 petroleum resins is not mainly used in being in harmonious proportion light oil, but not
The actual application situation of poly-carbon five allows of no optimist.After in June, 2012, country strengthens the chloride content to product oil and detects,
Require chloride less than 40ppm.And the catalyst that at present C 5 petroleum resin device uses has containing dichloroethanes etc. is chloride
Machine thing, these chlorine-bearing compounds enter polymerization with catalyst, during device generates C 5 petroleum resin, unreacted
The chlorinated organics such as dichloroethanes will enter in the most poly-carbon five, make the chloride content of the most poly-carbon five increase, affect the most poly-carbon five
Application.Calculating with 30,000 tons of C 5 petroleum resin devices of annual output, annual amounting to, produces carbon five resin 15000 tons, wherein by-product
The most poly-carbon five reaches 13000 tons.The chloride biggest obstacle having become the application of the most poly-carbon five in the most poly-carbon five.
Summary of the invention
The technical problem to be solved in the present invention is: overcome the deficiencies in the prior art, it is provided that one can effectively remove chloride
Organic Petropols device removes the method for total chlorine in the most poly-carbon five.
The technical solution adopted for the present invention to solve the technical problems is: remove in the most poly-carbon five in this Petropols device
The method of total chlorine, concrete technology step is:
1) utilize resin flash column that C 5 petroleum resin carries out flash distillation, resin flash column tower top output temperature 150 DEG C ~
155 DEG C, the raw material delivered in the middle part of dechlorination rectifying column of the most poly-carbon five mixed vapour containing organochlorine of pressure 50KPa ~ 55KPa enters
Mouthful；
2) carrying out rectification in dechlorination rectifying column, in dechlorination rectifying column, the number of plates is 40 ~ 70 pieces, controls in dechlorination rectifying column
Technological parameter is: dechlorination rectifying tower top pressure 25KPa ~ 35KPa, tower top temperature 40 DEG C ~ 55 DEG C, temperature 50 C ~ 60 DEG C, tower side, tower
Still temperature is at 60 DEG C ~ 90 DEG C；
3) the most poly-carbon five collection assembly of dechlorination rectifying tower top gaseous phase entrance carries out condensing to collect i.e. obtaining the most poly-carbon of dechlorination five,
The top pipeline of dechlorination rectifying column connects lime set capacity of returns is resin flash column inlet amount the 1.0 of the most poly-carbon five collection assembly
~ 3.0 times；
4) the residual heavy constituent in dechlorination tower bottom of rectifying tower is delivered to heavy constituent flash vaporization components and is carried out secondary flash and return further
Receive the most poly-carbon five.
The most poly-carbon five mixed vapour containing organochlorine described in step 1 is by being located between lower several 19th ~ 35 piece of plate number
Feed(raw material)inlet enter dechlorination rectifying column, rise together with steaming gas-phase carbon 5 petroleum resin in dechlorination tower bottom of rectifying tower and with de-
Chlorine rectifying column top return liquid heat exchange on column plate.The present invention selects the raw material of the most poly-carbon five mixed vapour containing organochlorine to enter
Mouth position, really selects on the basis of chlorinity in view of C 5 petroleum resin raw material, makes overhead reflux liquid and contain
The most poly-carbon five mixed vapour that the most poly-carbon five mixed vapour raw material of organochlorine and tower reactor steam containing organochlorine can reach
Good heat exchange balance, has ensured that the most poly-carbon five can gasify risings again, continues chlorine in the chloride heavy constituent refluxed as far as possible
Content reaches feasible maximization.Ensure maximum dechlorination efficiency.
It is to deliver to dechlorination essence after dechlorination rectifying tower top gaseous phase enters condenser condensation that process is collected in condensation described in step 3
Evaporating column overhead lime set tank, control dechlorination rectifying column tower top lime set tank liquid level is 20% ~ 70%, solidifying in dechlorination rectifying column tower top lime set tank
When liquid detection chlorinity is more than 40ppm, dechlorination rectifier column reflux it is pumped back on dechlorination rectifying column the superiors column plate continue essence
Evaporate.
The process of described condenser condensation is: dechlorination rectifying tower top gaseous phase enters the condensation of tower top the first condenser, tower top
The first uncooled gas phase in condenser upper strata enters and is condensed by tower top the second condenser, and tower top the first condenser and tower top second are cold
Dechlorination rectifying column tower top lime set tank delivered to by the condensed fluid of condenser.
Described tower top the first condenser utilizes circulating water condensing, described tower top the second condenser to utilize temperature 5 DEG C ~ 6
DEG C chilled water condensation.
