CN106478341A - Device and the technique of C-4-fraction is separated using binary mixed solvent - Google Patents

Device and the technique of C-4-fraction is separated using binary mixed solvent Download PDF

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Publication number
CN106478341A
CN106478341A CN201610880181.0A CN201610880181A CN106478341A CN 106478341 A CN106478341 A CN 106478341A CN 201610880181 A CN201610880181 A CN 201610880181A CN 106478341 A CN106478341 A CN 106478341A
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distillation column
extractive distillation
stripper
extracting rectifying
stripping
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CN201610880181.0A
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董令闻
郑李斌
叶昊天
韩志忠
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Dalian University of Technology
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Dalian University of Technology
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00Purification; Separation; Use of additives
    • C07C7/005Processes comprising at least two steps in series
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00Purification; Separation; Use of additives
    • C07C7/04Purification; Separation; Use of additives by distillation
    • C07C7/05Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds
    • C07C7/08Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds by extractive distillation
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention provides a kind of employing binary mixed solvent separates the device of C-4-fraction and technique, device includes extractive distillation column, extracting rectifying tower top condenser, extractive distillation column return tank, extractive distillation column reflux pump, extracting rectifying bottom of towe reboiler, extracting rectifying tower bottoms pump, stripper, stripping overhead condenser, stripper return tank, stripper reflux pump, stripping tower bottom reboiler, stripping tower bottoms pump and lean solvent cooler carry out four separation of carbon using technique of the present invention, the relative volatility being greatly improved between butylene and butane, improve solvent selectivity, reduce solvent/charge ratio, reduce bottom temperature, reduce tower reactor thermic load, realize energy-saving purpose.

