CN109851501A - Ethyl acetate integration system is for tower - Google Patents
Ethyl acetate integration system is for tower Download PDFInfo
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- CN109851501A CN109851501A CN201910213290.0A CN201910213290A CN109851501A CN 109851501 A CN109851501 A CN 109851501A CN 201910213290 A CN201910213290 A CN 201910213290A CN 109851501 A CN109851501 A CN 109851501A
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- Prior art keywords
- tower
- section
- redistributor
- internals
- ethyl acetate
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- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 230000010354 integration Effects 0.000 title claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 47
- 238000000605 extraction Methods 0.000 claims abstract description 40
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 48
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 37
- 235000019441 ethanol Nutrition 0.000 claims description 18
- 239000002608 ionic liquid Substances 0.000 claims description 16
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 15
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 15
- 229910000831 Steel Inorganic materials 0.000 claims description 10
- 239000010959 steel Substances 0.000 claims description 10
- -1 polytetrafluoroethylene Polymers 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 239000007792 gaseous phase Substances 0.000 claims description 7
- 238000004154 testing of material Methods 0.000 claims description 7
- 239000000945 filler Substances 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- 239000004033 plastic Substances 0.000 claims description 2
- 229920003023 plastic Polymers 0.000 claims description 2
- 238000009833 condensation Methods 0.000 claims 1
- 230000005494 condensation Effects 0.000 claims 1
- XUCNUKMRBVNAPB-UHFFFAOYSA-N fluoroethene Chemical compound FC=C XUCNUKMRBVNAPB-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 12
- 230000008569 process Effects 0.000 abstract description 8
- 239000002351 wastewater Substances 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 21
- 239000003054 catalyst Substances 0.000 description 20
- 229940058401 polytetrafluoroethylene Drugs 0.000 description 11
- 239000000047 product Substances 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 5
- 239000012071 phase Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000032050 esterification Effects 0.000 description 3
- 238000005886 esterification reaction Methods 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 238000005194 fractionation Methods 0.000 description 3
- 230000008929 regeneration Effects 0.000 description 3
- 238000011069 regeneration method Methods 0.000 description 3
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 230000009977 dual effect Effects 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000000052 vinegar Substances 0.000 description 2
- 235000021419 vinegar Nutrition 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- AUZONCFQVSMFAP-UHFFFAOYSA-N disulfiram Chemical group CCN(CC)C(=S)SSC(=S)N(CC)CC AUZONCFQVSMFAP-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of ethyl acetate integration systems for tower, including tower body, tower bottom reboiler and overhead condenser, the tower body is cylindrical pressure vessel, including cylinder, upper cover and lower head, the tower body passes through tower internals from the bottom to top and is successively divided into tower reactor section, stripping section, conversion zone, extraction section, rectifying section and tower top section.Of the invention prepares tower, and facility compact, overall 60% or more occupied area reduction, operation energy consumption is low, saves 40% or more compared with common process, and device wastewater flow rate is few, reduces 80% or more compared with prior art.
Description
Technical field
The present invention relates to a kind of ethyl acetate integration systems for tower, is knockdown tower structure, specifically a kind of anti-
Ethyl acetate should be generated and complete extraction and rectifying in same tower, can directly take out the integration system of finished product for tower.
Background technique
Ethyl acetate is a kind of important Organic chemical products, its main production process is to be with 98% concentrated sulfuric acid at present
Catalyst continuous esterification method, production process route are sub-thread charging, and acetic acid and ethyl alcohol enter reaction kettle under the action of sulfuric acid
Esterification is carried out, ethyl acetate and water are generated, the thick ester reacted is refining to obtain final products by rectifying column.This master
There are following problems for the production of ethyl technique of stream: (1) sulfuric acid corrosion resistance is strong, side reaction is more, by-product is difficult to handle, interval
Formula production, needs system update after a period of time；(2) thorough cleaning systems are needed, cause process to interrupt, system sewerage amount
Greatly, environmental protection pressure is high；(3) reaction, extraction and rectifying are individually completed in respective equipment in process, and power consumption, steam disappear
Consumption is all big, does not meet now environmentally protective production theory.
