CN109876485A - Acetic acid recovery is from backheat rectifier unit and method - Google Patents
Acetic acid recovery is from backheat rectifier unit and method Download PDFInfo
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- CN109876485A CN109876485A CN201910178637.2A CN201910178637A CN109876485A CN 109876485 A CN109876485 A CN 109876485A CN 201910178637 A CN201910178637 A CN 201910178637A CN 109876485 A CN109876485 A CN 109876485A
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention discloses a kind of acetic acid recoveries from backheat rectifier unit, it include: rectifying column, reboiler and phase-splitter, it is characterized in that, a compressor is equipped between the top of the distillation column steam (vapor) outlet and the thermal source inlet of the reboiler, the thermal source outlet of the reboiler is connected with the material inlet of one second heat exchanger, for overhead vapours further to be cooled down, the material outlet of second heat exchanger connects the phase-splitter, the first outlet of the phase-splitter is extraction mouth, and second outlet is connected with the tower top of the rectifying column.The present invention uses clean electrical energy drive compressor, and overhead vapours compression heating has been saved the use of a large amount of steam and recirculated water, while saving a large amount of operating cost as the heat source of tower reactor in a manner of mechanical compression.By taking the rectifying column of acetic acid recovery workshop section in the PTA device of somewhere as an example, about 61% operating cost can be saved every year compared with using the prior art, under same operating condition, meet the requirement of national energy-saving environmental protection policy.
Description
Technical field
The invention belongs to solvent recovery technical fields, and in particular to a kind of acetic acid recovery is from backheat rectifier unit and method.
Background technique
PTA (p-phthalic acid) is the important source material for synthesizing polyester, is using paraxylene as raw material, and acetic acid is solvent,
It is generated under certain temperature and pressure with air oxidation.There is water generation in the reaction process, it, must to guarantee going on smoothly for reaction
Water must be removed, while recycling design acetic acid.Acetic acid recovery unit is a part crucial in PTA production, is directly related to oxygen
Change the stabilization of water content in unit circulation acetic acid, and then influences the oxidation reaction of paraxylene.
Acetic acid and water do not form azeotropic mixture, and its relative volatility separate using conventional distillation method required close to 1
Theoretical cam curve and reflux ratio are larger, therefore steam consumption is very big.By taking the PTA device of 600,000 t/a scales as an example, acetic acid
The 0.5MPa quantity of steam of the rectifying column consumption of recovery unit reaches 95t/h or so.To reduce the energy consumption during separation acetic acid and water,
The method that existing apparatus mostly uses azeotropic distillation.Entrainer and material liquid enter azeotropy rectification column together, the water in distillation process
Be distilled out of with entrainer, after cooling with entrainer multi_layer extraction, entrainer return tower in, water discharge, in tower reactor i.e. obtain
Acetic acid.Acetic acid and water are separated compared with the method for conventional distillation using azeotropic distillation method, save steam to a certain extent
Dosage.But the energy consumption during acetic acid recovery is still within higher level.With phasing out for China's coal-burning boiler,
Steam price rises steadily, it would be highly desirable to which it is less to seek a kind of steam consumption quantity, the lower recovery method of operating cost.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of acetic acid recoveries of low energy consumption from backheat rectifying
Device and method.
The present invention is achieved by the following technical solutions:
A kind of acetic acid recovery is from backheat rectifier unit, comprising: rectifying column, reboiler and phase-splitter, which is characterized in that described
A compressor, the thermal source outlet of the reboiler are equipped between the top of the distillation column steam (vapor) outlet and the thermal source inlet of the reboiler
It is connected with the material inlet of one second heat exchanger, for overhead vapours further to be cooled down, the material of second heat exchanger
Outlet connects the entrance of the phase-splitter, which is equipped with extraction mouth and refluxing opening, and the extraction mouth connection extraction pump is described
Refluxing opening connects reflux pump, and the outlet of the reflux pump is connected with the tower top of the rectifying column.