The process of secondary flash described in step 4 is that the residual heavy constituent in dechlorination tower bottom of rectifying tower is by dechlorination tower bottom of rectifying tower
Extraction pump is pumped to heavy constituent rectifying column and carries out flash distillation, and in heavy constituent rectifying column, technological parameter is: heavy constituent tower bottom of rectifying tower pressure
Power 70KPa ~ 100Kpa, bottom temperature 70 DEG C ~ 100 DEG C, tower reactor liquid level 50% ~ 90%；Heavy constituent rectifying tower top gaseous phase is back to
Between lower several second column plates of dechlorination rectifying column, heavy constituent tower bottom of rectifying tower residual is discharged by heavy constituent extraction pump.
Use dechlorination rectifying column and heavy constituent rectifying column double tower process, control the tower top temperature of dechlorination rectifying column, will not gather
In carbon five, lighter component carbon five carries out cutting with heavy constituent chlorinated organics and separates, the chloride restructuring of dechlorination tower bottom of rectifying tower extraction
Point, the most poly-carbon five component that overhead extraction chlorinity is qualified.The chloride heavy constituent of tower reactor extraction enters back into heavy constituent rectifying column and carries out
Secondary flash, separates the light component of carbon five in dechlorinator's tower reactor with heavy constituent further, reduces the most poly-carbon five in heavy constituent
Loss.The present invention uses the most poly-carbon five steam directly to be entered dechlorinating refined tower, liquid phase the most poly-carbon five nothing by middle part gas-phase feed mouth
Need to gasify again, saving heat energy.Top gaseous phase condensation employing fractional condensaion, first-stage condenser employing circulating water condensing, two grades
Condenser uses chilled water condensation, chilled water temperature 5 DEG C ~ 6 DEG C, and condensation effect is good, and tower top emptying loss is little.Tower reactor heavy constituent is adopted
Carrying out secondary rectification with heavy constituent flash tank, the gas phase steamed returns treating column tower reactor.Heavy constituent circulation rectification, tower reactor heavy constituent
Lose little.
Adjust dechlorination process parameter, reduce the chlorinty in the most poly-carbon five further, it is contemplated that the chlorinty in the most poly-carbon five
Below 40ppm to be down to, creates more preferable economic benefit.
The inventive method exists and organizes technological balance more, the unified realization coordinating guarantee allomeric function before and after needs.
One is the balance of resin flash column feed rate and dechlorination rectifying column processing speed；Two is dechlorination rectifying column tower top lime set tank extraction
Proportional balancing method between speed and refluxer；Three is refluxer and the changing of the most poly-carbon five mixed vapour containing organochlorine
Heat regasifies balance；Four are to maintain liquid level equilibrium in dechlorination tower bottom of rectifying tower；Five is that heavy constituent rectifying column C 5 petroleum resin returns
It is closed flat weighing apparatus.Controlling of technological balance realizes just ensureing that the continuous-stable of C 5 petroleum resin dechlorination is efficiently carried out everywhere.
Compared with prior art, the Petropols device of the present invention removes the device and method institute of total chlorine in the most poly-carbon five
Have the beneficial effect that the present invention combines the resin flash column of C 5 petroleum resin device, utilize top gaseous phase as dechlorination
The charging of rectifying column, decreases the steam consumption of tower reactor；Use heavy constituent rectifying column simultaneously, the carbon five in heavy constituent is carried out two
Secondary flash distillation, decreases the most poly-carbon five consumption in tower reactor heavy constituent, ensure that the recovery that the most poly-carbon five consumes to greatest extent；Whole
Individual design, under relatively low energy consumption and material consumption, i.e. achieves the removing of total chlorine in the most poly-carbon five.Meanwhile, the process of the present invention
After dechlorination rectifying column, in the most poly-carbon five, chloride content is down to below 40ppm, by adjusting the capacity of returns of dechlorination rectifying column,
Chloride content in the most poly-carbon five can be down to below 10ppm.
Accompanying drawing explanation
Fig. 1 is that the device used by method removing total chlorine in the most poly-carbon five in the present invention a kind of Petropols device connects knot
Structure schematic diagram.
Wherein: 1, resin flash column 2, dechlorination rectifying column 3, dechlorination rectifying column reboiler 4, heavy constituent rectifying column 5, tower
Push up the first condenser 6, tower top the second condenser 7, dechlorination rectifying column tower top lime set tank 8, dechlorination rectifier column reflux pump 9, take off
Chlorine tower bottom of rectifying tower extraction pump 10, heavy constituent extraction pump.