Summary of the invention
The purpose of the present invention is to solve the above-mentioned problems of the prior art and deficiency, provide a kind of ethyl acetate one
Body prepares tower, and reaction, extraction and rectifying are integrated in a tower and completed, compact-sized, operation energy consumption is low, can serialization
Production, and catalyst can be produced online and regenerated, waste discharge amount is few, more environmentally protective.
In order to achieve the above objectives, the technical solution adopted by the present invention is that:
For tower, including tower body, tower bottom reboiler and overhead condenser, the tower body is circle for a kind of ethyl acetate integration system
Column-shape pressure container, including cylinder, upper cover and lower head, the tower body pass through tower internals from the bottom to top and are successively divided into tower reactor
The bottom of section, stripping section, conversion zone, extraction section, rectifying section and tower top section, the tower reactor section is equipped with tower reactor liquid outlet N7, institute
The top for stating tower reactor section is equipped with boils steam inlet N6 again, and the entrance of the tower bottom reboiler is connected to the tower reactor liquid outlet N7,
Steam inlet N6 is boiled described in outlet again, the lower part of the tower top section is equipped with reflux inlet N2, sets at the top of the tower top section
There is top gaseous phase to export N1, the entrance of the overhead condenser is connected to the top gaseous phase and exports N1, flows back described in outlet
Entrance N2, the tower internals include the first tower internals, the second tower internals and third tower internals, and first tower internals is from top to bottom
Including grid-like support plate and the first redistributor, the grid-like support plate is fixed on the cylinder, and described first divides again
Cloth device includes several circles for being equipped with the first redistributor bottom plate of several apertures and being arranged on the first redistributor bottom plate
Pipe, the first redistributor bottom plate are mounted on the grid-like support plate lower part, and diameter is slightly less than the diameter of the cylinder,
The edge of the first redistributor bottom plate is equipped with the anti-wall flow plate that disconnected section is arc-shaped, and second tower internals includes described
Grid-like support plate, the third tower internals include the second redistributor, and second redistributor includes being equipped with several apertures
The second redistributor bottom plate and several round tubes for being arranged on the second redistributor bottom plate, second redistribution
Device bottom plate is connect with the cylinder, is separated between the tower reactor section and the stripping section by second tower internals, the essence
Evaporate and separated between section and the tower top section by the third tower internals, the stripping section, the conversion zone, the extraction section and
It is separated between the rectifying section by first tower internals, the stripping section, the conversion zone, the extraction section and the essence
It evaporates and is filled with filler in section, the grid-like support of first tower internals between the stripping section and the conversion zone
Between plate and first redistributor be equipped with ethyl alcohol feed inlet N5, described first between the conversion zone and the extraction section
Between the grid-like support plate of tower internals and first redistributor be equipped with ionic liquid entrance N4, the extraction section with
Vinegar is equipped between the grid-like support plate and first redistributor of first tower internals between the rectifying section
Sour entrance N3.
Further, the stripping section, the conversion zone, the extraction section and the rectifying section respectively include several segments by institute
State the secondary section that the first tower internals separates.
Further, the top of the tower reactor section is equipped with testing of materials mouth N8, is equipped with top in the testing of materials mouth N8
Opening, the material that remaining side is equipped with several apertures hold pipe.
Further, the cylinder is divided into several sections, and every section is equipped with lifting lug, passes through flanged joint between every section.
Further, the tower reactor section, the stripping section, the conversion zone, the extraction section, the rectifying section and the tower
It is equipped with thermometer installing port and pressure gauge installing port in the section of top, and thermometer and pressure gauge are installed, the bottom of the tower reactor section
Portion is equipped with liquidometer installing port and is equipped with liquidometer.
Further, the inner wall of the tower body is equipped with liner, and the inner lining material is polytetrafluoroethylene (PTFE) or PFA plastics.
Further, the grid-like support plate includes the flange being arranged on the cylinder, positioning plate, plastic-steel bar, grid
Plate and polytetrafluoroethylene (PTFE) cushion block, the both ends of the every plastic-steel bar are equipped with the polytetrafluoroethylene (PTFE) cushion block, several plastic-steels
Bar and several positioning plate interconnections form support baseboard, and the support baseboard is supported on the flange, the grid
Plate is supported on the support baseboard, and the first redistributor bottom plate is lifted on the lower section of the flange by studs.
