CN106699552A - Method for producing isopropyl acetate through heat pump partition-wall reactive distillation tower - Google Patents
Method for producing isopropyl acetate through heat pump partition-wall reactive distillation tower Download PDFInfo
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- CN106699552A CN106699552A CN201611186121.5A CN201611186121A CN106699552A CN 106699552 A CN106699552 A CN 106699552A CN 201611186121 A CN201611186121 A CN 201611186121A CN 106699552 A CN106699552 A CN 106699552A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/03—Preparation of carboxylic acid esters by reacting an ester group with a hydroxy group
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/007—Energy recuperation; Heat pumps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/141—Fractional distillation or use of a fractionation or rectification column where at least one distillation column contains at least one dividing wall
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/32—Packing elements in the form of grids or built-up elements for forming a unit or module inside the apparatus for mass or heat transfer
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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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
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Abstract
The invention discloses a method for producing isopropyl acetate through a heat pump partition-wall reactive distillation tower and belongs to the technical field of rectification. Isopropanol and methyl acetate are respectively fed into a reaction and separation zone of the heat pump partition-wall reactive distillation tower to be in contact with a catalyst for reaction and separation zone, a vapor-phase mixture of methyl alcohol and methyl acetate flows out of a tower top separation zone and is divided into two ways, one way of mixture is compressed by a compressor and then provides reboiling heat for an isopropyl acetate reboiler at the bottom of the reaction and separation zone, then the way of mixture passes through a throttling valve and then is mixed with the other way of mixture, one part flows back to the tower after condensation, the other part is mixed with the raw material methyl acetate, and the mixture returns to the reaction and separation zone again. The target product high-purity isopropyl acetate is extracted from the lower portion of the reaction and separation zone, and the methyl alcohol is extracted from the lower portion of a methyl alcohol recovery zone. Multiple towers for traditional reaction, rectification and follow-up separation and purification processes are integrated to one partition-wall reactive distillation tower, and device investment is saved.
Description
Technical field
The invention belongs to technical field of rectification, it is related to the production method of ethyl ester isopropyl ester, specifically, is related to one kind to be used for
Prepare the heat pump partition wall reactive distillation column and its production method of isopropyl acetate.
Background technology
Isopropyl acetate is a kind of important carboxylic acid esters product.It is the raw material of synthetic resin and coating, it is also possible to be used as
Some perfume compositions, dehydrating agent, the solvent of coating, the solvent of printing-ink, and some medicines can be applied to as extractant
In the technique of thing synthesis.Isopropyl acetate has the title of " alembroth ", can be with the immiscible organic solvent such as alcohol, ketone, ethers.
The production technology of current synthesis of acetic acid isopropyl ester mainly has three kinds, and a kind of method is exactly that acetic acid is former with isopropanol
Material, the direct esterification generation isopropyl acetate in the presence of strongly acidic catalyst, the method as disclosed in CN103214367, this
, with the concentrated sulfuric acid as catalyst, because catalyst is easy to get, price is low for method, but its major defect is that device is perishable, easily pollutes ring
Border, product complicated difficult are separated, and the water for having equimolar quality after reaction is produced, and post processing flow is more long.Another method is to use
Acetic acid and propylene are directly synthesized isopropyl acetate, the method as disclosed in CN102757341.The method shortens reaction process,
The consumption of raw material is saved, acid reacts with the acid that alkene direct esterification is a molecule with a molecule propylene, generation one
The isopropyl acetate of molecule, does not have remaining accessory substance to produce in reaction, but the technique there is also weak point, can be sent out in reaction
The oligomer accumulation of raw alkene, causes subsequent separation process difficult.
In polyvinyl alcohol production technology, the methyl acetate yield as accessory substance is very big.Often produce one ton of polyethylene
Alcohol about produces 1.68 tons of methyl acetate.Methyl acetate value is not high, it is therefore desirable to convert it into more valuable acid
Or ester.Methyl acetate hydrolysis energy consumption is higher, limits its application.If use instead with isopropanol ester-interchange method recovery of acetic acid methyl esters,
There is obvious advantage in production energy-conservation and economic benefit.CN104945251A proposes a kind of with methyl acetate and isopropanol as former
Material, the reactive distillation process of ester-interchange method synthesis of acetic acid isopropyl ester.