Description

Device and the technique of C-4-fraction is separated using binary mixed solvent
Technical field
The invention belongs to C-4-fraction separation field in petrochemical industry, be related to a kind of employing phenol, water two end number mixing molten Agent separation of extractive distillation butylene and the technique of butane.Particularly as be on the basis of existing common process, using extraction rectifying method Separate butylene butane system.Wherein, extractant selects phenol, the binary mixed solvent of water, and butylene purity reaches after purification More than 99.0%.
Background technology
Butylene is close to 1 with butane relative volatility, it is difficult to separated using the method for conventional distillation.At present, industrial conventional Extracting rectifying carries out the separation of butylene and butane, and its principle is to add a kind of polar solvent in C-4-fraction, to increase butylene Relative volatility and between butane, realizes the separation of butylene and butane.This method stable operation, low production cost, therefore exist Refinery C four is most widely used in separating.
In four separation process of carbon, solvent nature will directly affect the separating effect of extracting rectifying, be increase butylene and butane it Between relative volatility, the solvent for being adopted is typically all polar solvent with electrophilic group.
Industrial conventional solvent has mixture of acetonitrile, 1-METHYLPYRROLIDONE, MEK and N- N-formyl morpholine N etc..But Carry out there is solvent/charge ratio during carbon four is detached greatly using above-mentioned solvent, the phenomenon such as bottom temperature height, cause to separate The problems such as journey solvent loss is big, high-temperature position energy consumption is higher.
A kind of method that patent CN101417913A provides use multiple mixed solvent separation of extractive distillation butylene and butane, The invention using ionic liquid, salt, MEK and N- N-formyl morpholine N multicomponent mixture as solvent, separated go out butylene pure Degree is up to 98.0%, but stripper bottom temperature is higher, and required thermal source is higher ranked, and running intermediate ion loss of liquid is relatively Greatly, cause separation process energy consumption, material consumption higher.
Content of the invention
For butylene and butane is efficiently separated, the energy-saving of four separation process of carbon is realized, propose one kind and adopt two end number mixing The new technology of solvent separation C-4-fraction, the relative volatility being remarkably improved in C-4-fraction between butylene and butane, while Dissolubility and the selectivity of solvent is improved, so as to reduce solvent/charge ratio, reduces extractive distillation column and regeneration stripper kettle temperature Degree, reduces tower reactor thermic load.
For achieving the above object, to propose a kind of two end number mixing for four cut of extracting distillation separation C molten for the present invention Agent, the consisting of of the solvent:Phenol 70~95%, water 5~30%.Phenol and water are mixed in proportion institute of the present invention is obtained The binary mixed solvent that states.
Using four cut of binary mixed solvent extracting distillation separation C of the present invention, the phase between butylene and butane can be improved To volatility, reduce solvent/charge ratio, solvent selectivity is improved, reduce the bottom temperature of extractive distillation column and stripper, reduce Tower reactor thermic load, so as to reduce operating cost, realizes energy-saving purpose.
Technical scheme:
A kind of employing binary mixed solvent separates the device of C-4-fraction, cold including extractive distillation column, extracting rectifying tower top Condenser, extractive distillation column return tank, extractive distillation column reflux pump, extracting rectifying bottom of towe reboiler, extracting rectifying tower bottoms pump, vapour Stripper, stripping overhead condenser, stripper return tank, stripper reflux pump, stripping tower bottom reboiler, stripping tower bottoms pump and lean Solvent cooler;Extracting rectifying tower top outlet is connected with extracting rectifying tower top condenser tube journey entrance, and extracting rectifying tower top is condensed The outlet of device tube side is connected with extractive distillation column return tank entrance, and the outlet of extractive distillation column return tank is pumped into extractive distillation column backflow Mouth is connected;The discharging point two-way connection of extractive distillation column reflux pump liquid phase:(1) extractive distillation column reflux pump liquid phase one tunnel of discharging and extraction Take rectifying tower top entrance to be connected;(2) extractive distillation column reflux pump liquid phase discharges another road for butane product;Extracting rectifying bottom of towe liquid Mutually discharging point two-way connection:(1) one tunnel of extracting rectifying bottom of towe liquid phase discharging is connected with extracting rectifying bottom of towe reboiler tube-side inlet, The outlet of extracting rectifying bottom of towe reboiler tube side is connected with extracting rectifying bottom of towe entrance;(2) discharging of extracting rectifying bottom of towe liquid phase is another Road is connected with extracting rectifying tower bottoms pump intake, and extracting rectifying tower bottoms pump discharge is connected with stripper charging aperture;Stripping tower top Outlet is connected with stripping tower top condenser tube journey entrance, and stripping tower top condenser tube journey is exported and stripper return tank entrance phase Even, the outlet of stripper return tank is connected with stripper backflow pump intake;One tunnel of stripper reflux pump discharging heads into mouth with stripper It is connected, another road is butylene product;Stripping tower bottom is exported a road and is connected with stripping tower bottom reboiler tube-side inlet, stripping tower bottom weight The tube side outlet of boiling device is connected with stripping tower bottom entrance;Stripping tower bottom is exported another road and is connected with stripping tower bottoms pump intake, stripping Tower bottoms pump discharge is connected with lean solvent cooler tube-side inlet, and the outlet of lean solvent cooler tube side is entered with extractive distillation column solvent Material mouth is connected.