Detailed description of the invention
Fig. 1 is to remove the optimal enforcement of the device used by method of total chlorine in the most poly-carbon five in Petropols device of the present invention
Example, 1 pair of equipment therefor of the present invention is described further below in conjunction with the accompanying drawings.
Referring to the drawings 1: a kind of Petropols device of the present invention removes the dress used by method of total chlorine in the most poly-carbon five
Putting, including resin flash column 1, dechlorination rectifying column 2 and heavy constituent rectifying column 4, the top gaseous phase export pipeline of resin flash column 1 is even
Being connected to the feed(raw material)inlet in the middle part of dechlorination rectifying column 2, in dechlorination rectifying column 2, the number of plates is 40 ~ 70 pieces, and feed(raw material)inlet is located at lower several
Between 19 ~ 35 pieces of plate numbers.The gaseous phase outlet pipeline at the top of dechlorination rectifying column 2 connects the gas phase entrance of tower top the first condenser 5,
The top of tower top the first condenser 5 has a gaseous phase outlet and pipeline is connected to the gas phase entrance of tower top the second condenser 6, tower top
The condensate outlet of one condenser 5 and tower top the second condenser 6 is connected to dechlorination rectifying column tower top lime set tank 7；Dechlorination rectifying column
Tower top lime set tank 7 top connects air pressure blowdown piping, and dechlorination rectifying column tower top lime set tank 7 bottom conduit connects dechlorination rectifying column
Reflux pump 8, the output pipe of dechlorination rectifier column reflux pump 8 connects the two valvular pipelines of band, Qi Zhongyi respectively by threeway
The valvular pipeline of band is connected between the superiors' column plate of dechlorination rectifying column 2；By with dechlorination bottom dechlorination rectifying column 2
The pipeline of tower bottom of rectifying tower extraction pump 9 is connected to heavy constituent rectifying column 4 centre entrance, and the top gas phase of heavy constituent rectifying column 4 goes out
Mouth is connected to lower several second layer column plate middlewares of dechlorination rectifying column 2 by pipeline；The bottom of dechlorination rectifying column 2 is provided with dechlorination essence
Evaporating tower reboiler 3, set two-layer packing layer in dechlorination rectifying column 2, feed(raw material)inlet is located at the bottom of the packing layer of upper strata.
Below by specific embodiment the method for total chlorine in the most poly-carbon five that removes in Petropols device of the present invention done into
One step explanation, wherein embodiment 1 is most preferred embodiment.
Embodiment 1
1) utilize resin flash column 1 that C 5 petroleum resin carries out flash distillation, resin flash column 1 tower top output temperature 150 DEG C,
The most poly-carbon five mixed vapour containing organochlorine of pressure 50KPa delivers to the feed(raw material)inlet in the middle part of dechlorination rectifying column 2；Dechlorination rectification
In tower 2, the number of plates is 42 pieces, and feed(raw material)inlet is located on lower several 20th piece of plate number.
2) carrying out rectification in dechlorination rectifying column 2, in controlling dechlorination rectifying column 2, technological parameter is: dechlorination rectifying column 2 top pressure
30KPa, tower top temperature 45 DEG C, capacity of returns 10m3/ h, tower side temperature 55 DEG C, tower reactor Liquid level 80%, bottom temperature is 82
DEG C, tower reactor pressure is 48KPa.
3) dechlorination rectifying column 2 top gaseous phase entrance tower top the first condenser 5 condenses, and tower top the first condenser 5 upper strata is the coldest
Solidifying gas phase enters and is condensed by tower top the second condenser 6, and the condensed fluid of tower top the first condenser 5 and tower top the second condenser 6 send
To dechlorination rectifying column tower top lime set tank 7, control dechlorination rectifying column tower top lime set tank 7 liquid level 50%, dechlorination rectifying column tower top lime set
When lime set detection chlorinity is more than 40ppm in tank 7, dechlorination rectifier column reflux pump 8 return to dechlorination rectifying column 2 the superiors column plate
Upper continuation rectification, lime set capacity of returns is 1.5 times of resin flash column inlet amount.
4) the residual heavy constituent in dechlorination rectifying column 2 tower reactor is pumped to heavy constituent essence by dechlorination tower bottom of rectifying tower extraction pump 9
Evaporating tower 4 and carry out flash distillation, in heavy constituent rectifying column 4, technological parameter is: heavy constituent rectifying column 4 top pressure 49 KPa, tower reactor pressure
90KPa, bottom temperature 86 DEG C, tower reactor liquid level 82%；Heavy constituent rectifying column 4 top gaseous phase is back to lower several the of dechlorination rectifying column 2
Continuing rectification between two column plates, heavy constituent rectifying column 4 tower reactor residual is discharged by heavy constituent extraction pump 10.