The value the esters higher although reactive distillation process of ester-interchange method synthesis of acetic acid isopropyl ester can be applied,
Its energy consumption higher also should have one of problems faced extensively in the industry as this method.Patent CN105017019 proposes one
Plant the energy saving technique for using reaction under high pressure rectifying column and normal pressure methyl acetate recovery tower be thermally integrated generation isopropyl acetate.
The content of the invention
The deficiency that the present invention exists for above-mentioned technology, proposes a kind of with methyl acetate and isopropanol as raw material, ester exchange
The heat pump partition wall reactive distillation process of method synthesis of acetic acid isopropyl ester, the process set heat pump distillation and partition wall reactive distillation
The characteristics of, product purity high advantage low with energy consumption.
It is that, up to this purpose, the present invention uses following technical scheme：
A kind of isopropyl acetate heat pump partition wall reactive distillation column, comprising the king-tower with partition wall, overhead condenser, tower
Kettle isopropyl acetate reboiler, tower reactor methyl alcohol reboiler, are divided into Reaction Separation region, Methanol Recovery region and tower top inside king-tower
Separated region.Reaction Separation region and Methanol Recovery region are located at the middle and lower part of rectifying column, and both are separated by vertical dividing plate
Come, vertical dividing plate lower end is connected with tower bottom of rectifying tower, upper end extends to tower top separated region lower section.
Tower top separated region top outwards connects steam pipe, and steam pipe is divided into two, a connection compressor, another company
Connect overhead condenser；The rectifying column in Reaction Separation region is externally connected to raw material isopropanol feed pipe and the charging of raw acetic acid methyl esters
Pipe, the bottom in Reaction Separation region is provided with discharge nozzle, and discharge nozzle is divided into two, and a connection tower reactor isopropyl acetate reboiler is again
Coupled reaction separated region, another extraction isopropyl acetate；The bottom in Methanol Recovery region is provided with discharge nozzle, one point of discharge nozzle
It is two, a connection tower reactor methyl alcohol reboiler reconnects Methanol Recovery region, another extraction methyl esters.
Reaction Separation region middle part filled solid catalyst, upper and lower part filling High Efficient Standard Packing or column plate, plays rectifying
Centrifugation；Tower top separated region and the filling of Methanol Recovery region High Efficient Standard Packing or column plate, play rectifying centrifugation.
The method for preparing isopropyl acetate using heat pump partition wall reactive distillation column of the invention is：Isopropanol and acetic acid first
The Reaction Separation region that ester respectively enters heat pump partition wall reactive distillation column contacts with catalyst and carries out Reaction Separation, methyl alcohol and second
The vapour mixture of sour methyl esters is flowed out by tower top separated region, and vapour mixture is divided into two strands, and one gives after being compressed through compressor
Reaction Separation sections bottom isopropyl acetate reboiler provides boiling hot amount again, then by mixing with another burst of vapour phase after choke valve
Thing mixes, and by condensing in rear portion reflux column, another part mixes with raw acetic acid methyl esters and returns to Reaction Separation area
Domain.The isopropyl acetate of target product high-purity is produced by Reaction Separation region bottom, and methyl alcohol is adopted by Methanol Recovery region bottom
Go out.
Described catalyst is solid acid catalyst, can be Amberlyst-15, Amberlyst-35, Amberlyst-46
Deng storng-acid cation exchange resin.
Heat pump partition wall reactive distillation column operating pressure is 100~600kPa, and tower top separated region tower top operation temperature is
50~80 DEG C, number of theoretical plate is 5~15 pieces, and Reaction Separation sections bottom temperature is 90~150 DEG C, wherein 9~12 pieces of rectifying section
Plate, 40~50 blocks of plates of conversion zone, conversion zone loads solid catalyst, 10~15 blocks of plates of stripping section.Methanol Recovery region operation temperature
It is 64~72 DEG C to spend, and number of theoretical plate is 5~15 pieces.
