CN109180435A - A kind of device and method preparing isopropanol from recuperation of heat reactive distillation - Google Patents
A kind of device and method preparing isopropanol from recuperation of heat reactive distillation Download PDFInfo
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- CN109180435A CN109180435A CN201811186711.7A CN201811186711A CN109180435A CN 109180435 A CN109180435 A CN 109180435A CN 201811186711 A CN201811186711 A CN 201811186711A CN 109180435 A CN109180435 A CN 109180435A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/128—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by alcoholysis
- C07C29/1285—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by alcoholysis of esters of organic acids
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment 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
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention discloses a kind of device and methods from recuperation of heat reaction rectification technique petrohol, belong to technical field of rectification.After being heated up by the mixed vapour material of reactive distillation column and recovery tower overhead extraction using compressor boost, institute's calorific requirement is boiled again to reactive distillation column and the offer of recovery tower tower reactor respectively, is completed at the same time the condensation of tower top mixed vapour material itself.The preheating of raw material and intermediate product is most of in the present invention uses tower top material to increase temperature after compressor boost heats up for the waste heat after each tower heat supply, realize that tower top material condenses using cooling water relative to tradition, and the scheme of tower reactor heating and raw material preheating is realized using hot public work, the present invention realizes self-heating by compressor and recycles, the energy consumption and expense of compressor generate good economic benefit far below traditional cooling water and hot public work.Compared with traditional reactive distillation process, 50% or more can save energy from recuperation of heat reaction rectification technique.
Description
Technical field
The invention belongs to technical field of rectification, are related to the production method of isopropanol, specifically, being related to a kind of based on self-heating
The reactive distillation of recycling prepares the energy saving technique of isopropanol.
Background technique
Isopropanol has extensive use as Organic Ingredients and solvent.As Organic Ingredients, isopropanol mainly for the production of
Acetone, it is also possible to make the raw material of the products such as synthetic glycerine, isopropyl acetate, isopropyl amine salt, nitrous acid diisopropylamine.As
Solvent, isopropanol can be used for producing coating, ink, extractant, aerosol agent etc., and isopropanol is also widely used as oil-fired anti-
Freeze additive.In addition, isopropanol can also be used to manufacture fungicide, insecticide, disinfectant and preservative etc..
Currently, the method for industrial petrohol mainly has propylene hydration method.Propylene hydration method can be divided into direct hydration
With two kinds of indirect hydration method.
United States Patent (USP) US3352930A prepares isopropanol using propylene indirect hydration method.In 70~80 DEG C of temperature and pressure
Under conditions of 1.5~6.0MPa, propylene is dissolved in 70~80% sulfuric acid and carries out esterification, then obtained through hydrolysis purification
High-purity isopropanol.But propylene indirect hydration method process is complicated, and selectivity of product is low, and sulfuric acid is big to equipment corrosion.
European patent EP 0323268 and United States Patent (USP) US5012014A propose that propylene direct hydration method prepares isopropanol.?
At 200 DEG C of temperature and pressure 7.0MPa, propylene and water directly carry out hydration reaction in the presence of a zeolite catalyst and generate isopropanol.
Propylene direct hydration method overcomes equipment etching problem, but propylene one way conversion ratio is low, and propylene internal circulating load ambassador's process energy consumption mentions
Height, and this method requires height to raw material and reaction condition.
Chinese patent CN102976894B provides a kind of catalytic rectification process of ester-interchange method petrohol.Raw material second
In the conversion zone of catalytic rectifying tower ester exchange reaction occurs for isopropyl propionate and methanol under the catalytic action of cation exchange resin
And vapour-liquid Pignus pignoris is carried out, realize continuous catalyzing rectifying process.Process avoids the recycling of alkali salt catalyst, have reaction conversion
The features such as rate is high, produces stay in grade.But its higher energy consumption also becomes this method should one of problems faced extensively in the industry.
Summary of the invention
The present invention is existing insufficient in view of the above technology, proposes a kind of using isopropyl acetate and methanol as raw material, transesterification
Method petrohol based on the reactive distillation process from recuperation of heat, the process set is from heat recovery technology and reactive distillation
Feature, have low energy consumption, the high advantage of product purity.
To achieve this purpose, the present invention adopts the following technical scheme:
A kind of device of the reaction rectification technique petrohol from recuperation of heat, comprising: First Heat Exchanger, described first changes
Hot device has the first fluid channel and second fluid channel that are spaced apart from each other, the output end in first fluid channel and preheater it is defeated
Enter end connection；
Second heat exchanger, second heat exchanger have the third fluid channel and the 4th fluid channel being spaced apart from each other, the
The output end of four fluid channels is connect with the input terminal in second fluid channel；
Third heat exchanger, the third heat exchanger have the 5th fluid channel and the 6th fluid channel being spaced apart from each other, the
Five fluid channel output ends are connect with reactive distillation column tower reactor, the input terminal of the 6th fluid channel and the output end of the first compressor
It is connected, the output end of the 6th fluid channel is connected with the input terminal of the 4th fluid channel；
4th heat exchanger, the 4th heat exchanger have the 7th fluid channel and the 8th fluid channel being spaced apart from each other；The
Seven fluid channel input terminals are connect with reactive distillation column tower top outlet, the input of the 7th fluid channel output end and the second compressor
End connection, the input terminal of the 8th fluid channel are connected with the output end in second fluid channel, the output end of the 8th fluid channel
It is connected with the input terminal of the first cooler；
5th heat exchanger, the 5th heat exchanger have the 9th fluid channel and the tenth fluid channel being spaced apart from each other, the
Nine fluid channel output ends are connect with recovery tower tower reactor, and the tenth fluid channel input terminal is connected with the output end of the second compressor,
Tenth fluid channel output end is connect with the second cooler；
The input terminal of preheater, the preheater is connected with first fluid channel output end；
Reactive distillation column, the reactive distillation column have the first and second feed inlet, reactive distillation column tower top outlet and reaction essence
The outlet of tower tower reactor is evaporated, the first charging aperture is connected with the output end of the preheater, the second charging aperture and the third
Fluid channel output end is connected, and the outlet of reactive distillation column tower reactor has the first output end and second output terminal, reactive distillation column tower
First output end of kettle outlet is connected with the 5th fluid channel input terminal, and the second output terminal of reactive distillation column tower reactor outlet is object
Material outlet；
The input terminal of first compressor, first compressor is connected with reactive distillation column tower top outlet；
Recovery tower, the recovery tower have third feed inlet, recovery tower tower top outlet and the outlet of recovery tower tower reactor；Described
Three feed inlets are connected with the pump output terminal, and the outlet of recovery tower tower reactor has the first output end and second output terminal, recovery tower tower
First output end of kettle outlet is connected with the 9th fluid channel input terminal, and the second output terminal of recovery tower tower reactor outlet goes out for material
Mouthful；
The input terminal of second compressor, second compressor is connected with the 7th fluid channel output end.