In the above-mentioned technical solutions, one is equipped between the tower bottoms outlet and the tower bottoms import of the tower of the rectifying column
First Heat Exchanger heats the kettle material of the tower for supplementing steam.
In the above-mentioned technical solutions, a spray port is additionally provided on the phase-splitter, the spray port is connected with a spray pump
It connects, inlet and outlet of the outlet of the spray pump respectively with the compressor is connected.
In the above-mentioned technical solutions, the compressor is screw compressor, Roots Compressor or centrifugal compressor.
It in the above-mentioned technical solutions, further include a circulating pump, the entrance of the circulating pump connects the tower reactor of the rectifying column,
The outlet of the circulating pump connects the material inlet of the reboiler, and the reboiler is horizontal tube falling film reboiler.
In the above-mentioned technical solutions, the flow of the First Heat Exchanger supplement steam is 1~5t/h.
In the above-mentioned technical solutions, the pressure ratio of the compressor is 1.1~6.
In the above-mentioned technical solutions, the inlet steam temperature of the compressor be 80~100 DEG C, outlet temperature be 110~
140℃。
Application of the above-mentioned acetic acid recovery from backheat rectifier unit in PTA production.
A method of using above-mentioned acetic acid recovery from backheat rectifier unit recovery of acetic acid characterized by comprising will contain
The material of acetic acid and water introduces the feed inlet of the rectifying column, and the overhead vapours of the tower enters the compressor, heats up through compression
Afterwards as the heat source of tower reactor reboiler, the temperature of reboiler heat source is 110~140 DEG C, and the overhead vapours after exchanging heat enters the
Two heat exchangers further cool down, and the material inlet temperature of the second heat exchanger is 110~140 DEG C, and outlet temperature is 75~90 DEG C, so
Enter phase-splitter multi_layer extraction afterwards and obtain oily phase and water phase, wherein oil is mutually back to tower top through reflux pump, and water phase is by tower reactor pumping section
Divide extraction.
The advantages and benefits of the present invention are:
1. the present invention uses clean electrical energy drive compressor, overhead vapours is compressed into heating in a manner of mechanical compression and is made
For the heat source of tower reactor, the use of a large amount of steam and recirculated water has been saved, while having saved a large amount of operating cost.
2. using horizontal tube falling film reboiler realize overhead vapours and tower bottoms heat exchange, take full advantage of overhead vapours by
Saturated vapor becomes the heat of transformation of lime set, and the thermal efficiency is higher.
3. by taking the rectifying column of acetic acid recovery workshop section in the PTA device of somewhere as an example, compared with using the prior art, same operating condition
The operating cost that about 61% can be saved every year down, meets the requirement of national energy-saving environmental protection policy.
Detailed description of the invention
Fig. 1 is the acetic acid recovery of the embodiment of the present invention 1 from the general flow chart of backheat distillation process.
Wherein, 1 is compressor, and 2 be reboiler, and 3 be the second heat exchanger, and 4 be phase-splitter, and 5 be First Heat Exchanger, and 6 be essence
Tower is evaporated, 7 be extraction pump, and 8 be reflux pump, and 9 be spray pump, and 10 be circulating pump, and 11 pump for tower reactor, and LS is steam inlet, and LC is to steam
Vapor outlet, CWS are circulation water inlet, and CWR is circulating water outlet.
Specific embodiment
In order to enable those skilled in the art to better understand the solution of the present invention, in the following with reference to the drawings and specific embodiments into
One step illustrates technical solution of the present invention.