Further, the bottom of the tower body is equipped with skirt, and the bottom plate of the skirt is equipped with foundation bolt for fixing
Hole.
Ethyl acetate integration system of the invention for tower working principle
Ethyl alcohol enters the tower body by the ethyl alcohol feed inlet N5, and high-temperature steam is encountered in the stripping section and realizes gas
Change, forms gaseous state ethyl alcohol and rise along the tower body, meanwhile, ionic liquid enters the tower body through the ionic liquid entrance N4,
Acetic acid enters the tower body through the acetic acid entrance N3, the ionic liquid and the acetic acid enter in the tower body after down
Stream encounters gaseous state ethyl alcohol in the conversion zone, realizes that esterification forms ethyl acetate and water, ionic liquid play catalysis and extraction
The dual function taken, ethyl acetate is risen as most light component along the tower body with gaseous state, through the extraction section by the vinegar
Sour further extraction dehydration, then after the rectifying section takes off acetic acid, into the overhead condenser, available purity reaches
99.9% ethyl acetate is as product.The water that ionic liquid and reaction generate is together along the tower body toward flowing down, into described
Stripping section and the tower reactor section produce together with catalyst.It removes water simply, while being also able to achieve continuous outside the tower of catalyst outside tower
Change regeneration, reduces the wash number of the regularly tower body, reduce the generation of waste water.The effect of the stripping section is mainly
Ethyl alcohol stripping section will be entered from N5 mouthfuls of the ethyl alcohol feed inlet into gaseous state, return to the conversion zone.
Compared with prior art, the advantages of the present invention are as follows:
Ethyl acetate integration system provided by the invention is for tower, by three reaction of ethyl acetate, extraction, rectifying main works
Skill process concentrates on Tai Tanei completion, i.e. acetic acid, ethyl alcohol, catalyst (ionic liquid) is added in Integral tower and completes instead
It answers, extraction, rectifying, tower ejecting product ethyl acetate, the water of tower reactor catalyst and reaction generation is regenerated in tower body outer circulation, by water
After taking off, catalyst returns integration system for reaction is carried out continuously in tower.Three conventional equipment are integrated into a combined column,
Although slightly more complex some in structure, whole device process is simplified, process complexity is reduced, equipment can be greatly reduced
Investment reduces operating cost.And reaction heat is not only adequately utilized during upwards in gaseous products in reaction process,
Also adverse current and the catalyst (ionic liquid) of low water content, the acetic acid of high concentration, form natural extraction process, reduce thick rouge
In water content, reduce the basis that has created of moisture content for top fractionation.Integration system is designed for tower using structured packing, gas-liquid
Contact surface is big, and reaction efficiency is high, and after reducing moisture content by extraction section, top fractionation can go out qualified products.In the process without another
Condense or heat up again outside heating, and capacity usage ratio is high.Every section of filler bottom, the redistributor of grid-like support plate and lower part, group
Unify body, when installation adjustable redistributor levelness, reach optimal distributed effect, anti-wall flow structure can also further be kept away
Exempt from being unevenly distributed for filler liquid phase.Such structure avoids liner tower that distributor tower section is separately provided simultaneously, and reduction finishes
Structure length reduces additional sealing surface, reduces risk of leakage.
It is all to be enriched with to tower reactor section, together with catalyst in rectifying and extraction process due to the moisture content in reaction process
Extraction, system remove water the outer serialization regeneration of system that is simple, while being also able to achieve catalyst outside, reduce regularly cleaning systems
Number reduces the generation of waste water.
For thick ester during upwards, gas phase can adequately utilize reaction heat, and use the crude product after extraction water removal,
In top fractionation, the amount for consuming steam will also reduce much compared with traditional equipment.Because initial water concentration is low, the reason of top filler
By tower tray number also less than conventional equipment, integral device investment is more saved.
Of the invention prepares tower, and rectifying section theory tower section number can control at 16 pieces, the water content of thick ester after extraction
It can be less than 0.05%.