Dechlorination process is carried out continuously 150h, the 1st hour, the 1.5th hour, the 5th hour, the 11st hour, the 30th hour,
60 hours, the 120th hour, the most poly-carbon of the 150th hour respectively extraction pipeline of sampling Detection dechlorination rectifying column tower top lime set tank 7
Five content, dechlorination effect continuous-stable, chlorinity be respectively 5.0ppm, 4.9ppm, 5.2ppm, 5.1ppm, 5.1ppm,
5.0ppm、4.9ppm、5.0ppm.Removing chlorinity is 200ppm former C 5 petroleum resin 5t, the matter of the most poly-carbon of final gained five
Amount is 4.87t.
Embodiment 2
1) utilize resin flash column 1 that C 5 petroleum resin carries out flash distillation, resin flash column 1 tower top output temperature 152 DEG C,
The most poly-carbon five mixed vapour containing organochlorine of pressure 52KPa delivers to the feed(raw material)inlet in the middle part of dechlorination rectifying column 2；Dechlorination rectification
In tower 2, the number of plates is 50 pieces, and feed(raw material)inlet is located on lower several 22nd piece of plate number.
2) carrying out rectification in dechlorination rectifying column 2, in controlling dechlorination rectifying column 2, technological parameter is: dechlorination rectifying column 2 top pressure
31KPa, tower top temperature 44 DEG C, capacity of returns 10m3/ h, tower side temperature 54 DEG C, tower reactor Liquid level 70%, bottom temperature is 81
DEG C, tower reactor pressure is 47.5KPa.
3) dechlorination rectifying column 2 top gaseous phase entrance tower top the first condenser 5 condenses, and tower top the first condenser 5 upper strata is the coldest
Solidifying gas phase enters and is condensed by tower top the second condenser 6, and the condensed fluid of tower top the first condenser 5 and tower top the second condenser 6 send
To dechlorination rectifying column tower top lime set tank 7, control dechlorination rectifying column tower top lime set tank 7 liquid level 50%, dechlorination rectifying column tower top lime set
When lime set detection chlorinity is more than 40ppm in tank 7, dechlorination rectifier column reflux pump 8 return to dechlorination rectifying column 2 the superiors column plate
Upper continuation rectification, lime set capacity of returns is 1.6 times of resin flash column inlet amount.
4) the residual heavy constituent in dechlorination rectifying column 2 tower reactor is pumped to heavy constituent essence by dechlorination tower bottom of rectifying tower extraction pump 9
Evaporating tower 4 and carry out flash distillation, in heavy constituent rectifying column 4, technological parameter is: heavy constituent rectifying column 4 top pressure 42KPa, tower reactor pressure 80KPa,
Bottom temperature 90 DEG C, tower reactor liquid level 79%；Heavy constituent rectifying column 4 top gaseous phase is back to lower several second column plates of dechlorination rectifying column 2
Between continue rectification, heavy constituent rectifying column 4 tower reactor residual discharged by heavy constituent extraction pump 10.
Dechlorination process is carried out continuously 150h, the 1st hour, the 1.5th hour, the 5th hour, the 11st hour, the 30th hour,
60 hours, the 120th hour, the most poly-carbon of the 150th hour respectively extraction pipeline of sampling Detection dechlorination rectifying column tower top lime set tank 7
Five content, dechlorination effect continuous-stable, chlorinity be respectively 5.0ppm, 5.1ppm, 5.0ppm, 4.9ppm, 5.1ppm,
5.0ppm、5.1ppm、5.0ppm.Removing chlorinity is 200ppm former C 5 petroleum resin 5t, the matter of the most poly-carbon of final gained five
Amount is 4.86t.
Embodiment 3
1) utilize resin flash column 1 that C 5 petroleum resin carries out flash distillation, resin flash column 1 tower top output temperature 153 DEG C,
The most poly-carbon five mixed vapour containing organochlorine of pressure 53KPa delivers to the feed(raw material)inlet in the middle part of dechlorination rectifying column 2；Dechlorination rectification
In tower 2, the number of plates is 60 pieces, and feed(raw material)inlet is located on lower several 30th piece of plate number.
2) carrying out rectification in dechlorination rectifying column 2, in controlling dechlorination rectifying column 2, technological parameter is: dechlorination rectifying column 2 top pressure
26KPa, tower top temperature 52 DEG C, capacity of returns 10m3/ h, tower side temperature 57 DEG C, tower reactor Liquid level 75%, bottom temperature is 86
DEG C, tower reactor pressure is 46KPa.