Embodiment 1
A kind of acetic acid recovery is from backheat rectifier unit, comprising: rectifying column 4, reboiler 2 and phase-splitter 6, wherein reboiler
For horizontal tube falling film reboiler.A Roots Compressor 1 is equipped between the top of the distillation column steam (vapor) outlet and the thermal source inlet of reboiler,
Pressure ratio is 1.6, and the thermal source outlet of reboiler is connected with the material inlet of one second heat exchanger 5, and overhead vapours is further cold
But, the material outlet of the second heat exchanger connects phase-splitter, which is equipped with extraction mouth and refluxing opening, extraction mouth connection extraction pump
7, refluxing opening connects reflux pump 8, and the outlet of reflux pump is connected with the tower top of rectifying column.A spray port is additionally provided on phase-splitter,
Spray port is connected with a spray pump 9, is communicated with filter on the export pipeline of spray pump.The outlet of spray pump respectively with compression
The inlet and outlet of machine is connected.One first heat exchange is equipped between the tower bottoms outlet and the tower bottoms import of the tower of rectifying column
Device 3 heats the kettle material of the tower for supplementing steam.The device further includes a circulating pump 10, and the entrance of circulating pump connects essence
Evaporate the tower reactor of tower, the material inlet of the outlet connection reboiler of the circulating pump.
The charging of rectifying column comes from PTA device oxidation section, and group becomes acetic acid 41%, and water 55%, methyl acetate 4% is (
For mass percent), the entrainer used is n-butyl acetate.50 DEG C of material is introduced to the feed inlet of rectifying column, which is
Atmospheric tower, tower top temperature are 95 DEG C, and the gas phase azeotropic mixture that entrainer and water and some organic impurities (methyl acetate) are formed is from tower
Top steams.Overhead vapours enters compressor, and 113 DEG C of boil down to, the heat source after the saturated vapor of 160kPa as tower reactor reboiler
(outlet of compressor is superheated steam, therefore extracts the cold process liquid in phase-splitter using spray pump to spray compressor
Steam in inlet and outlet is to eliminate overheat), tower bottoms is pumped into reboiler through circulation and exchanges heat with overhead vapours.Because of overhead vapours
The heat of release is less than the thermic load of tower reactor, and the steam heat tower reactor of 1.7t need to be supplemented through First Heat Exchanger.It exchanges heat with tower bottoms
Overhead vapours (condensed is saturated liquid) afterwards enters the second heat exchanger and is cooled further to 90 DEG C, subsequently into phase-splitter point
The isolated oil phase of layer and water phase, wherein oil is mutually back to tower top through reflux pump, and water phase is produced by tower reactor pump portion.Tower bottom obtains
To dewatered acetate products through 11 extraction of tower reactor pump.
Embodiment 2
A kind of acetic acid recovery is from backheat rectifier unit, comprising: rectifying column 4, reboiler 2 and phase-splitter 6, wherein reboiler
For horizontal tube falling film reboiler.A screw compressor 1 is equipped between the top of the distillation column steam (vapor) outlet and the thermal source inlet of reboiler,
Pressure ratio is that pressure ratio is 5.4, and the thermal source outlet of reboiler is connected with the material inlet of one second heat exchanger 5, by overhead vapours into
One step is cooling, and the material outlet of the second heat exchanger connects phase-splitter, which is equipped with extraction mouth and refluxing opening, extraction mouth connection
Extraction pump 7, refluxing opening connects reflux pump 8, and the outlet of reflux pump is connected with the tower top of rectifying column.A spray is additionally provided on phase-splitter
Mouth is drenched, spray port is connected with a spray pump 9, and the outlet of spray pump is connected with the inlet and outlet of compressor respectively.In essence
It evaporates and is equipped with a First Heat Exchanger 3 between the tower bottoms outlet of tower and the tower bottoms import of the tower, heat the tower for supplementing steam
Kettle material.The device further includes a circulating pump 10, the tower reactor of the entrance connection rectifying column of circulating pump, the outlet of the circulating pump
Connect the material inlet of reboiler.