A kind of device of the reaction rectification technique petrohol from recuperation of heat, further includes the first cooler, and described first
Cooler input terminal is connected with the output end of the 8th fluid channel, the first cooler output end and the first pressure reducing valve input terminal
It is connected；
The input terminal of second cooler, second cooler is connected with the tenth fluid channel output end, the second cooler
Output end be connected with the second pressure reducing valve input terminal；
First pressure reducing valve, the first pressure reducing valve input terminal are connected with the first cooler output end, and described first subtracts
Pressure valve has the first output end and second output terminal, and the first output end of the first pressure reducing valve is connected with reactive distillation column overhead, the
Two output ends are connected with the pump input terminal；
Second pressure reducing valve, the second pressure reducing valve input terminal are connected with the second cooler output end, and described second subtracts
Pressure valve has the first output end and second output terminal, and the first output end of the second pressure reducing valve is connected with recycling column overhead, and second is defeated
Outlet is connected with the second charging aperture；
Pump, the pump input terminal is connected with the second output terminal of first pressure reducing valve, the pump output terminal and described the
Three feed inlets are connected.
The number of theoretical plate of the reactive distillation column is 43~53 pieces, wherein 4~8 pieces of rectifying section, 31~36 pieces of conversion zone,
Conversion zone loads cation exchange resin, can be the highly acids such as Amberlyst-15, Amberlyst-35, Amberlyst-46
Cation exchange resin, 6~10 pieces of stripping section, first charging aperture is located at the 9th~15 block of plate, and second charging aperture is located at the 22nd~
At 31 blocks of plates, operating pressure is 0.1MPa~0.11MPa, and 52~56 DEG C of tower top temperature, bottom temperature is 83~87 DEG C.
The number of theoretical plate of the recovery tower is 40~50 pieces, and third feed inlet is located at the 25th~34 block of plate, operating pressure
For 0.1MPa~0.11MPa, 52~55 DEG C of tower top temperature, bottom temperature is 59~62 DEG C.
The temperature difference >=5 DEG C of each fluid channel.The compression ratio 2.7~3.7 of first compressor, the pressure of the second compressor
Contracting is than being 1.1~2.1.
According to a kind of above-mentioned method of the reaction rectification technique petrohol from recuperation of heat, carry out as steps described below:
After raw acetic acid isopropyl ester is via First Heat Exchanger, preheater preheating, to be saturated liquid phase from reactive distillation column first
Feed inlet enters, and after material benzenemethanol is preheated via the second heat exchanger, is entered with being saturated liquid phase from reactive distillation column second charging aperture,
Two raw materials carry out ester exchange reaction, reactive distillation column under catalyzing cation exchange resin effect in reactive distillation column conversion zone
Tower kettle product is isopropanol, is produced as product.The top gaseous phase material of reactive distillation column is pressurized through the first compressor compresses and rises
Wen Hou, into third heat exchanger, provides again boiling hot amount for reactive distillation column, changes through second as reactive distillation column tower reactor heat source
Hot device exchanges heat with material benzenemethanol, then exchanges heat through First Heat Exchanger and raw acetic acid isopropyl ester, after through the 4th heat exchange
Device exchanges heat with recovery tower top gaseous phase logistics, then after the first cooler and the cooling decompression of the first pressure reducing valve, is divided into two strands,
One is back to reactive distillation column overhead, and another stock-traders' know-how pump enters progress rectifying separation in recovery tower by third feed inlet, returns
Receipts tower tower kettle product is methyl acetate, is produced as product.The top gaseous phase material of recovery tower through the 4th heat exchanger preheating after, then
It is pressurized and heats up through the second compressor compresses, provided again for recovery tower boiling hot as recovery tower tower reactor heat source into the 5th heat exchanger
Amount, then after the second cooler and the cooling decompression of the second pressure reducing valve, it is divided into two strands, one flows back into recycling column overhead, another
Stock returns to reactive distillation column from second charging aperture.
In above-mentioned steps, raw acetic acid isopropyl ester enters reactive distillation column conversion zone top, material benzenemethanol with from cooler
The methyl acetate of return enters reactive distillation column conversion zone lower part after mixing with the mixture of methanol, urges in cation exchange resin
Change effect is lower to carry out ester exchange reaction, the mixture of methyl acetate and methanol as light component from reactive distillation column overhead extraction,
Tower reactor obtains the isopropanol finished product of high-purity, and the mixture of methyl acetate and methanol from reactive distillation column overhead extraction enters back
It receives tower tower to be separated, the mixture of methyl acetate and methanol reaches azeotropic state, methyl acetate at this time after distillation operation
With the azeotropic mixture of methanol as light component from recovery tower overhead extraction, recovery tower tower reactor obtains the methyl acetate finished product of high-purity.