3) dechlorination rectifying column 2 top gaseous phase entrance tower top the first condenser 5 condenses, and tower top the first condenser 5 upper strata is the coldest
Solidifying gas phase enters and is condensed by tower top the second condenser 6, and the condensed fluid of tower top the first condenser 5 and tower top the second condenser 6 send
To dechlorination rectifying column tower top lime set tank 7, control dechlorination rectifying column tower top lime set tank 7 liquid level 60%, dechlorination rectifying column tower top lime set
When lime set detection chlorinity is more than 40ppm in tank 7, dechlorination rectifier column reflux pump 8 return to dechlorination rectifying column 2 the superiors column plate
Upper continuation rectification, lime set capacity of returns is 2 times of resin flash column inlet amount.
4) the residual heavy constituent in dechlorination rectifying column 2 tower reactor is pumped to heavy constituent essence by dechlorination tower bottom of rectifying tower extraction pump 9
Evaporating tower 4 and carry out flash distillation, in heavy constituent rectifying column 4, technological parameter is: heavy constituent rectifying column 4 top pressure 41 KPa, tower reactor pressure
80KPa, bottom temperature 90 DEG C, tower reactor liquid level 65%；Heavy constituent rectifying column 4 top gaseous phase is back to lower several the of dechlorination rectifying column 2
Continuing rectification between two column plates, heavy constituent rectifying column 4 tower reactor residual is discharged by heavy constituent extraction pump 10.
Dechlorination process is carried out continuously 150h, the 1st hour, the 1.5th hour, the 5th hour, the 11st hour, the 30th hour,
60 hours, the 120th hour, the most poly-carbon of the 150th hour respectively extraction pipeline of sampling Detection dechlorination rectifying column tower top lime set tank 7
Five content, dechlorination effect continuous-stable, chlorinity be respectively 5.3ppm, 5.2ppm, 5.2ppm, 5.4ppm, 5.3ppm,
5.2ppm、5.4ppm、5.3ppm.Removing chlorinity is 200ppm former C 5 petroleum resin 5t, the matter of the most poly-carbon of final gained five
Amount is 4.85t.
Embodiment 4
1) utilize resin flash column 1 that C 5 petroleum resin carries out flash distillation, resin flash column 1 tower top output temperature 150 DEG C,
The most poly-carbon five mixed vapour containing organochlorine of pressure 50KPa delivers to the feed(raw material)inlet in the middle part of dechlorination rectifying column 2；Dechlorination rectification
In tower 2, the number of plates is 40 pieces, and feed(raw material)inlet is located on lower several 19th piece of plate number.
2) carrying out rectification in dechlorination rectifying column 2, in controlling dechlorination rectifying column 2, technological parameter is: dechlorination rectifying column 2 top pressure
25KPa, tower top temperature 55 DEG C, capacity of returns 9m3/ h, tower side temperature 60 C, tower reactor Liquid level 80%, bottom temperature at 90 DEG C,
Tower reactor pressure is 48KPa.
3) dechlorination rectifying column 2 top gaseous phase entrance tower top the first condenser 5 condenses, and tower top the first condenser 5 upper strata is the coldest
Solidifying gas phase enters and is condensed by tower top the second condenser 6, and the condensed fluid of tower top the first condenser 5 and tower top the second condenser 6 send
To dechlorination rectifying column tower top lime set tank 7, control dechlorination rectifying column tower top lime set tank 7 liquid level 20%, dechlorination rectifying column tower top lime set
When lime set detection chlorinity is more than 40ppm in tank 7, dechlorination rectifier column reflux pump 8 return to dechlorination rectifying column 2 the superiors column plate
Upper continuation rectification, lime set capacity of returns is 1 times of resin flash column inlet amount.
4) the residual heavy constituent in dechlorination rectifying column 2 tower reactor is pumped to heavy constituent essence by dechlorination tower bottom of rectifying tower extraction pump 9
Evaporating tower 4 and carry out flash distillation, in heavy constituent rectifying column 4, technological parameter is: heavy constituent rectifying column 4 top pressure 40 KPa, tower reactor pressure
70KPa, bottom temperature 100 DEG C, tower reactor liquid level 50%；Heavy constituent rectifying column 4 top gaseous phase is back to the lower number of dechlorination rectifying column 2
Continuing rectification between the second column plate, heavy constituent rectifying column 4 tower reactor residual is discharged by heavy constituent extraction pump 10.