Of the invention prepares tower, and facility compact, overall 60% or more occupied area reduction, operation energy consumption is low, more conventional work
Skill saves 40% or more, and device wastewater flow rate is few, reduces 80% or more compared with prior art.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the embodiment of the present invention；
Fig. 2 is grid-like support plate main view in the embodiment of the present invention；
Fig. 3 is grid-like support plate top view in the embodiment of the present invention；
Fig. 4 is the first redistributor main view in the embodiment of the present invention；
Fig. 5 is the first redistributor top view in the embodiment of the present invention；
In figure: 1 be tower body, 2 be tower bottom reboiler, 3 be overhead condenser, 4 be cylinder, 5 be upper cover, 6 be lower head,
7 it is tower internals, 8 be tower reactor section, 9 be stripping section, 10 be conversion zone, 11 be extraction section, 12 be rectifying section, 13 is tower top section, 14
For the first tower internals, 15 be the second tower internals, 16 be third tower internals, 17 be grid-like support plate, 18 be the first redistributor,
19 be the first redistributor bottom plate, 20 be round tube, 21 be anti-wall flow plate, 22 be the second redistributor, 23 be the second redistributor
Bottom plate, 24 be filler, 25 be material hold pipe, 26 be flange, 27 be positioning plate, 28 be plastic-steel bar, 29 be flase floor, 30 be poly-
Tetrafluoroethene cushion block, 31 be skirt, N1 is top gaseous phase outlet, N2 is reflux inlet, N3 is acetic acid entrance, N4 is ionic liquid
Entrance, N5 be ethyl alcohol feed inlet, N6 be boil steam inlet again, N7 is tower reactor liquid outlet, N8 is testing of materials mouth.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, with reference to the accompanying drawing and specific real
Applying mode, the present invention is described in further detail.
It is as shown in Figures 1 to 5: to be boiled again for a kind of ethyl acetate integration system of the invention for tower, including tower body 1, tower bottom
Device 2 and overhead condenser 3, the tower body 1 are cylindrical pressure vessel, including cylinder 4, upper cover 5 and lower head 6, the tower
Body 1 is successively divided into tower reactor section 8, stripping section 9, conversion zone 10, extraction section 11, rectifying section 12 and tower by tower internals 7 from the bottom to top
Section 13 is pushed up, the bottom of the tower reactor section 8 is equipped with tower reactor liquid outlet N7, and the top of the tower reactor section 8 is equipped with boils steam inlet again
N6, the entrance of the tower bottom reboiler 2 are connected to the tower reactor liquid outlet N7, boil steam inlet N6, institute again described in outlet
The lower part for stating tower top section 13 is equipped with reflux inlet N2, and the top of the tower top section 13 is equipped with top gaseous phase and exports N1, the tower top
The entrance of condenser 3 is connected to the top gaseous phase and exports N1, reflux inlet N2 described in outlet, and the tower internals 7 includes the
One tower internals 14, the second tower internals 15 and third tower internals 16, first tower internals 14 from top to bottom include grid-like support
Plate 17 and the first redistributor 18, the grid-like support plate 17 are fixed on the cylinder 4, and first redistributor 18 wraps
Including equipped with several apertures first redistributor bottom plate 19 and several round tubes for being arranged on the first redistributor bottom plate 19
20, the first redistributor bottom plate 19 is mounted on 17 lower part of grid-like support plate, and diameter is slightly less than the cylinder 4
Diameter, the edge of the first redistributor bottom plate 19 are equipped with disconnected section for the anti-wall flow plate 21 of arc-shaped, in second tower
Part 15 includes the grid-like support plate 17, and the third tower internals 16 includes the second redistributor 22, second redistribution
If device 22 includes being equipped with the second redistributor bottom plate 23 of several apertures and being arranged on the second redistributor bottom plate 23
Do the round tube 20, the second redistributor bottom plate 23 is connect with the cylinder 4, the tower reactor section 8 and the stripping section 9 it
Between separated by second tower internals 15, pass through the third tower internals 16 between the rectifying section 12 and the tower top section 13
It separates, by first tower between the stripping section 9, the conversion zone 10, the extraction section 11 and the rectifying section 12
Part 14 separates, and is filled with respectively in the stripping section 9, the conversion zone 10, the extraction section 11 and the rectifying section 12
Material 24, the grid-like support plate 17 of first tower internals 14 between the stripping section 9 and the conversion zone 10 and institute
It states and is equipped with ethyl alcohol feed inlet N5 between the first redistributor 18, described first between the conversion zone 10 and the extraction section 11
Ionic liquid entrance N4, the extraction are equipped between the grid-like support plate 17 of tower internals 14 and first redistributor 18
The grid-like support plate 17 and described first of first tower internals 14 between section 11 and the rectifying section 12 is taken to divide again
Acetic acid entrance N3 is equipped between cloth device 18.