Compared with prior art, the invention has the following advantages that
The method of reaction rectification technique petrohol of the present invention from recuperation of heat, will be by reactive distillation column overhead
After the mixed vapour material of extraction is using compressor boost heating, institute's calorific requirement is boiled again to the offer of reactive distillation column tower reactor, simultaneously
The condensation of reactive distillation column overhead mixed vapour material itself is completed, will equally be used by the azeotropic vaporization material of recycling overhead extraction
After compressor boost heating, institute's calorific requirement is boiled again to the offer of recovery tower tower reactor, is completed at the same time recovery tower azeotropic vaporization itself condensation.
It realizes that tower top material condenses using cooling water relative to tradition, and realizes the scheme of tower reactor heating, this hair using hot public work
It is bright that self-heating recycling is realized by compressor.Furthermore conventional raw material preheating generally uses hot public work direct heating,
It will lead to the degradation of energy in this way, the preheating of raw material and intermediate product largely uses reactive distillation column and recovery tower in the present invention
Tower top material is that the waste heat after each tower heat supply increases temperature after compressor boost heats up, thus the heat in realization system
Match, the expense of energy production consumed by compressor is far below traditional cooling water and hot public work, generates good warp
Ji benefit.
Detailed description of the invention
Fig. 1 is the flow chart of the device and method of the invention from recuperation of heat reaction rectification technique petrohol
Figure label is as follows: 1- reactive distillation column, 2- recovery tower, 3- First Heat Exchanger, the second heat exchanger of 4-, 5-
Third heat exchanger, the 4th heat exchanger of 6-, the 5th heat exchanger of 7-, 8- preheater, the first compressor of 9-, 10- second compress
Machine, the first cooler of 11-, the second cooler of 12-, 13- pump, the first pressure reducing valve of 14-, the second pressure reducing valve of 15-.
Fig. 2 is the flow chart of traditional reactive distillation process of petrohol
Figure label is as follows: 1- reactive distillation column, 2- recovery tower, 3- reactive distillation column overhead condenser, 4-reactions
Tower bottom of rectifying tower reboiler, 5- recovery tower overhead condenser, the anti-tower reactor reboiler of 6- recovery tower, 7-feed preheaters, 8-
Preheater preheater, 9- pump.
Specific embodiment
A kind of device of the reaction rectification technique petrohol from recuperation of heat, comprising: First Heat Exchanger, described first changes
Hot device has the first fluid channel and second fluid channel being spaced apart from each other, and wherein the intake pipeline in first fluid channel is raw material
Feed pipe 15, the output end in first fluid channel and the input terminal of preheater connect, connecting pipeline 17；
Second heat exchanger, second heat exchanger have the third fluid channel and the 4th fluid channel being spaced apart from each other, the
The intake pipeline of four fluid channels is material feeding tube 19, the output end of the 4th fluid channel and the input terminal in second fluid channel
Connection, connecting pipeline 24；
Third heat exchanger, the third heat exchanger have the 5th fluid channel and the 6th fluid channel being spaced apart from each other, the
Five fluid channel output ends are connect with reactive distillation column tower reactor, connecting pipeline 30, the input terminal and first of the 6th fluid channel
The output end of compressor is connected, connecting pipeline 22, the input terminal phase of the output end and the 4th fluid channel of the 6th fluid channel
Even, connecting pipeline 23；
4th heat exchanger, the 4th heat exchanger have the 7th fluid channel and the 8th fluid channel being spaced apart from each other；The
Seven fluid channel input terminals are connect with reactive distillation column tower top outlet, connecting pipeline 34, the 7th fluid channel output end and
The input terminal of two compressors connects, connecting pipeline 35, the input terminal of the 8th fluid channel and the output end in second fluid channel
It is connected, the output end of connecting pipeline 25, the 8th fluid channel is connected with the input terminal of the first cooler, and connecting pipeline is
26；
5th heat exchanger, the 5th heat exchanger have the 9th fluid channel and the tenth fluid channel being spaced apart from each other, the
Nine fluid channel output ends are connect with recovery tower tower reactor, connecting pipeline 42, the tenth fluid channel input terminal and the second compressor
Output end be connected, connecting pipeline 36, the tenth fluid channel output end is connect with the second cooler, connecting pipeline 37；
The input terminal of preheater, the preheater is connected with first fluid channel output end, connecting pipeline 17；
Reactive distillation column, the reactive distillation column have the first and second feed inlet, reactive distillation column tower top outlet and reaction essence
Evaporate the outlet of tower tower reactor, the first charging aperture is connected with the output end of the preheater, connecting pipeline 18, described second into
Material mouth is connected with the third fluid channel output end, connecting pipeline 20, and the outlet of reactive distillation column tower reactor has the first output
First output end of end and second output terminal, the outlet of reactive distillation column tower reactor is connected with the 5th fluid channel input terminal, connecting tube
Line is 29, and the second output terminal of reactive distillation column tower reactor outlet is material discharge nozzle 31；
The input terminal of first compressor, first compressor is connected with reactive distillation column tower top outlet, and connecting pipeline is
21；
Recovery tower, the recovery tower have third feed inlet, recovery tower tower top outlet and the outlet of recovery tower tower reactor；Described
Three feed inlets are connected with the pump output terminal, connecting pipeline 33, and the outlet of recovery tower tower reactor is defeated with the first output end and second
First output end of outlet, the outlet of recovery tower tower reactor is connected with the 9th fluid channel input terminal, connecting pipeline 41, recovery tower tower
The second output terminal of kettle outlet is material discharge nozzle 43；
The input terminal of second compressor, second compressor is connected with the 7th fluid channel output end, and connecting pipeline is
35。
A kind of petrohol from recuperation of heat reactive distillation process, further include the first cooler, first cooler
Input terminal is connected with the output end of the 8th fluid channel, connecting pipeline 26, the first cooler output end and first decompression
Valve input terminal is connected, connecting pipeline 27；
The input terminal of second cooler, second cooler is connected with the tenth fluid channel output end, and connecting pipeline is
37, the output end of the second cooler is connected with the second pressure reducing valve input terminal, connecting pipeline 38；
First pressure reducing valve, the first pressure reducing valve input terminal are connected with the first cooler output end, and connecting pipeline is
27, first pressure reducing valve has the first output end and second output terminal, the first output end and reactive distillation of the first pressure reducing valve
Column overhead is connected, and connecting pipeline 28, second output terminal is connected with the pump input terminal, connecting pipeline 32；
Second pressure reducing valve, the second pressure reducing valve input terminal are connected with the second cooler output end, and connecting pipeline is
38, second pressure reducing valve has the first output end and second output terminal, the first output end and recovery tower tower of the second pressure reducing valve
Top is connected, and connecting pipeline 39, second output terminal is connected with the second charging aperture, connecting pipeline 40；
Pump, the pump input terminal are connected with the second output terminal of first pressure reducing valve, connecting pipeline 32, and the pump is defeated
Outlet is connected with the third feed inlet, connecting pipeline 33.