The charging of rectifying column comes from PTA device oxidation section, and group becomes acetic acid 51%, and water 47%, methyl acetate 3% is (
For mass percent), use entrainer for isobutyl acetate.40 DEG C of material is introduced to the feed inlet of the rectifying column, the tower
For atmospheric tower, tower top temperature is 82 DEG C, the gas phase azeotropic mixture that entrainer and water and some organic impurities (methyl acetate) are formed from
Tower top steams.Overhead vapours enters the compressor, and 132 DEG C of boil down to, tower reactor reboiler is used as after the saturated vapor of 550kPa
Heat source (outlet of compressor is superheated steam, therefore extracts the cold process liquid in phase-splitter using spray pump and spray
Steam in compressor inlet and outlet is to eliminate overheat), tower bottoms is pumped into reboiler through circulation and exchanges heat with overhead vapours.Because of tower
The heat for pushing up steam release is less than the thermic load of tower reactor, and the steam heat tower reactor of 5t need to be supplemented through First Heat Exchanger.With tower bottoms
Overhead vapours (condensed is saturated liquid) after heat exchange enters the second heat exchanger and is cooled further to 79 DEG C, subsequently into split-phase
Device multi_layer extraction obtains oily phase and water phase, wherein oil is mutually back to tower top through reflux pump, and water phase is produced by tower reactor pump portion.Tower
Bottom obtains dewatered acetate products through 11 extraction of tower reactor pump.
Embodiment 3
A kind of acetic acid recovery is from backheat rectifier unit, comprising: rectifying column 4, reboiler 2 and phase-splitter 6, wherein reboiler
For horizontal tube falling film reboiler.A Roots Compressor 1 is equipped between the top of the distillation column steam (vapor) outlet and the thermal source inlet of reboiler,
Pressure ratio is 2.5, and the thermal source outlet of reboiler is connected with the material inlet of one second heat exchanger 5, and overhead vapours is further cold
But, the material outlet of the second heat exchanger connects phase-splitter, which is equipped with extraction mouth and refluxing opening, extraction mouth connection extraction pump
7, refluxing opening connects reflux pump 8, and the outlet of reflux pump is connected with the tower top of rectifying column.A spray port is additionally provided on phase-splitter,
Spray port is connected with a spray pump 9, and the outlet of spray pump is connected with the inlet and outlet of compressor respectively.In rectifying column
It is equipped with a First Heat Exchanger 3 between tower bottoms outlet and the tower bottoms import of the tower, the tower reactor of the tower is heated for supplementing steam
Material.The device further includes a circulating pump 10, and the tower reactor of the entrance connection rectifying column of circulating pump, the outlet connection of the circulating pump is again
Boil the material inlet of device.
The charging of rectifying column comes from PTA device oxidation section, and organizing becomes acetic acid 41%, water 52%, and methyl acetate 4% is right
Dimethylbenzene 3% (being mass percent), uses entrainer for propyl acetate.By 70 DEG C of material introduce the rectifying column into
Material mouth, the tower are atmospheric tower, and tower top temperature is 85 DEG C, entrainer and water and some organic impurities (methyl acetate, paraxylene)
The gas phase azeotropic mixture of formation is steamed from tower top.Overhead vapours enters the compressor, and 125 DEG C of boil down to, the saturation of 255kPa is steamed
As the heat source of tower reactor reboiler after vapour, tower bottoms is pumped up in reboiler to exchange heat with overhead vapours.Because overhead vapours discharges
Heat be less than tower reactor thermic load, need to through First Heat Exchanger supplement 4.1t steam heat tower reactor.After tower bottoms heat exchange
Overhead vapours (condensed is saturated liquid) enters the second heat exchanger and is cooled further to 80 DEG C, subsequently into phase-splitter layering point
From obtain it is oily mutually and water phase, wherein oil is mutually back to tower top, and aqueous portion produces.Tower bottom obtains dewatered acetate products.
It is compared with the operating cost of the prior art of same thermic load: (according to local concrete condition, according to steam price
200 yuan/ton, 0.7 yuan of electricity price/degree, 0.2 yuan/m of cooling water price3, annual to be calculated by operation in 8000 hours)
By comparison it is found that method of the invention can save the use of a large amount of steam and recirculated water, production is greatly reduced
The expense of operation, year operating cost can save about 61% compared with prior art.