The stripping section 9, the conversion zone 10, the extraction section 11 and the rectifying section 12 respectively include several segments by institute
State the secondary section that the first tower internals 14 separates.(secondary section is one section in the present embodiment)
The top of the tower reactor section 8 is equipped with testing of materials mouth N8, be equipped in the testing of materials mouth N8 upper opening its
The material that remaining side is equipped with several apertures holds pipe 25.
The cylinder 4 is divided into several sections, and every section is equipped with lifting lug, passes through flanged joint between every section.
The tower reactor section 8, the stripping section 9, the conversion zone 10, the extraction section 11, the rectifying section 12 and described
It is equipped with thermometer installing port and pressure gauge installing port in tower top section 13, and thermometer and pressure gauge are installed, the tower reactor section 8
Bottom be equipped with and liquidometer installing port and liquidometer be installed.
The inner wall of the tower body 1 is equipped with liner, and the inner lining material is polytetrafluoroethylene (PTFE).
As shown in Figures 2 and 3, the grid-like support plate 17 includes flange 26, the positioning plate being arranged on the cylinder 4
27, the both ends of plastic-steel bar 28, flase floor 29 and polytetrafluoroethylene (PTFE) cushion block 30, the every plastic-steel bar 28 are equipped with the polytetrafluoro
Ethylene cushion block 30, several plastic-steel bars 28 form support baseboard, the support bottom with several 27 interconnections of positioning plate
Plate is supported on the flange 26, and the flase floor 29 is supported on the support baseboard, the first redistributor bottom plate 19
The lower section of the flange 26 is lifted on by studs.
The bottom of the tower body 1 is equipped with skirt 31, and the bottom plate of the skirt 31 is equipped with anchor (bolt) hole for fixing.
Of the invention prepares tower integration system for the method for ethyl acetate, is by the reaction of ethyl acetate, extraction, rectifying three
A main processes concentrate on Tai Tanei completion, i.e., acetic acid, ethyl alcohol, that catalyst (ionic liquid) is added to integration system is standby
Reaction is completed in tower, is extracted, rectifying, tower ejecting product ethyl acetate, and the water that tower reactor catalyst is generated with reaction follows outside tower body
Ring regeneration, after water is taken off, catalyst returns integration system for reaction is carried out continuously in tower, specifically includes the following steps:
1, the requirement of reaction solution:
Acetic acid industry grade, purity are more than or equal to 99%, and other impurity meet national standard GB/T1628.1-2008；
Ethanol industry grade, purity are greater than 95%, and in addition to water, the total mass concentration of other impurity is no more than 0.05%, meet
National standard GB10343-2008；
Catalyst (ionic liquid): pyridine and alkyl pyridine hydrogen sulfate and hydrophosphate, imidazoles and alkyl imidazole hydrogen sulfate
With about 8 kinds of component prescription mixtures such as hydrophosphate, free acid, water.
2, in mass ratio by acetic acid: ethyl alcohol: catalyst is (1.05~1): 1:(1.4~1.5) to be sent to preheater respectively pre-
Heat enters integration system to 80 DEG C~90 DEG C in tower, and tower reactor reaction temperature is 110~120 DEG C, and pressure is normal pressure.