The method for preparing isopropyl acetate using above-mentioned heat pump partition wall reactive distillation column, is carried out as steps described below：It is different
Propyl alcohol and methyl acetate respectively enter the Reaction Separation region of heat pump partition wall reactive distillation column, high boiling reactant isopropanol
The acetic acid first returned from the charging of Reaction Separation area top, lower boiling methyl acetate and from tower top separated region overhead condenser
Ester mixes with carbinol mixture, and from the charging of Reaction Separation region bottom, two raw materials are under solid catalyst effect in Reaction Separation
There is ester exchange reaction in region, generate target product isopropyl acetate and by-product carbinol, wherein target product isopropyl acetate
After reacted separated region is further separated, from the extraction of Reaction Separation sections bottom.Other components are entered into tower top separated region
One step is separated, and the methyl alcohol and the vapour mixture of methyl acetate obtained at the top of tower top separated region are divided into two strands, a stock-traders' know-how pressure
The compression of contracting machine enters isopropyl acetate reboiler with the tower reactor logistics heat exchange of Reaction Separation region after improving pressure and temp, there is provided boil again
Heat, then by mixing with another strand of vapour mixture after choke valve, is back to by overhead condenser condensation rear portion
Tower top separated region, another part mixes with raw acetic acid methyl esters and returns to Reaction Separation region.In the reaction of heat pump partition wall
The Methanol Recovery region of rectifying column, methyl alcohol enters a part from tower reactor obtains the methyl alcohol of high-purity with unreacted methyl acetate.It is whole
Individual process completes the coupling of heat by tower reactor isopropyl acetate reboiler.
Relative to prior art, effect of the invention is that：High-purity is realized in heat pump partition wall reactive distillation column
The production of isopropyl acetate, a partition wall reaction is incorporated into by the multitower of traditional reactive distillation and later separation purifying technique
In rectifying column, equipment investment is saved, meanwhile, by the energy coupling of liquid phase stream stock in tower, make full use of overhead gas
Latent heat, reduces the energy of external heat source, reduces energy consumption.The unreacted raw material backflow of heat pump partition wall reactive distillation column repeats to make
With improve total conversion.
Brief description of the drawings
Fig. 1 is heat pump partition wall reactive distillation column apparatus structure of the invention and technological process.
Label is as follows in figure：1- partition wall reactive distillation columns, 2- tower top separated regions, 3- isopropyl acetates recovery area
Domain, 4- Methanol Recoveries region, 5- isopropyl acetate reboilers, 6- methyl alcohol reboilers, 7- overhead condensers, 8- compressors,
9- choke valves, 10- raw material isopropanol feed pipes, 11 raw acetic acid methyl esters feed pipes, 12- partition wall reactive distillation column overheads
Steam pipe, 13- compressor vapour phase feed pipes, 14- isopropyl acetate reboiler steam feed pipes, 15- choke valve discharge nozzles,
16- overhead condenser feed pipes, 17- overhead reflux pipes, 18- partition wall reactive distillation column overhead extraction circulation pipes, 19- second
Isopropyl propionate recovery zone bottom extraction pipe, the extraction of 20- Methanol Recoveries region bottom.
Specific embodiment
Detailed narration is carried out to specific embodiment of the invention below in conjunction with accompanying drawing：
As shown in Figure 1：Isopropyl acetate heat pump partition wall reactive distillation column of the invention includes the king-tower with partition wall
1st, overhead condenser 7, isopropyl acetate reboiler 5, methyl alcohol reboiler 6 are divided into tower top separated region 2, reaction point inside king-tower
From region 3 and Methanol Recovery region 4.Reaction Separation region 3 and Methanol Recovery region 4 are located at the middle and lower part of rectifying column, Liang Zhetong
Cross vertical dividing plate to separate, vertical dividing plate lower end is connected with tower bottom of rectifying tower, and upper end is extended under tower top separated region 2
Side.