Illustrative description has been done to the present invention above, it should explanation, the case where not departing from core of the invention
Under, any simple deformation, modification or other skilled in the art can not spend the equivalent replacement of creative work equal
Fall into protection scope of the present invention.
Claims (10)
1. a kind of acetic acid recovery is from backheat rectifier unit, comprising: rectifying column, reboiler and phase-splitter, which is characterized in that the essence
It evaporates and is equipped with a compressor, the thermal source outlet of the reboiler between the overhead vapours outlet of tower and the thermal source inlet of the reboiler
It is connected with the material inlet of one second heat exchanger, for overhead vapours further to be cooled down, the material of second heat exchanger
Outlet connects the phase-splitter, which is equipped with extraction mouth and refluxing opening, the one extraction pump of extraction mouth connection, the reflux
Mouth one reflux pump of connection, the outlet of the reflux pump is connected with the tower top of the rectifying column.
2. rectifier unit according to claim 1, which is characterized in that in tower bottoms outlet and the tower of the rectifying column
It is equipped with a First Heat Exchanger between tower bottoms import, the kettle material of the tower is heated for supplementing steam.
3. rectifier unit according to claim 1, which is characterized in that a spray port is additionally provided on the phase-splitter, it is described
Spray port is connected with a spray pump, and the outlet of the spray pump is connected with the inlet and outlet of the compressor respectively.
4. rectifier unit according to claim 1, which is characterized in that the compressor is screw compressor, roots-type
Compressor or centrifugal compressor.
5. rectifier unit according to claim 1, which is characterized in that further include a circulating pump, the entrance of the circulating pump
The tower reactor of the rectifying column is connected, the outlet of the circulating pump connects the material inlet of the reboiler, and the reboiler is transverse tube
Falling-film reboiler.
6. rectifier unit according to claim 2, which is characterized in that the flow of the First Heat Exchanger supplement steam is 1
~5t/h.
7. rectifier unit according to claim 1, which is characterized in that the pressure ratio of the compressor is 1.1~6.
8. rectifier unit according to claim 1, which is characterized in that the inlet steam temperature of the compressor be 80~
100 DEG C, outlet temperature is 110~140 DEG C.
9. application of the rectifier unit in PTA production as described in claim 1~7.
10. utilizing the method for the rectifier unit recovery of acetic acid as described in claim 1~7 characterized by comprising vinegar will be contained
The material of acid and water introduces the feed inlet of the rectifying column, and the overhead vapours of the tower enters the compressor, and pressure ratio is 1.1~
6, the heat source after compression heating as tower reactor reboiler, the temperature of reboiler heat source is 110~140 DEG C, the tower after exchanging heat
Top steam enters the second heat exchanger and further cools down, and the material inlet temperature of the second heat exchanger is 110~140 DEG C, outlet temperature
Degree is 75~90 DEG C, obtains oily phase and water phase subsequently into phase-splitter multi_layer extraction, wherein oil is mutually back to tower through reflux pump
Top, water phase are produced by tower reactor pump portion.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201910178637.2A CN109876485A (en) | 2019-03-11 | 2019-03-11 | Acetic acid recovery is from backheat rectifier unit and method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910178637.2A CN109876485A (en) | 2019-03-11 | 2019-03-11 | Acetic acid recovery is from backheat rectifier unit and method |
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Cited By (3)
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| CN112902686A (en) * | 2021-01-26 | 2021-06-04 | 河北易高生物能源有限公司 | Furfural primary distillation tower steam recycling method |
| CN113617051A (en) * | 2021-10-12 | 2021-11-09 | 天津乐科节能科技有限公司 | Energy-saving rectifying device and method and application |
| CN114192085A (en) * | 2021-12-15 | 2022-03-18 | 珠海谦信新材料有限公司 | Heat recycling system and method for acetic acid process production device |
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