A kind of method that employing binary mixed solvent separates C-4-fraction, step are as follows:
C-4-fraction is added by the middle part of extractive distillation column, and binary mixed solvent is added by the top of extractive distillation column, tower Top extraction butane cut, enters extractive distillation column return tank, extractive distillation column after the condensation cooling of extracting rectifying tower top condenser In return tank, through extractive distillation column reflux pump, a part of liquid is produced as butane liquid as overhead reflux, another part liquid Product go out device;Using 1.0MPag steam as thermal source, bottom of towe produces the solvent rich solution containing butylene to extracting rectifying bottom of towe reboiler, Stripper is pumped to through extracting rectifying tower bottoms.Stripping overhead extraction butene fraction, through stripping after overhead condenser condensation cooling Stripper return tank is entered, through stripper reflux pump, a part of liquid is as overhead reflux, another for liquid in stripper return tank Partially liq goes out device as butylene product;, using 1.0MPag steam as thermal source, bottom of towe extraction is lean molten for stripping tower bottom reboiler Agent is recycled to extractive distillation column top through stripping after tower bottoms pump, lean solvent cooler.
Extractive distillation column operating parameter:Tower top temperature is 45~55 DEG C, and column bottom temperature is 125~140 DEG C, and operating pressure is 0.45~0.55MPag, theoretical cam curve are 150~170, reflux ratio 2~4.
Stripper operating parameter:Tower top temperature is 45~55 DEG C, and column bottom temperature is 140~160 DEG C, and operating pressure is 0.35 ~0.45MPag, theoretical cam curve are 40~60, reflux ratio 2~5.
Described binary mixed solvent is the mixture of phenol and water;Mass percent of the phenol in binary mixed solvent Content is 70~95%, and remaining is water.
Beneficial effects of the present invention:The present invention adopts phenol, the binary mixed solvent separation of extractive distillation butylene of water and fourth The technique of alkane, more existing common process, product purity is high, solvent is more relatively low than required thermal source grade during little, solvent reclamation.
Description of the drawings
Fig. 1 is the process flow diagram for separating C-4-fraction using binary mixed solvent.
In figure:1 extractive distillation column;2 extracting rectifying tower top condensers;3 extractive distillation column return tanks;4 extractive distillation columns are returned Stream pump;5 extracting rectifying bottom of towe reboilers;6 extracting rectifying tower bottoms pumps;7 strippers;8 stripping overhead condensers;9 strippers are returned Stream tank;10 stripper reflux pumps;11 stripping tower bottom reboilers;12 stripping tower bottoms pumps;13 lean solvent coolers.
Specific embodiment
Below in conjunction with the accompanying drawings and technical scheme, the specific embodiment of the present invention is further illustrated.
The present invention is achieved through the following technical solutions:
C-4-fraction is added by the middle part of extractive distillation column 1, and binary mixed solvent is added by the top of extractive distillation column 1, Overhead extraction butane cut, enters extractive distillation column return tank 3, extraction essence after the condensation cooling of extracting rectifying tower top condenser 2 , through extractive distillation column reflux pump 4, used as overhead reflux, another part liquid is used as fourth for a part of liquid to evaporate liquid in tower return tank Alkane product goes out device;Using 1.0MPag steam as thermal source, bottom of towe produces the solvent containing butylene to extracting rectifying bottom of towe reboiler 5 Rich solution, delivers to stripper 7 through extracting rectifying tower bottoms pump 6.The top of stripper 7 extraction butene fraction, cold through stripping overhead condenser 8 Stripper return tank 9 is entered after solidifying cooling, through stripper reflux pump 10, a part of liquid is used as tower for liquid in stripper return tank Top backflow, another part liquid go out device as butylene product;Stripping tower bottom reboiler 11 is using 1.0MPag steam as warm Source, bottom of towe extraction lean solvent are recycled to 1 top of extractive distillation column through stripping after tower bottoms pump 12, lean solvent cooler 13.
Embodiment:
By taking certain four separation process of carbon as an example, using technique of the present invention.C-4-fraction inlet amount is 10t/h, charging group Become:Propane 0.08%, propylene 0.02%, iso-butane 44.1%, normal butane 15%, 1- butylene 16%, isobutene 0.35%, trans- 2- butylene 14.6%, cis-2-butene 9.5%, 1,3-butadiene 0.35%;Solvent/charge ratio is 10 (mass ratioes), mixed solvent Measure as 100t/h, solvent consists of phenol 75%, water 25%.Extractive distillation column number of theoretical plate is 165, C-4-fraction feed entrance point For the 84th block of plate, feed location of mixed solvent is the 12nd block of plate, and operating pressure is 0.5MPag, and extracting rectifying tower top produced quantity is 6t/h, in extraction product, butane content controls more than 98.2%.Stripper number of theoretical plate is 45, the position of solvent feed containing butylene For the 25th block of plate, operating pressure is 0.4MPag, and stripping tower top produced quantity is 3.6t/h, and butene content control in extraction product exists More than 99.0%.
For ease of the technical advantage of the present invention is described, will be contrasted with existing solvent using technique of the present invention, two As shown in table 1, tower operating parameter is as shown in table 2 to plant each stream stock composition in the result of calculation of technique.
Table 1 is respectively flowed in contrast with stock group
2 tower operating parameter of table is contrasted
Comparing result shows that, using phenol of the present invention, aqueous mixtures as solvent, extracting distillation separation C four evaporates Point, compared with existing dicyandiamide solution, extracting rectifying tower reactor constitutes the butylene purity (without solvent) and can reach 99.82%, improves fourth Alkene purity 2.18%, solvent ratio are 10, it is possible to decrease solvent compares 16.7%, and reduces extractive distillation column and stripper tower reactor temperature Degree, reduces tower reactor thermic load, adds up to and reduces tower reactor thermic load 9.6%, effectively realizes energy-saving purpose.