The top of tower top separated region 2 outwards connects steam pipe, and steam pipe is divided into two, a connection compressor 8, Ling Yigen
Connection overhead condenser 7；The rectifying column in Reaction Separation region 3 is externally connected to raw material isopropanol feed pipe and raw acetic acid methyl esters
Feed pipe, the bottom in Reaction Separation region 3 is provided with discharge nozzle, and discharge nozzle is divided into two, and a connection tower reactor isopropyl acetate is again
Boiling device 5 reconnects Reaction Separation region, another extraction isopropyl acetate；The bottom in Methanol Recovery region 4 is provided with discharge nozzle, goes out
Expects pipe is divided into two, and a connection tower reactor methyl alcohol reboiler 6 reconnects Methanol Recovery region, another extraction methyl esters.
The middle part of Reaction Separation region 3 filling catalysts, upper and lower part filling High Efficient Standard Packing or column plate, play essence
Evaporate centrifugation；Tower top separated region 2 and the filling of Methanol Recovery region 4 High Efficient Standard Packing or column plate, play rectifying and separate and make
With.
The technological process that heat pump partition wall reactive distillation column of the present invention prepares isopropyl acetate is：Raw material isopropyl
Alcohol and methyl acetate respectively enter the Reaction Separation region 3 of heat pump partition wall reactive distillation column R1, high boiling reactant isopropyl
Methyl acetate and methyl alcohol that alcohol is returned from the charging of the top of Reaction Separation region 3, lower boiling methyl acetate and from overhead condenser 7
Mixture mixes, and from the charging of the bottom of Reaction Separation region 3, two raw materials are sent out under solid catalyst effect in Reaction Separation region 3
Raw ester exchange reaction, generates target product isopropyl acetate and by-product carbinol, and wherein target product isopropyl acetate is reacted
After separated region 3 is further separated, from the extraction of Reaction Separation region tower bottom.Other components enter one into tower top separated region 2
Step is separated, and the methyl alcohol and methyl acetate vapour mixture obtained at the top of tower top separated region 2 are divided into two strands, and one is through compressor
8 compressions, enter isopropyl acetate reboiler 5 with the heat exchange of the bottoms of Reaction Separation region 3, there is provided boil again after improving pressure and temp
Heat, then mixes by choke valve 9 with another strand of vapour mixture, is back to by the condensation of overhead condenser 7 rear portion
Tower top separated region 2, another part mixes with raw acetic acid methyl esters and returns to Reaction Separation region 3.It is anti-in heat pump partition wall
The Methanol Recovery region 4 of rectifying column 1 is answered, methyl alcohol enters a part from the bottom of Methanol Recovery region 4 obtains with unreacted methyl acetate
To the methyl alcohol of high-purity.Due to making full use of the latent heat of overhead gas, the energy of external heat source is reduced, reduce energy consumption.
Embodiment 1
Using the technological process shown in accompanying drawing 1, the heat pump partition wall reactive distillation column 1 for being used is diameter 2300mm, 45
The packed tower of rice, 5 meters of the built-in structured packing of tower top separated region 2, number of theoretical plate is 10 pieces；Reaction Separation region 3 is built-in regular
35 meters of filler, number of theoretical plate is 74 pieces, wherein 9 blocks of plates of rectifying section, and 43 blocks of plates of conversion zone, conversion zone loads solid catalyst, institute
It is Amberlyst-15 storng-acid cation exchange resins, 12 blocks of plates of stripping section with catalyst.Loaded in Methanol Recovery region III
5 meters of structured packing, heat pump partition wall reactive distillation column RDWC operating pressures are 1atm, and the head temperature of tower top separated region 2 is 54
DEG C, the bottom temp of Reaction Separation region 3 is 91 DEG C, and the bottom temp of Methanol Recovery region 4 is 65 DEG C of
Raw material isopropanol is fed with 3005kg/h from the top of Reaction Separation region 3, lower boiling methyl acetate 3704kg/h
Mix with carbinol mixture 3785kg/h with the methyl acetate returned from evaporator overhead condenser E3, enter from the bottom of Reaction Separation region 3