The number of theoretical plate of the reactive distillation column is 43~53 pieces, wherein 4~8 pieces of rectifying section, 31~36 pieces of conversion zone,
Conversion zone loads cation exchange resin, and 6~10 pieces of stripping section, first charging aperture is located at the 9th~15 block of plate, second charging aperture
At the 22nd~31 block of plate, operating pressure be 0.1MPa~0.11MPa, 52~56 DEG C of tower top temperature, bottom temperature be 83~
87℃。
The number of theoretical plate of the recovery tower is 40~50 pieces, and third feed inlet is located at the 25th~34 block of plate, operating pressure
For 0.1MPa~0.11MPa, 52~55 DEG C of tower top temperature, bottom temperature is 59~62 DEG C.
The temperature difference >=5 DEG C of each fluid channel.The compression ratio 2.7~3.7 of first compressor, the pressure of the second compressor
Contracting is than being 1.1~2.1.
The method for a kind of reaction rectification technique petrohol from recuperation of heat implemented according to the present invention, according to above-mentioned
It is carried out in the device of petrohol described in one, comprising the following steps:
Raw acetic acid isopropyl ester is smart from reaction through 18 to be saturated liquid phase after 16 are preheated by First Heat Exchanger 3, preheater 8
It evaporates tower first charging aperture and enters reactive distillation column 1, material benzenemethanol is after 19 by the preheating of the second heat exchanger 4, to be saturated liquid phase through 20
Enter reactive distillation column 1 from reactive distillation column second charging aperture, two raw materials are reacting under catalyzing cation exchange resin effect
Ester exchange reaction is carried out in 1 conversion zone of rectifying column, reactive distillation column tower kettle product is isopropanol material, is adopted through 31 as product
Out.The top gaseous phase material of reactive distillation column 1 is after 21 compress pressurization heating by the first compressor 9, as reactive distillation column tower
Kettle heat source, enters third heat exchanger 5 through 22, boiling hot amount is provided again for reactive distillation column 1, through 23 by the second heat exchanger 4 and raw material
Methanol exchanges heat, then is exchanged heat through 24 by First Heat Exchanger 3 and raw acetic acid isopropyl ester, after through 25 by the 4th heat exchanger
6 exchange heat with recovery tower top gaseous phase logistics, then successively cooling by the first cooler 11 and the first pressure reducing valve 14 through 26,27
After decompression, it is divided into two strands, a stock-traders' know-how 28 flows back into 1 tower top of reactive distillation column, and another stock-traders' know-how 32 passes through 33 from third by pump 13
Feed inlet enters progress rectifying separation in recovery tower 2, and recovery tower tower kettle product is methyl acetate material, adopts through 43 as product
Out.The top gaseous phase material of recovery tower is after 34 by the preheating of the 4th heat exchanger 6, then is compressed and be pressurized by the second compressor 10 through 35
Heating enters the 5th heat exchangers 7 through 36 as recovery tower tower reactor heat source, provides again boiling hot amount for recovery tower 2, then successively through 37,
After 38 by the second cooler 12 and the cooling decompression of the second pressure reducing valve 15, it is divided into two strands, a stock-traders' know-how 39 flows back into 2 tower of recovery tower
Top, another stock-traders' know-how 40 return to reactive distillation column from second charging aperture.
In the present invention, raw acetic acid isopropyl ester enters 1 conversion zone top of reactive distillation column, and material benzenemethanol is returned with from cooler
Pars infrasegmentalis is reacted into reactive distillation column 1 after the mixture mixing of the methyl acetate and methanol that return, is urged in cation exchange resin
Change effect is lower to carry out ester exchange reaction, the mixture of methyl acetate and methanol as light component from 1 overhead extraction of reactive distillation column,
Tower reactor obtains the isopropanol finished product of high-purity, and the mixture of methyl acetate and methanol from 1 overhead extraction of reactive distillation column enters
Recovery tower 2 is separated, and the mixture of methyl acetate and methanol reaches azeotropic state after distillation operation, acetic acid first at this time
The azeotropic mixture of ester and methanol as light component from 2 overhead extraction of recovery tower, 2 tower reactor of recovery tower obtain the methyl acetate of high-purity at
Product.
Refer in the present invention from heat recovery section and reactive distillation column and recovery tower overhead vapours are pressed using compressor
It is pressurized heating after contracting, then gives reactive distillation column and recovery tower tower reactor heat supply respectively, while recycling to its waste heat, is used
In the preheating of raw material and intermediate product, so that the heat in realization system matches, the defeated of engineering is shared without extraneous heat
Enter, the expense of energy production consumed by compressor is far below traditional cooling water and hot public work, generates good warp
Ji benefit.