Dechlorination process is carried out continuously 150h, the 1st hour, the 1.5th hour, the 5th hour, the 11st hour, the 30th hour,
60 hours, the 120th hour, the most poly-carbon of the 150th hour respectively extraction pipeline of sampling Detection dechlorination rectifying column tower top lime set tank 7
Five content, dechlorination effect continuous-stable, chlorinity be respectively 6.1ppm, 5.9ppm, 6.1ppm, 6.0ppm, 6.1ppm,
6.0ppm、5.9ppm、6.0ppm.Removing chlorinity is 200ppm former C 5 petroleum resin 5t, the matter of the most poly-carbon of final gained five
Amount is 4.85t.
Embodiment 5
1) utilize resin flash column 1 that C 5 petroleum resin carries out flash distillation, resin flash column 1 tower top output temperature 155 DEG C,
The most poly-carbon five mixed vapour containing organochlorine of pressure 55KPa delivers to the feed(raw material)inlet in the middle part of dechlorination rectifying column 2；Dechlorination rectification
In tower 2, the number of plates is 70 pieces, and feed(raw material)inlet is located on lower several 35th piece of plate number.
2) carrying out rectification in dechlorination rectifying column 2, in controlling dechlorination rectifying column 2, technological parameter is: dechlorination rectifying column 2 top pressure
35KPa, tower top temperature 40 DEG C, capacity of returns 10m3/ h, tower side temperature 50 C, tower reactor Liquid level 80%, bottom temperature is 60
DEG C, tower reactor pressure is 50KPa.
3) dechlorination rectifying column 2 top gaseous phase entrance tower top the first condenser 5 condenses, and tower top the first condenser 5 upper strata is the coldest
Solidifying gas phase enters and is condensed by tower top the second condenser 6, and the condensed fluid of tower top the first condenser 5 and tower top the second condenser 6 send
To dechlorination rectifying column tower top lime set tank 7, control dechlorination rectifying column tower top lime set tank 7 liquid level 70%, dechlorination rectifying column tower top lime set
When lime set detection chlorinity is more than 40ppm in tank 7, dechlorination rectifier column reflux pump 8 return to dechlorination rectifying column 2 the superiors column plate
Upper continuation rectification, lime set capacity of returns is 1.5 times of resin flash column inlet amount.
4) the residual heavy constituent in dechlorination rectifying column 2 tower reactor is pumped to heavy constituent essence by dechlorination tower bottom of rectifying tower extraction pump 9
Evaporating tower 4 and carry out flash distillation, in heavy constituent rectifying column 4, technological parameter is: heavy constituent rectifying column 4 top pressure 39KPa, tower reactor pressure 70KPa,
Bottom temperature 100 DEG C, tower reactor liquid level 50%；Heavy constituent rectifying column 4 top gaseous phase is back to lower several second towers of dechlorination rectifying column 2
Continuing rectification between plate, heavy constituent rectifying column 4 tower reactor residual is discharged by heavy constituent extraction pump 10.
Dechlorination process is carried out continuously 150h, the 1st hour, the 1.5th hour, the 5th hour, the 11st hour, the 30th hour,
60 hours, the 120th hour, the most poly-carbon of the 150th hour respectively extraction pipeline of sampling Detection dechlorination rectifying column tower top lime set tank 7
Five content, dechlorination effect continuous-stable, chlorinity be respectively 4.8ppm, 4.9ppm, 4.8ppm, 4.8ppm, 5.0ppm,
4.9ppm、4.9ppm、4.8ppm.Removing chlorinity is 200ppm former C 5 petroleum resin 5t, the matter of the most poly-carbon of final gained five
Amount is 4.85t.
Comparative example 1
1) directly C 5 petroleum resin is delivered to the feed(raw material)inlet in the middle part of dechlorination rectifying column 2；
2) carrying out rectification in dechlorination rectifying column 2, in controlling dechlorination rectifying column 2, technological parameter is: dechlorination rectifying column 2 top pressure
30KPa, tower top temperature 45 DEG C, capacity of returns 10m3/ h, tower side temperature 55 DEG C, tower reactor Liquid level 80%, bottom temperature is 82
DEG C, tower reactor pressure is 48KPa；
3) dechlorination rectifying column 2 top gaseous phase entrance tower top the first condenser 5 condenses, and tower top the first condenser 5 upper strata is the coldest
Solidifying gas phase enters and is condensed by tower top the second condenser 6, and the condensed fluid of tower top the first condenser 5 and tower top the second condenser 6 send
To dechlorination rectifying column tower top lime set tank 7, control dechlorination rectifying column tower top lime set tank 7 liquid level 50%, dechlorination rectifying column tower top lime set
When lime set detection chlorinity is more than 40ppm in tank 7, dechlorination rectifier column reflux pump 8 return to dechlorination rectifying column 2 upper strata packing layer
Rectification is continued in top.