There is ester exchange reaction in material, two raw materials, generate target product isopropyl acetate under solid catalyst effect in Reaction Separation region 3
After the reacted separated region 3 of ester and by-product carbinol, wherein target product isopropyl acetate is further separated, from Reaction Separation area
The bottom of domain 3 produces, and obtains the isopropyl acetate 5099kg/h that mass fraction is 99.7%.Other components enter tower top separated region
2 further separate, and the methyl alcohol and the vapour mixture of methyl acetate obtained from the tower top of tower top separated region 2 are divided into two strands, one
Compressed through compressor 8, isopropyl acetate reboiler 5 and the heat exchange of the bottoms of Reaction Separation region 3 entered after improving pressure and temp,
Boiling hot amount again is provided, is then mixed with another strand of vapour mixture by choke valve 9, latter portion is condensed by overhead condenser 7
Point backflow tower top separated region 2, another part mixes with raw acetic acid methyl esters and returns to Reaction Separation region 3.In heat pump point
The Methanol Recovery region 4 of next door reactive distillation column 1, methyl alcohol enters a part from from methanol recovery zone with unreacted methyl acetate
The bottom of domain 4 extraction mass fraction is 99.5% methyl alcohol 1612kg/h.The energy consumption of compressor 8 is 880kW, the energy consumption of overhead condenser 7
It is -1110kW, the energy consumption of III bottom methyl alcohol reboiler of Methanol Recovery region 6 is 387kW.Due to making full use of the latent of overhead gas
Heat, reduces the energy of external heat source, reduces energy consumption.
Embodiment 2
Using the technological process shown in accompanying drawing 1, the heat pump partition wall reactive distillation column 1 for being used is diameter 2100mm, high
10 pieces of column plate is set in 50 meters of plate column, tower top separated region 2；The number of plates is 76 pieces, wherein rectifying section in Reaction Separation region 3
10 blocks of plates, 44 blocks of plates of conversion zone, conversion zone loads solid catalyst, and used catalyst is Amberlyst-15 highly acidic cations
Exchanger resin, 12 blocks of plates of stripping section.6 pieces of column plate, the operating pressure of heat pump partition wall reactive distillation column 1 are set in Methanol Recovery region 4
It is 2atm, the head temperature of tower top separated region 2 is 73 DEG C, and the bottom temp of Reaction Separation region 3 is 113 DEG C, Methanol Recovery region 4
Bottom temp is 83 DEG C of
Raw material isopropanol is fed with 3005kg/h from the top of Reaction Separation region 3, lower boiling methyl acetate 3704kg/h
Mix with carbinol mixture 3520kg/h with the methyl acetate returned from overhead condenser 7, enter from the bottom of Reaction Separation region 3
There is ester exchange reaction in material, two raw materials, generate target product isopropyl acetate under solid catalyst effect in Reaction Separation region 3
After the reacted separated region 3 of ester and by-product carbinol, wherein target product isopropyl acetate is further separated, from Reaction Separation area
The bottom of domain 3 produces, and obtains the isopropyl acetate 5099kg/h that mass fraction is 99.6%.Other components enter tower top separated region
2 further separate, and the methyl alcohol and the vapour mixture of methyl acetate obtained from the tower top of tower top separated region 2 are divided into two strands, one
Compressed through compressor 8, tower reactor isopropyl acetate reboiler 5 and the bottoms of Reaction Separation region 3 are entered after improving pressure and temp
Heat exchange, there is provided boiling hot amount again, then mix by choke valve 9 with another strand of vapour mixture, by overhead condenser E3 condensations
Rear portion backflow tower top separated region 2, another part mixes with raw acetic acid methyl esters and returns to Reaction Separation region 3.
The Methanol Recovery region 4 of heat pump partition wall reactive distillation column 1, methyl alcohol enters a part from from methyl alcohol with unreacted methyl acetate
The bottom of recovery zone 4 extraction mass fraction is 99.5% methyl alcohol 1611kg/h, and the energy consumption of compressor 8 is 1121kW, overhead condensation
The energy consumption of device 7 is -1237kW, and the energy consumption of III tower reactor methyl alcohol reboiler of Methanol Recovery region 6 is 375kW.Due to making full use of tower overhead gas
The latent heat of body, reduces the energy of external heat source, reduces energy consumption.