Embodiment 1
The number of plates of reactive distillation column 1 is 48 pieces, wherein 6 pieces of rectifying section, and 34 pieces of conversion zone, conversion zone loads cation and hands over
Resin is changed, 8 pieces of stripping section, first charging aperture is located at the 11st block of plate, and second charging aperture is located at the 27th block of plate, and operating pressure is
0.1MPa, 54 DEG C of tower top temperature, bottom temperature is 85 DEG C, and the compression ratio of the first compressor 9 is 3.24.The number of plates of recovery tower 2
It is 45 pieces, third feed inlet is located at the 29th block of plate, operating pressure 0.1MPa, and 53.6 DEG C of tower top temperature, bottom temperature is
60.3 DEG C, the compression ratio of the second compressor 10 is 1.54.
The inlet amount of raw acetic acid isopropyl ester and methanol is 50kmol/h.
Raw acetic acid isopropyl ester is smart from reaction through 18 to be saturated liquid phase after 16 are preheated by First Heat Exchanger 3, preheater 8
It evaporates tower first charging aperture and enters reactive distillation column 1, material benzenemethanol is after 19 by the preheating of the second heat exchanger 4, to be saturated liquid phase through 20
Enter reactive distillation column 1 from reactive distillation column second charging aperture, two raw materials are reacting under catalyzing cation exchange resin effect
Ester exchange reaction, the isopropyl that reactive distillation column tower reactor is 99.22% through 31 extraction molar fractions are carried out in 1 conversion zone of rectifying column
Alcohol, flow 50kmol/h.The top gaseous phase material of reactive distillation column 1 through 21 by the first compressor 9 compress pressurization heating after,
As reactive distillation column tower reactor heat source, enter third heat exchangers 5 through 22, provide again boiling hot amount for reactive distillation column 1, through 23 by the
Two heat exchangers 4 exchange heat with material benzenemethanol, then are exchanged heat through 24 by First Heat Exchanger 3 and raw acetic acid isopropyl ester, later
Exchanged heat through 25 by the 4th heat exchanger 6 and recovery tower top gaseous phase logistics, then successively through 26,27 by the first cooler 11 with
After the cooling decompression of first pressure reducing valve 14, it is divided into two strands, a stock-traders' know-how 28 flows back into 1 tower top of reactive distillation column, and another plume amount is
130kmol/h, mole group become methyl acetate 79.40%, methanol 0.13% and isopropanol 20.47%, are passed through through 32 by pump 13
33 enter progress rectifying separation in recovery tower 2 from third feed inlet, and recovery tower tower reactor is 99.3% through 43 extraction molar fractions
Methyl acetate, flow 50kmol/h.The top gaseous phase material of recovery tower through 34 by the 4th heat exchanger 6 preheating after, then through 35 by
The compression pressurization heating of second compressor 10 enters the 5th heat exchanger 7 through 36, provides for recovery tower 2 as recovery tower tower reactor heat source
Boiling hot amount again, then successively it is divided into two strands, a stock-traders' know-how after 37,38 by the second cooler 12 and the cooling decompression of the second pressure reducing valve 15
39 flow back into 2 tower top of recovery tower, and another plume amount is 80kmol/h, and mole group becomes methyl acetate 67.49% and methanol
32.51%, reactive distillation column is returned from second charging aperture through 40.
When stable operation, reactive distillation column 1 and 2 tower reactor institute's calorific requirement of recovery tower are heated up by overhead vapours through compression pressurization
After provide, steam waste heat again preheats raw material and intermediate product, and external heat public work can be greatly reduced.Only preheat
Device needs 37.86kW, and the first compressor 9 needs 526.74kW, and the second compressor 10 needs 92.88kW, and system total energy consumption is
1896.71kW。
Embodiment 2
The number of plates of reactive distillation column 1 is 51 pieces, wherein 7 pieces of rectifying section, and 36 pieces of conversion zone, conversion zone loads cation and hands over
Resin is changed, 8 pieces of stripping section, first charging aperture is located at the 12nd block of plate, and second charging aperture is located at the 29th block of plate, and operating pressure is
0.1MPa, 54 DEG C of tower top temperature, bottom temperature is 86.2 DEG C, and the compression ratio of the first compressor 9 is 3.34.The column plate of recovery tower 2
Number is 42 pieces, and third feed inlet is located at the 26th block of plate, operating pressure 0.1MPa, and 53.6 DEG C of tower top temperature, bottom temperature is
59.8 DEG C, the compression ratio of the second compressor 10 is 1.54.
The inlet amount of raw acetic acid isopropyl ester and methanol is 50kmol/h.
Raw acetic acid isopropyl ester is smart from reaction through 18 to be saturated liquid phase after 16 are preheated by First Heat Exchanger 3, preheater 8
It evaporates tower first charging aperture and enters reactive distillation column 1, material benzenemethanol is after 19 by the preheating of the second heat exchanger 4, to be saturated liquid phase through 20
Enter reactive distillation column 1 from reactive distillation column second charging aperture, two raw materials are reacting under catalyzing cation exchange resin effect
Ester exchange reaction is carried out in 1 conversion zone of rectifying column, reactive distillation column tower reactor produces the isopropanol that molar fractions are 99.2% through 31,
Flow is 50kmol/h.The top gaseous phase material of reactive distillation column 1 through 21 by the first compressor 9 compress pressurization heating after, as
Reactive distillation column tower reactor heat source, enters third heat exchanger 5 through 22, provides again boiling hot amount for reactive distillation column 1, is changed through 23 by second
Hot device 4 exchanges heat with material benzenemethanol, then is exchanged heat through 24 by First Heat Exchanger 3 and raw acetic acid isopropyl ester, after through 25
It is exchanged heat by the 4th heat exchanger 6 and recovery tower top gaseous phase logistics, then successively through 26,27 by the first cooler 11 and first
After the cooling decompression of pressure reducing valve 14, it is divided into two strands, a stock-traders' know-how 28 flows back into 1 tower top of reactive distillation column, and another plume amount is
130kmol/h, mole group become methyl acetate 79.40%, methanol 0.13% and isopropanol 20.47%, are passed through through 32 by pump 13
33 enter progress rectifying separation in recovery tower 2 from third feed inlet, and recovery tower tower reactor is 99.3% through 43 extraction molar fractions
Methyl acetate, flow 50kmol/h.The top gaseous phase material of recovery tower through 34 by the 4th heat exchanger 6 preheating after, then through 35 by
The compression pressurization heating of second compressor 10 enters the 5th heat exchanger 7 through 36, provides for recovery tower 2 as recovery tower tower reactor heat source
Boiling hot amount again, then successively it is divided into two strands, a stock-traders' know-how after 37,38 by the second cooler 12 and the cooling decompression of the second pressure reducing valve 15
39 flow back into 2 tower top of recovery tower, and another plume amount is 80kmol/h, and mole group becomes methyl acetate 67.49% and methanol
32.51%, reactive distillation column is returned from second charging aperture through 40.