4) the residual heavy constituent in dechlorination rectifying column 2 tower reactor is pumped to heavy constituent essence by dechlorination tower bottom of rectifying tower extraction pump 9
Evaporating tower 4 and carry out flash distillation, in heavy constituent rectifying column 4, technological parameter is: heavy constituent rectifying column 4 top pressure 49 KPa, tower reactor pressure
90KPa, bottom temperature 86 DEG C, tower reactor liquid level 82%；Heavy constituent rectifying column 4 top gaseous phase is back to the lower floor of dechlorination rectifying column 2 and fills out
Continuing rectification in the middle part of the bed of material, heavy constituent rectifying column 4 tower reactor residual is discharged by heavy constituent extraction pump 10.
Dechlorination process is carried out continuously 150h, the 1st hour, the 1.5th hour, the 5th hour, the 11st hour, the 30th hour,
60 hours, the 120th hour, the most poly-carbon of the 150th hour respectively extraction pipeline of sampling Detection dechlorination rectifying column tower top lime set tank 7
Five content, dechlorination effect continuous-stable, chlorinity be respectively 22ppm, 22ppm, 21ppm, 20ppm, 18ppm, 15ppm,
12ppm、11ppm.Owing to C 5 petroleum resin does not has flash distillation to be gas phase, when charging, in dechlorination rectifying column, energy consumption increases, dechlorination
Inefficient, it is impossible to complete the dechlorination of continuous high-efficient.
Comparative example 2
1) utilize resin flash column 1 that C 5 petroleum resin carries out flash distillation, resin flash column 1 tower top output temperature 150 DEG C,
The most poly-carbon five mixed vapour containing organochlorine of pressure 50KPa delivers to the feed(raw material)inlet in the middle part of dechlorination rectifying column 2；Dechlorination rectification
In tower 2, the number of plates is 42 pieces, and feed(raw material)inlet is located on lower several 20th piece of plate number.
2) carrying out rectification in dechlorination rectifying column 2, in controlling dechlorination rectifying column 2, technological parameter is: dechlorination rectifying column 2 top pressure
30KPa, tower top temperature 45 DEG C, capacity of returns 10m3/ h, tower side temperature 55 DEG C, tower reactor Liquid level 80%, bottom temperature is 82
DEG C, tower reactor pressure is 48KPa.
3) dechlorination rectifying column 2 top gaseous phase entrance tower top the first condenser 5 condenses, and tower top the first condenser 5 upper strata is the coldest
Solidifying gas phase enters and is condensed by tower top the second condenser 6, and the condensed fluid of tower top the first condenser 5 and tower top the second condenser 6 send
To dechlorination rectifying column tower top lime set tank 7, control dechlorination rectifying column tower top lime set tank 7 liquid level 50%, dechlorination rectifying column tower top lime set
When lime set detection chlorinity is more than 40ppm in tank 7, dechlorination rectifier column reflux pump 8 return to dechlorination rectifying column 2 the superiors column plate
Upper continuation rectification, lime set capacity of returns is 1.5 times of resin flash column inlet amount.The chloride heavy constituent of dechlorination rectifying column 2 tower reactor is direct
Discharge.
Owing to not carrying out secondary flash, being just discharged in the case of chloride heavy constituent content is relatively low, removing chlorinity is
200ppm former C 5 petroleum resin 5t, the quality of the most poly-carbon of final gained five is 3.5t.Significant loss is serious.
Comparative example 3
Basic craft course and implementation condition are with embodiment 1, except that feed(raw material)inlet is located at lower several 10th piece of plate number
On.
Dechlorination process is carried out continuously 150h, the 1st hour, the 1.5th hour, the 5th hour, the 11st hour, the 30th hour,
60 hours, the 120th hour, the most poly-carbon of the 150th hour respectively extraction pipeline of sampling Detection dechlorination rectifying column tower top lime set tank 7
Five content, dechlorination effect continuous-stable, chlorinity be respectively 7.1ppm, 60.9ppm, 5.2ppm, 70ppm, 65.1ppm,
50.0ppm、40.9ppm、25.0ppm.Due to feed(raw material)inlet position change, between condensed fluid capacity of returns and the amount of gaseous component
Condenserization balance is destroyed, it is impossible to carry out the stable dechlorination of continuous high-efficient again.
The above, be only presently preferred embodiments of the present invention, is not the restriction that the present invention makees other form, appoints
What those skilled in the art changed possibly also with the technology contents of the disclosure above or be modified as equivalent variations etc.
Effect embodiment.But every without departing from technical solution of the present invention content, the technical spirit of the foundation present invention is to above example institute
Any simple modification, equivalent variations and the remodeling made, still falls within the protection domain of technical solution of the present invention.