Claims (4)
1. the method that heat pump partition wall reactive distillation column prepares isopropyl acetate, it is characterised in that carry out as steps described below：It is different
The Reaction Separation region that propyl alcohol and methyl acetate respectively enter heat pump partition wall reactive distillation column contacts with catalyst and is reacted
Separate, the vapour mixture of methyl alcohol and methyl acetate is flowed out by tower top separated region, and vapour mixture is divided into two strands, a stock-traders' know-how pressure
There is provided boiling hot amount again to Reaction Separation sections bottom isopropyl acetate reboiler after the compression of contracting machine, then by after choke valve with it is another
One vapour mixture mixes, and by condensing in rear portion reflux column, another part mixes with raw acetic acid methyl esters and returns again
Go back to Reaction Separation region；The isopropyl acetate of target product high-purity is produced by Reaction Separation region bottom, and methyl alcohol is returned by methyl alcohol
Receive the extraction of region bottom.
2. the method that heat pump partition wall reactive distillation column according to claim 1 prepares isopropyl acetate, it is characterised in that
Described catalyst is solid acid catalyst, can be the highly acids such as Amberlyst-15, Amberlyst-35, Amberlyst-46
Cationic ion-exchange resin.
3. the method that heat pump partition wall reactive distillation column according to claim 1 prepares isopropyl acetate, it is characterised in that
Heat pump partition wall reactive distillation column operating pressure is 100~600kPa, and tower top separated region tower top operation temperature is 50~80 DEG C,
Number of theoretical plate is 5~15 pieces, and Reaction Separation sections bottom temperature is 90~150 DEG C, wherein 9~12 blocks of plates of rectifying section, conversion zone
40~50 blocks of plates, conversion zone loads solid catalyst, 10~15 blocks of plates of stripping section；Methanol Recovery region operation temperature is 64~72
DEG C, number of theoretical plate is 5~15 pieces.
4. the method that heat pump partition wall reactive distillation column according to claim 1 prepares isopropyl acetate, it is characterised in that
Isopropanol and methyl acetate respectively enter the Reaction Separation region of heat pump partition wall reactive distillation column, high boiling reactant isopropyl
The acetic acid that alcohol is returned from the charging of Reaction Separation area top, lower boiling methyl acetate and from tower top separated region overhead condenser
Methyl esters mixes with carbinol mixture, and from the charging of Reaction Separation region bottom, two raw materials are under solid catalyst effect in reaction point
There is ester exchange reaction from region, generate target product isopropyl acetate and by-product carbinol, wherein target product isopropyl acetate
After the reacted separated region of ester is further separated, from the extraction of Reaction Separation sections bottom；Other components enter tower top separated region
Further separate, the methyl alcohol and the vapour mixture of methyl acetate obtained at the top of tower top separated region are divided into two strands, a stock-traders' know-how
Compressor compresses enter isopropyl acetate reboiler with the tower reactor logistics heat exchange of Reaction Separation region after improving pressure and temp, there is provided again
Boiling hot amount, then by mixing with another strand of vapour mixture after choke valve, flows back by overhead condenser condensation rear portion
Tower top separated region is returned, another part mixes with raw acetic acid methyl esters and returns to Reaction Separation region；It is anti-in heat pump partition wall
The Methanol Recovery region of rectifying column is answered, methyl alcohol enters a part from tower reactor obtains the methyl alcohol of high-purity with unreacted methyl acetate；