3, in preparing tower, acetic acid and catalyst (ionic liquid) are past dirty along tower, exist with the ethyl alcohol vaporized from tower lower part
Main reaction section (N4 to N5 nozzle section) reaction generates ethyl acetate and water, ionic liquid play the dual function of catalysis and extraction；
Ethyl acetate is up walked in the form of vapour phase as most light component along tower, is further extracted through acetic acid extraction section (N3 to N4 nozzle section)
After taking dehydration, rectifying section (the nozzle section from N2 to N3) desacetoxy, the condenser into tower top is condensed into product purity and can reach
99.9%.
4, catalyst (ionic liquid) and reaction generate water together along tower toward flow down, into stripping section (from N5 to N6 manage
Mouth section) and tower reactor；The effect of stripping section returns to conversion zone mainly by the ethyl alcohol stripping entered from N5 mouthfuls at vapour phase；Tower bottoms
There are also the water of excessive acetic acid about 15~18% besides the catalyst in phase；The tower bottoms, can under the evaporation of tower bottom reboiler
The light components total content such as ethyl acetate, ethyl alcohol is removed to 0.1% or less；Catalyst and water are regenerated in tower outer circulation to be separated, will
After water is taken off, catalyst returns in Integral tower and is carried out continuously reaction.
The above is only a preferred embodiment of the present invention, it should be pointed out that: for the ordinary skill people of the art
For member, without departing from the principle of the present invention, some improvements and modifications can also be made, these improvement and modification are also answered
It is considered as protection scope of the present invention.
Claims (8)
1. a kind of ethyl acetate integration system is for tower, it is characterised in that: including tower body (1), tower bottom reboiler (2) and overhead condensation
Device (3), the tower body (1) are cylindrical pressure vessel, including cylinder (4), upper cover (5) and lower head (6), the tower body
(1) successively it is divided into tower reactor section (8), stripping section (9), conversion zone (10), extraction section (11), essence by tower internals (7) from the bottom to top
Section (12) and tower top section (13) are evaporated, the bottom of the tower reactor section (8) is equipped with tower reactor liquid outlet (N7), the tower reactor section (8)
Top is equipped with boils steam inlet (N6) again, and the entrance of the tower bottom reboiler (2) is connected to the tower reactor liquid outlet (N7), outlet
Connection is described to boil steam inlet (N6) again, and the lower part of the tower top section (13) is equipped with reflux inlet (N2), the tower top section (13)
Top be equipped with top gaseous phase outlet (N1), the entrance of the overhead condenser (3) is connected to the top gaseous phase outlet (N1), out
Mouth is connected to the reflux inlet (N2), and the tower internals (7) includes the first tower internals (14), the second tower internals (15) and third tower
Internals (16), first tower internals (14) from top to bottom include grid-like support plate (17) and the first redistributor (18), institute
It states grid-like support plate (17) to be fixed on the cylinder (4), first redistributor (18) includes being equipped with several apertures
First redistributor bottom plate (19) and several round tubes (20) being arranged on the first redistributor bottom plate (19), described first
Redistributor bottom plate (19) is mounted on the grid-like support plate (17) lower part, and diameter is slightly less than the diameter of the cylinder (4),
The edge of the first redistributor bottom plate (19) is equipped with the anti-wall flow plate (21) that disconnected section is arc-shaped, second tower internals
It (15) include the grid-like support plate (17), the third tower internals (16) includes the second redistributor (22), and described second
Redistributor (22) includes being equipped with the second redistributor bottom plate (23) of several apertures and being arranged at second redistributor bottom
Several round tubes (20) on plate (23), the second redistributor bottom plate (23) connect with the cylinder (4), the tower reactor
It is separated between section (8) and the stripping section (9) by second tower internals (15), the rectifying section (12) and the tower top section
(13) it is separated between by the third tower internals (16), the stripping section (9), the conversion zone (10), the extraction section
(11) it is separated between the rectifying section (12) by first tower internals (14), the stripping section (9), the conversion zone
(10), it is filled with filler (24) in the extraction section (11) and the rectifying section (12), the stripping section (9) is reacted with described
Section (10) between first tower internals (14) the grid-like support plate (17) and first redistributor (18) it
Between be equipped with ethyl alcohol feed inlet (N5), first tower internals (14) between the conversion zone (10) and the extraction section (11)
It is equipped with ionic liquid entrance (N4) between the grid-like support plate (17) and first redistributor (18), the extraction section
(11) grid-like support plate (17) and described first of first tower internals (14) between the rectifying section (12)
Acetic acid entrance (N3) is equipped between redistributor (18).