Claims (2)
1. a Petropols device removes the method for total chlorine in the most poly-carbon five, it is characterised in that concrete technology step is:
1) utilize resin flash column (1) that C 5 petroleum resin carries out flash distillation, resin flash column (1) tower top output temperature 150 DEG C ~
155 DEG C, the most poly-carbon five mixed vapour containing organochlorine of pressure 50KPa ~ 55KPa deliver to dechlorination rectifying column (2) middle part former
Material entrance；
2) carrying out rectification in dechlorination rectifying column (2), dechlorination rectifying column (2) the interior number of plates is 40 ~ 70 pieces, controls dechlorination rectifying column
(2) interior technological parameter is: dechlorination rectifying column (2) top pressure 25KPa ~ 35KPa, tower top temperature 40 DEG C ~ 55 DEG C, tower side temperature 50 C ~
60 DEG C, bottom temperature is at 60 DEG C ~ 90 DEG C；
3) the most poly-carbon five collection assembly of dechlorination rectifying column (2) top gaseous phase entrance carries out condensing to collect i.e. obtaining the most poly-carbon of dechlorination five,
The top pipeline connection of dechlorination rectifying column (2) has the lime set capacity of returns of the most poly-carbon five collection assembly to be resin flash column inlet amount
1.0 ~ 3.0 times；
4) the residual heavy constituent in dechlorination rectifying column (2) tower reactor is delivered to heavy constituent flash vaporization components and is carried out secondary flash and reclaim further
The most poly-carbon five；
The most poly-carbon five mixed vapour containing organochlorine described in step 1 is former by be located between lower several 19th ~ 35 piece of plate number
Material entrance enter dechlorination rectifying column (2), rise together with steaming gas-phase carbon 5 petroleum resin in dechlorination rectifying column (2) tower reactor and with
The heat exchange on column plate of dechlorination rectifying column (2) overhead reflux liquid；
It is to deliver to dechlorination essence after dechlorination rectifying column (2) top gaseous phase enters condenser condensation that process is collected in condensation described in step 3
Evaporate column overhead lime set tank (7), control dechlorination rectifying column tower top lime set tank (7) liquid level 20% ~ 70%, dechlorination rectifying column tower top lime set
When tank (7) interior lime set detection chlorinity is more than 40ppm, dechlorination rectifier column reflux pump (8) returns to dechlorination rectifying column (2) and go up most
Rectification is continued on layer column plate；
The process of described condenser condensation is: dechlorination rectifying column (2) top gaseous phase enters tower top the first condenser (5) condensation, tower
Push up the uncooled gas phase in the first condenser (5) upper strata to enter by tower top the second condenser (6) condensation, tower top the first condenser (5)
Dechlorination rectifying column tower top lime set tank (7) is delivered to the condensed fluid of tower top the second condenser (6)；
The process of secondary flash described in step 4 is that the residual heavy constituent in dechlorination rectifying column (2) tower reactor is by dechlorination tower bottom of rectifying tower
Extraction pump (9) is pumped to heavy constituent rectifying column (4) and carries out flash distillation, and heavy constituent rectifying column (4) interior technological parameter is: heavy constituent rectification
Tower (4) tower reactor pressure 70KPa ~ 100Kpa, bottom temperature 70 DEG C ~ 100 DEG C, tower reactor liquid level 50% ~ 90%；Heavy constituent rectifying column (4)
Top gaseous phase is back between lower several second column plates of dechlorination rectifying column (2), and heavy constituent rectifying column (4) tower reactor residual is adopted by heavy constituent
Go out pump (10) to discharge.
A kind of carry out Petropols device removes the method for total chlorine, its feature in the most poly-carbon five
It is: described tower top the first condenser (5) utilizes circulating water condensing, described tower top the second condenser (6) to utilize temperature 5 DEG C
The chilled water condensation of ~ 6 DEG C.
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| CN201410474456.1A CN104311740B (en) | 2014-09-18 | 2014-09-18 | A kind of Petropols device removes the method for total chlorine in the most poly-carbon five |
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| CN201410474456.1A CN104311740B (en) | 2014-09-18 | 2014-09-18 | A kind of Petropols device removes the method for total chlorine in the most poly-carbon five |
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| CN110229377B (en) * | 2019-06-28 | 2021-06-22 | 濮阳班德路化学有限公司 | Dechlorination method of carbon five solvent |
| CN113801372A (en) * | 2021-03-26 | 2021-12-17 | 广东新华粤树脂科技有限公司 | Carbon five-carbon nine-copolymerization petroleum resin non-polymerized mixture carbon five-separation method |
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