When stable operation, reactive distillation column 1 and 2 tower reactor institute's calorific requirement of recovery tower are heated up by overhead vapours through compression pressurization
After provide, steam waste heat again preheats raw material and intermediate product, and external heat public work can be greatly reduced.Only preheat
Device needs 37.86kW, and the first compressor 9 needs 541.16kW, and the second compressor 10 needs 92.88kW, and system total energy consumption is 1940kW.
Embodiment 3
The number of plates of reactive distillation column 1 is 45 pieces, wherein 5 pieces of rectifying section, and 33 pieces of conversion zone, conversion zone loads cation and hands over
Resin is changed, 8 pieces of stripping section, first charging aperture is located at the 10th block of plate, and second charging aperture is located at the 25th block of plate, and operating pressure is
0.1MPa, 54 DEG C of tower top temperature, bottom temperature is 84.5 DEG C, and the compression ratio of the first compressor 9 is 3.34.The column plate of recovery tower 2
Number is 48 pieces, and third feed inlet is located at the 31st block of plate, operating pressure 0.1MPa, and 53.6 DEG C of tower top temperature, bottom temperature is
60.4 DEG C, the compression ratio of the second compressor 10 is 1.64.
The inlet amount of raw acetic acid isopropyl ester and methanol is 50kmol/h.
Raw acetic acid isopropyl ester is smart from reaction through 18 to be saturated liquid phase after 16 are preheated by First Heat Exchanger 3, preheater 8
It evaporates tower first charging aperture and enters reactive distillation column 1, material benzenemethanol is after 19 by the preheating of the second heat exchanger 4, to be saturated liquid phase through 20
Enter reactive distillation column 1 from reactive distillation column second charging aperture, two raw materials are reacting under catalyzing cation exchange resin effect
Ester exchange reaction is carried out in 1 conversion zone of rectifying column, reactive distillation column tower reactor produces the isopropanol that molar fractions are 99.1% through 31,
Flow is 50kmol/h.The top gaseous phase material of reactive distillation column 1 through 21 by the first compressor 9 compress pressurization heating after, as
Reactive distillation column tower reactor heat source, enters third heat exchanger 5 through 22, provides again boiling hot amount for reactive distillation column 1, is changed through 23 by second
Hot device 4 exchanges heat with material benzenemethanol, then is exchanged heat through 24 by First Heat Exchanger 3 and raw acetic acid isopropyl ester, after through 25
It is exchanged heat by the 4th heat exchanger 6 and recovery tower top gaseous phase logistics, then successively through 26,27 by the first cooler 11 and first
After the cooling decompression of pressure reducing valve 14, it is divided into two strands, a stock-traders' know-how 28 flows back into 1 tower top of reactive distillation column, and another plume amount is
130kmol/h, mole group become methyl acetate 79.40%, methanol 0.13% and isopropanol 20.47%, are passed through through 32 by pump 13
33 enter progress rectifying separation in recovery tower 2 from third feed inlet, and recovery tower tower reactor is 99.3% through 43 extraction molar fractions
Methyl acetate, flow 50kmol/h.The top gaseous phase material of recovery tower through 34 by the 4th heat exchanger 6 preheating after, then through 35 by
The compression pressurization heating of second compressor 10 enters the 5th heat exchanger 7 through 36, provides for recovery tower 2 as recovery tower tower reactor heat source
Boiling hot amount again, then after 37,38 by the second cooler 12 and the cooling decompression of the second pressure reducing valve 15, it is divided into two strands, a stock-traders' know-how 39 is returned
Stream enters 2 tower top of recovery tower, and another plume amount is 80kmol/h, and mole group becomes methyl acetate 67.49% and methanol
32.51%, reactive distillation column is returned from second charging aperture through 40.
When stable operation, reactive distillation column 1 and 2 tower reactor institute's calorific requirement of recovery tower are heated up by overhead vapours through compression pressurization
After provide, steam waste heat again preheats raw material and intermediate product, and external heat public work can be greatly reduced.Only preheat
Device needs 37.86kW, and the first compressor 9 needs 541.16kW, and the second compressor 10 needs 92.88kW, and system total energy consumption is
1938.36kW。
Comparative example 1
A kind of traditional reactive distillation process of petrohol:
As shown in Fig. 2, traditional synthesis includes reactive distillation column 1, and recovery tower 2, reactive distillation column overhead condenser 3,
Reactive distillation column tower reactor reboiler 4, recovery tower overhead condenser 5, recovery tower tower reactor reboiler 6, the first preheater 7, second is pre-
Hot device 8 and pump 9.
Reactive distillation column 1, the reactive distillation column 1 have the first and second feed inlet, 1 tower top outlet of reactive distillation column and anti-
1 tower reactor of rectifying column is answered to export, the first charging aperture is connected with 7 output end of the first preheater, the second charging aperture and second
8 output end of preheater is connected, and the outlet of 1 tower reactor of reactive distillation column has the first output end and second output terminal, 1 tower of reactive distillation column
First output end of kettle outlet is connected with 1 tower reactor of reactive distillation column, and the second output terminal of 1 tower reactor of reactive distillation column outlet is material
Outlet；
Recovery tower 2, the recovery tower 2 have third feed inlet, 2 tower top outlet of recovery tower and the outlet of 2 tower reactor of recovery tower；Institute
It states third feed inlet to be connected with 9 output ends of pump, the outlet of 2 tower reactor of recovery tower has the first output end and second output terminal, recovery tower 2
First output end of tower reactor outlet is connected with 2 tower reactor of recovery tower, and the second output terminal of 2 tower reactor of recovery tower outlet is material outlet.