Whole process completes the coupling of heat by tower reactor isopropyl acetate reboiler.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109180435A (en) * | 2018-10-12 | 2019-01-11 | 常州大学 | A kind of device and method preparing isopropanol from recuperation of heat reactive distillation |
| CN109369340A (en) * | 2018-11-14 | 2019-02-22 | 常州大学 | A kind of device and method of reactive distillation transesterification preparing isopropanol |
| CN109438179A (en) * | 2018-10-24 | 2019-03-08 | 常州大学 | A kind of reactive distillation prepares the power-economizing method of isopropanol |
| CN109771980A (en) * | 2018-12-23 | 2019-05-21 | 中国科学院山西煤炭化学研究所 | A kind of heterogeneous azeotropic rectification method separating 2 pentanone, 4- heptanone, water and carbon dioxide mixture |
| CN109987660A (en) * | 2017-12-29 | 2019-07-09 | 财团法人工业技术研究院 | Solvent slop processing system and its method |
| CN110280033A (en) * | 2019-06-04 | 2019-09-27 | 常州大学 | A kind of device and method preparing propyl propionate from recuperation of heat reactive distillation |
| CN112675564A (en) * | 2020-07-24 | 2021-04-20 | 天津科技大学 | Baffle rectifying tower for separating four products without gas phase separation |
| CN115232006A (en) * | 2022-06-17 | 2022-10-25 | 天津大学 | Method and device for producing isopropanol and co-producing methyl acetate by two-tower reaction-variable pressure mixed rectification and application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102423539A (en) * | 2011-09-05 | 2012-04-25 | 天津大学 | Energy-saving technology of catalytic reaction distillation process and device thereof |
| CN104788295A (en) * | 2015-03-19 | 2015-07-22 | 万华化学集团股份有限公司 | Preparation method of 3-methyl-2-butylene-1-aldehyde diisopentenyl acetal |
| CN105017019A (en) * | 2015-07-08 | 2015-11-04 | 常州大学 | Energy-saving method for preparing isopropyl acetate |
-
2016
- 2016-12-21 CN CN201611186121.5A patent/CN106699552A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102423539A (en) * | 2011-09-05 | 2012-04-25 | 天津大学 | Energy-saving technology of catalytic reaction distillation process and device thereof |
| CN104788295A (en) * | 2015-03-19 | 2015-07-22 | 万华化学集团股份有限公司 | Preparation method of 3-methyl-2-butylene-1-aldehyde diisopentenyl acetal |
| CN105017019A (en) * | 2015-07-08 | 2015-11-04 | 常州大学 | Energy-saving method for preparing isopropyl acetate |
Non-Patent Citations (2)
| Title |
|---|
| GERD KAIBEL: "Distillation Columns with Vertical Partitions", 《CHEM. ENG. TECHNOL.》 * |
| 陈梦琪等: "反应精馏隔壁塔生产乙酸正丁酯的优化与控制", 《化工学报》 * |
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| CN109180435A (en) * | 2018-10-12 | 2019-01-11 | 常州大学 | A kind of device and method preparing isopropanol from recuperation of heat reactive distillation |
| CN109438179A (en) * | 2018-10-24 | 2019-03-08 | 常州大学 | A kind of reactive distillation prepares the power-economizing method of isopropanol |
| CN109369340A (en) * | 2018-11-14 | 2019-02-22 | 常州大学 | A kind of device and method of reactive distillation transesterification preparing isopropanol |
| CN109771980A (en) * | 2018-12-23 | 2019-05-21 | 中国科学院山西煤炭化学研究所 | A kind of heterogeneous azeotropic rectification method separating 2 pentanone, 4- heptanone, water and carbon dioxide mixture |
| CN109771980B (en) * | 2018-12-23 | 2021-04-13 | 中国科学院山西煤炭化学研究所 | Heterogeneous azeotropic rectification method for separating mixture of 2-pentanone, 4-heptanone, water and carbon dioxide |
| CN110280033A (en) * | 2019-06-04 | 2019-09-27 | 常州大学 | A kind of device and method preparing propyl propionate from recuperation of heat reactive distillation |
| CN110280033B (en) * | 2019-06-04 | 2021-11-02 | 常州大学 | Device and method for preparing propyl propionate through self-heating recovery reaction rectification |
| CN112675564A (en) * | 2020-07-24 | 2021-04-20 | 天津科技大学 | Baffle rectifying tower for separating four products without gas phase separation |
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