Claims (3)

1. a kind of employing binary mixed solvent separates the device of C-4-fraction, it is characterised in that the device include extractive distillation column, Extracting rectifying tower top condenser, extractive distillation column return tank, extractive distillation column reflux pump, extracting rectifying bottom of towe reboiler, extraction Rectifying tower reactor liquid pump, stripper, stripping overhead condenser, stripper return tank, stripper reflux pump, stripping tower bottom reboiler, Stripping tower bottoms pump and lean solvent cooler;Extracting rectifying tower top outlet is connected with extracting rectifying tower top condenser tube journey entrance, The outlet of extracting rectifying tower top condenser tube journey is connected with extractive distillation column return tank entrance, and extractive distillation column return tank is exported and extraction Take rectifier column reflux pump intake to be connected;The discharging point two-way connection of extractive distillation column reflux pump liquid phase:(1) extractive distillation column reflux pump One tunnel of liquid phase discharging heads into mouth with extractive distillation column and is connected;(2) extractive distillation column reflux pump liquid phase discharges another road for butane product Product;The discharging point two-way connection of extracting rectifying bottom of towe liquid phase:(1) one tunnel of extracting rectifying bottom of towe liquid phase discharging and extracting rectifying bottom of towe weight Boiling device tube-side inlet is connected, and the outlet of extracting rectifying bottom of towe reboiler tube side is connected with extracting rectifying bottom of towe entrance;(2) extracting rectifying Another road of bottom of towe liquid phase discharging is connected with extracting rectifying tower bottoms pump intake, and extracting rectifying tower bottoms pump discharge is fed with stripper Mouth is connected;Stripping tower top outlet is connected with stripping tower top condenser tube journey entrance, and stripping tower top condenser tube journey is exported and stripping Tower return tank entrance is connected, and the outlet of stripper return tank is connected with stripper backflow pump intake;One tunnel of stripper reflux pump discharging Mouth is headed into stripper to be connected, another road is butylene product;Stripping tower bottom exports a road and stripping tower bottom reboiler tube-side inlet It is connected, the outlet of stripping tower bottom reboiler tube side is connected with stripping tower bottom entrance;Stripping tower bottom exports another road with stripping tower bottoms Pump intake be connected, stripping tower bottoms pump discharge be connected with lean solvent cooler tube-side inlet, lean solvent cooler tube side outlet and Extractive distillation column solvent feed mouth is connected.
2. a kind of method that employing binary mixed solvent separates C-4-fraction, it is characterised in that step is as follows:
C-4-fraction is added by the middle part of extractive distillation column, and binary mixed solvent is added by the top of extractive distillation column, overhead extraction Butane cut, enters extractive distillation column return tank, liquid in extractive distillation column return tank after the cooling of extracting rectifying tower top condenser Body goes out device as overhead reflux, another part liquid as butane product through extractive distillation column reflux pump, a part of liquid;Extraction Rectifying bottom reboiler is taken using 1.0MPag steam as thermal source, bottom of towe produces the solvent rich solution containing butylene, through extractive distillation column Kettle liquid is pumped to stripper;Stripping overhead extraction butene fraction, enters stripper return tank through stripping after overhead condenser cooling, In stripper return tank, through stripper reflux pump, used as overhead reflux, another part liquid is used as butylene for a part of liquid for liquid Product goes out device;, using 1.0MPag steam as thermal source, bottom of towe extraction lean solvent is through stripping tower bottoms pump for stripping tower bottom reboiler After lean solvent cooler, recycle to extractive distillation column top;
Extractive distillation column operating parameter:Tower top temperature is 45~55 DEG C, and column bottom temperature is 125~140 DEG C, and operating pressure is 0.45 ~0.55MPag, theoretical cam curve are 150~170, reflux ratio 2~4;
Stripper operating parameter:Tower top temperature be 45~55 DEG C, column bottom temperature be 140~160 DEG C, operating pressure be 0.35~ 0.45MPag, theoretical cam curve are 40~60, reflux ratio 2~5.
3. method according to claim 2, it is characterised in that described binary mixed solvent is the mixing of phenol and water Thing;Mass percentage content of the phenol in binary mixed solvent is 70~95%, and remaining is water.
CN201610880181.0A 2016-10-09 2016-10-09 Device and the technique of C-4-fraction is separated using binary mixed solvent Withdrawn CN106478341A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108237136A (en) * 2017-12-30 2018-07-03 山东恒力新能源工程有限公司 Three-level counter-current extraction coal-tar residue device and its processing method
CN109179542A (en) * 2018-11-13 2019-01-11 重庆华峰化工有限公司 Ethylene glycol, the Distallation systm of diethylene glycol and distillation technique in polyalcohol waste liquid
CN109867582A (en) * 2019-04-11 2019-06-11 山东东明石化集团有限公司 After a kind of removing ether in carbon four light dydrocarbon heavy constituent method
CN114618181A (en) * 2022-03-17 2022-06-14 北京道思克矿山装备技术有限公司 System and method for recycling hydrocyanic acid in pentenenitrile synthesis reaction

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108237136A (en) * 2017-12-30 2018-07-03 山东恒力新能源工程有限公司 Three-level counter-current extraction coal-tar residue device and its processing method
CN108237136B (en) * 2017-12-30 2023-08-15 山东恒力新能源工程有限公司 Three-stage countercurrent extraction device for coal tar residues and treatment method thereof
CN109179542A (en) * 2018-11-13 2019-01-11 重庆华峰化工有限公司 Ethylene glycol, the Distallation systm of diethylene glycol and distillation technique in polyalcohol waste liquid
CN109179542B (en) * 2018-11-13 2023-11-24 重庆华峰化工有限公司 Distillation system and distillation process for glycol and diethylene glycol in polyol waste liquid
CN109867582A (en) * 2019-04-11 2019-06-11 山东东明石化集团有限公司 After a kind of removing ether in carbon four light dydrocarbon heavy constituent method
CN114618181A (en) * 2022-03-17 2022-06-14 北京道思克矿山装备技术有限公司 System and method for recycling hydrocyanic acid in pentenenitrile synthesis reaction
CN114618181B (en) * 2022-03-17 2023-12-08 北京道思克矿山装备技术有限公司 System and method for recycling hydrocyanic acid in pentenenitrile synthesis reaction

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