The number of plates of reactive distillation column 1 is 48 pieces, wherein 6 pieces of rectifying section, and 34 pieces of conversion zone, conversion zone loads cation and hands over
Resin is changed, 8 pieces of stripping section, first charging aperture is located at the 11st block of plate, and second charging aperture is located at the 27th block of plate, and operating pressure is
0.1MPa, 54 DEG C of tower top temperature, bottom temperature is 85 DEG C.The number of plates of recovery tower 2 is 45 pieces, and third feed inlet is located at the 29th piece
At plate, operating pressure 0.1MPa, 53.6 DEG C of tower top temperature, bottom temperature is 60.3 DEG C.
The inlet amount of raw acetic acid isopropyl ester and methanol is 50kmol/h.
Raw acetic acid isopropyl ester is after 10 by the preheating of the first preheater 7, to be saturated liquid phase through 11 from reactive distillation column first
Feed inlet enters reactive distillation column 1, and material benzenemethanol is smart from reaction through 13 to be saturated liquid phase after 12 by the preheating of the second preheater 8
It evaporates tower second charging aperture and enters reactive distillation column 1, two kinds of raw materials are under catalyzing cation exchange resin effect in reactive distillation column 1
Ester exchange reaction is carried out in conversion zone, reactive distillation column tower bottoms is divided into two parts, and a part is through 16 by reactive distillation column tower reactor
Reboiler is thermally formed boil gas again after through 17 return reactive distillation column tower reactors, another part through 18 extraction molar fractions be
99.22% isopropanol, flow 50kmol/h.1 top gaseous phase material of reactive distillation column is cold by reactive distillation column overhead through 14
Condenser 3 is divided into two strands after condensing, a stock-traders' know-how 15 reflux returns to reactive distillation column overhead, reflux ratio 2.09, another plume amount
For 130kmol/h, mole group becomes methyl acetate 79.40%, methanol 0.13% and isopropanol 20.47%, is led to through 19 by pump 9
Cross 20 and enter in recovery tower 2 progress rectifying separation from third feed inlet, recovery tower tower bottoms is divided into two parts, a part through 23 by
Reactive distillation column tower reactor reboiler is thermally formed boil gas again after through 24 return reactive distillation column tower reactors, another part through 25 extraction rub
The methyl acetate that your score is 99.3%, flow 50kmol/h.2 top gaseous phase material of recovery tower is through 21 by recycling column overhead
Condenser 5 is divided into two strands after condensing, a stock-traders' know-how 22 reflux is back to recycling column overhead, reflux ratio 1.49, another plume amount
80kmol/h, mole group become methyl acetate 67.49% and methanol 32.51%, return to reactive distillation from second charging aperture through 26
Tower.
When stable operation, the system total energy consumption of traditional handicraft is 5147.95kW.And it uses from recuperation of heat reactive distillation process
When, 50% or more the energy conservation compared with traditional handicraft.
It is can be seen that in the present invention from the above description from recuperation of heat reactive distillation process to reactive distillation column and recovery tower tower
Top steam is pressurized heating after being compressed using compressor, then gives reactive distillation column and recovery tower tower reactor heat supply respectively, replaces
Traditional handicraft low pressure steam heat supply, while recycling to the waste heat of steam after compression is used for raw material and intermediate produces
The preheating of object, reduces hot public work, the expense of energy production consumed by compressor far below traditional cooling water and
Hot public work, to significantly reduce the energy consumption from recuperation of heat reactive distillation process, compared with traditional handicraft energy conservation 50% with
On.
Claims (7)
1. a kind of device of the reactive distillation petrohol from recuperation of heat, characterized by comprising: First Heat Exchanger, described
One heat exchanger has the first fluid channel and second fluid channel being spaced apart from each other, the output end and preheater in first fluid channel
Input terminal connection；
Second heat exchanger, second heat exchanger have the third fluid channel and the 4th fluid channel being spaced apart from each other, the 4th stream
The output end in body channel is connect with the input terminal in second fluid channel；
Third heat exchanger, the third heat exchanger have the 5th fluid channel and the 6th fluid channel being spaced apart from each other, the 5th stream
Body channel output end is connect with reactive distillation column tower reactor, the output end phase of the input terminal and the first compressor of the 6th fluid channel
Even, the output end of the 6th fluid channel is connected with the input terminal of the 4th fluid channel；
4th heat exchanger, the 4th heat exchanger have the 7th fluid channel and the 8th fluid channel being spaced apart from each other；7th stream
Body path input is connect with reactive distillation column tower top outlet, and the input terminal of the 7th fluid channel output end and the second compressor connects
It connects, the input terminal of the 8th fluid channel is connected with the output end in second fluid channel, the output end of the 8th fluid channel and
The input terminal of one cooler is connected；
5th heat exchanger, the 5th heat exchanger have the 9th fluid channel and the tenth fluid channel being spaced apart from each other, the 9th stream
Body channel output end is connect with recovery tower tower reactor, and the tenth fluid channel input terminal is connected with the output end of the second compressor, and the tenth
Fluid channel output end is connect with the second cooler；
The input terminal of preheater, the preheater is connected with first fluid channel output end；
Reactive distillation column, the reactive distillation column have the first and second feed inlet, reactive distillation column tower top outlet and reactive distillation column
Tower reactor outlet, the first charging aperture are connected with the output end of the preheater, the second charging aperture and the third fluid
Channel output end is connected, and the outlet of reactive distillation column tower reactor has the first output end and second output terminal, and reactive distillation column tower reactor goes out
First output end of mouth is connected with the 5th fluid channel input terminal, and the second output terminal of reactive distillation column tower reactor outlet goes out for material
Mouthful；
The input terminal of first compressor, first compressor is connected with reactive distillation column tower top outlet；
Recovery tower, the recovery tower have third feed inlet, recovery tower tower top outlet and the outlet of recovery tower tower reactor；The third into
Material mouth is connected with the pump output terminal, and the outlet of recovery tower tower reactor has the first output end and second output terminal, and recovery tower tower reactor goes out
First output end of mouth is connected with the 9th fluid channel input terminal, and the second output terminal of recovery tower tower reactor outlet is material outlet；
The input terminal of second compressor, second compressor is connected with the 7th fluid channel output end.