2. a kind of ethyl acetate integration system according to claim 1 is for tower, it is characterised in that: the stripping section (9), institute
It states conversion zone (10), the extraction section (11) and the rectifying section (12) and respectively includes several segments by first tower internals (14)
The secondary section separated.
3. a kind of ethyl acetate integration system according to claim 1 is for tower, it is characterised in that: the tower reactor section (8)
Top is equipped with testing of materials mouth (N8), is equipped with upper opening in the testing of materials mouth (N8), remaining side is equipped with several apertures
Material hold pipe (25).
4. a kind of ethyl acetate integration system according to claim 1 is for tower, it is characterised in that: the cylinder (4) is divided into
Several sections, every section are equipped with lifting lug, pass through flanged joint between every section.
5. a kind of ethyl acetate integration system according to claim 1 is for tower, it is characterised in that: the tower reactor section (8), institute
It states in stripping section (9), the conversion zone (10), the extraction section (11), the rectifying section (12) and the tower top section (13)
It is provided with thermometer installing port and pressure gauge installing port, and thermometer and pressure gauge are installed, the bottom of the tower reactor section (8) is set
It is equipped with liquidometer installing port and liquidometer is installed.
6. a kind of ethyl acetate integration system according to claim 1 is for tower, it is characterised in that: the tower body (1) it is interior
Wall is provided with liner, and the material of the liner is polytetrafluoroethylene (PTFE) or PFA plastics.
7. a kind of ethyl acetate integration system according to claim 1 is for tower, it is characterised in that: the grid-like support plate
It (17) include flange (26), positioning plate (27), plastic-steel bar (28), flase floor (29) He Jusi being arranged on the cylinder (4)
Vinyl fluoride cushion block (30), the both ends of the every plastic-steel bar (28) are equipped with the polytetrafluoroethylene (PTFE) cushion block (30), several described
Plastic-steel bar (28) and several positioning plate (27) interconnections form support baseboard, and the support baseboard is supported on the flange
(26) on, the flase floor (29) is supported on the support baseboard, and the first redistributor bottom plate (19) passes through double end spiral shell
Column is lifted on the lower section of the flange (26).
8. a kind of ethyl acetate integration system according to claim 1 is for tower, it is characterised in that: the bottom of the tower body (1)
Portion is provided with skirt (31), and the bottom plate of the skirt (31) is equipped with anchor (bolt) hole for fixing.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910213290.0A CN109851501A (en) | 2019-03-20 | 2019-03-20 | Ethyl acetate integration system is for tower |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910213290.0A CN109851501A (en) | 2019-03-20 | 2019-03-20 | Ethyl acetate integration system is for tower |
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| CN201910213290.0A Pending CN109851501A (en) | 2019-03-20 | 2019-03-20 | Ethyl acetate integration system is for tower |
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| CN111167146A (en) * | 2019-12-26 | 2020-05-19 | 重庆市中润化学有限公司 | NMP waste liquid is retrieved with dehydration tower |
| CN111265902A (en) * | 2020-03-09 | 2020-06-12 | 内蒙古兰格生物科技有限公司 | Continuous rectification device |
| CN114524727A (en) * | 2022-02-23 | 2022-05-24 | 南京大学 | Ethyl acetate clean production system with double-tower structure and production process |
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Effective date of registration: 20200103 Address after: 212006 No. 88 Qiusuo Road, Jingkou District, Zhenjiang City, Jiangsu Province Applicant after: Jiangsu Sopo Chemical Co.,Ltd. Applicant after: Jiangsu Thorpe Engineering Technology Co., Ltd. Address before: Xiangshan mayor of Zhenjiang city in Jiangsu province 212006 Gang Jingkou District Applicant before: Jiangsu Soap (Group) Co., Ltd. Applicant before: Jiangsu Thorpe Engineering Technology Co., Ltd. |