2. a kind of device of the reactive distillation petrohol from recuperation of heat, further includes first cold according to claim 1
But device, the first cooler input terminal are connected with the output end of the 8th fluid channel, the first cooler output end and described the
One pressure reducing valve input terminal is connected；
The input terminal of second cooler, second cooler is connected with the tenth fluid channel output end, the second cooler it is defeated
Outlet is connected with the second pressure reducing valve input terminal；
First pressure reducing valve, the first pressure reducing valve input terminal are connected with the first cooler output end, first pressure reducing valve
With the first output end and second output terminal, the first output end of the first pressure reducing valve is connected with reactive distillation column overhead, and second is defeated
Outlet is connected with the pump input terminal；
Second pressure reducing valve, the second pressure reducing valve input terminal are connected with the second cooler output end, second pressure reducing valve
With the first output end and second output terminal, the first output end of the second pressure reducing valve is connected with recycling column overhead, second output terminal
It is connected with the second charging aperture；
Pump, the pump input terminal is connected with the second output terminal of first pressure reducing valve, the pump output terminal and the third into
Material mouth is connected.
3. a kind of device of the reactive distillation petrohol from recuperation of heat according to claim 1, it is characterised in that institute
The number of theoretical plate for stating reactive distillation column is 43~53 pieces, wherein 4~8 pieces of rectifying section, and 31~36 pieces of conversion zone, conversion zone loads sun
Ion exchange resin, 6~10 pieces of stripping section, first charging aperture is located at the 9th~15 block of plate, and second charging aperture is located at the 22nd~31
At block plate, operating pressure is 0.1MPa~0.11MPa, and 52~56 DEG C of tower top temperature, bottom temperature is 83~87 DEG C.
4. a kind of device of the reactive distillation petrohol from recuperation of heat according to claim 1, it is characterised in that institute
The number of theoretical plate for stating recovery tower is 40~50 pieces, and third feed inlet is located at the 25th~34 block of plate, operating pressure be 0.1MPa~
0.11MPa, 52~55 DEG C of tower top temperature, bottom temperature is 59~62 DEG C.
5. a kind of device of the reaction rectification technique petrohol from recuperation of heat, feature according to claim 1 exist
In the temperature difference >=5 DEG C of each fluid channel；The compression ratio 2.7~3.7 of first compressor, the compression ratio of the second compressor are
1.1~2.1.
6. according to a kind of above-mentioned method of the reactive distillation petrohol from recuperation of heat, it is characterised in that as steps described below into
Row:
After raw acetic acid isopropyl ester is via First Heat Exchanger, preheater preheating, fed with being saturated liquid phase from reactive distillation column first
Mouth enters, and after material benzenemethanol is preheated via the second heat exchanger, is entered with being saturated liquid phase from reactive distillation column second charging aperture, two is former
Material carries out ester exchange reaction, reactive distillation column tower reactor under catalyzing cation exchange resin effect in reactive distillation column conversion zone
Product is isopropanol material, is produced as product, and the top gaseous phase material of reactive distillation column is pressurized through the first compressor compresses to be risen
Wen Hou, into third heat exchanger, provides again boiling hot amount for reactive distillation column, changes through second as reactive distillation column tower reactor heat source
Hot device exchanges heat with material benzenemethanol, then exchanges heat through First Heat Exchanger and raw acetic acid isopropyl ester, after through the 4th heat exchange
Device exchanges heat with recovery tower top gaseous phase logistics, then after the first cooler and the cooling decompression of the first pressure reducing valve, is divided into two strands,
One flows back into reactive distillation column overhead, and another stock-traders' know-how pump enters progress rectifying separation in recovery tower by third feed inlet, returns
Receipts tower tower kettle product is methyl acetate material, is produced as product, and the top gaseous phase material of recovery tower is preheated through the 4th heat exchanger
Afterwards, it then is pressurized and heats up through the second compressor compresses, provided as recovery tower tower reactor heat source into the 5th heat exchanger for recovery tower
Boiling hot amount again, then after the second cooler and the cooling decompression of the second pressure reducing valve, it is divided into two strands, one flows back into recovery tower tower
Top, another stock return to reactive distillation column from second charging aperture.
7. a kind of method from recuperation of heat reactive distillation petrohol according to claim 6, it is characterised in that above-mentioned
In step, raw acetic acid isopropyl ester enters reactive distillation column conversion zone top, material benzenemethanol and the acetic acid first returned from cooler
Ester enters reactive distillation column conversion zone lower part after mixing with the mixture of methanol, carries out under catalyzing cation exchange resin effect
As light component from reactive distillation column overhead extraction, tower reactor obtains high-purity the mixture of ester exchange reaction, methyl acetate and methanol
The isopropanol finished product of degree, the mixture of methyl acetate and methanol from reactive distillation column overhead extraction enter recovery tower tower and are divided
From the mixture of methyl acetate and methanol reaches azeotropic state after distillation operation, the azeotropic of methyl acetate and methanol at this time
For object as light component from recovery tower overhead extraction, recovery tower tower reactor obtains the methyl acetate finished product of high-purity.
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| 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 |
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| CN114797147A (en) * | 2022-05-16 | 2022-07-29 | 湖南中创化工股份有限公司 | Method and device for recovering tail gas of isopropyl acetate refining tower |
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