CN103214367B - Continuous production device and method for isopropyl acetate - Google Patents
Continuous production device and method for isopropyl acetate Download PDFInfo
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- CN103214367B CN103214367B CN201310168318.6A CN201310168318A CN103214367B CN 103214367 B CN103214367 B CN 103214367B CN 201310168318 A CN201310168318 A CN 201310168318A CN 103214367 B CN103214367 B CN 103214367B
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Abstract
The invention provides a continuous production device and a continuous production method for isopropyl acetate. The continuous production method for the isopropyl acetate comprises the following steps of: continuously feeding acetic acid and isopropanol in a reactor, and carrying out an esterification reaction under the catalysis of concentrated sulfuric acid to obtain a reaction mixture; feeding the reaction mixture to a reaction rectification tower; carrying out an esterification reaction and rectification when the liquid level exceeds 4/5; feeding one part of an obtained tower-bottom mixture to the reactor, returning the rest part of the obtained tower-bottom mixture to a reaction rectification tower, and keeping the circulation; carrying out condensation and phase separation onto the obtained tower-top mixture in sequence to obtain an isopropyl acetate crude product; feeding the isopropyl acetate crude product to a finished product rectification tower for carrying out rectification and condensation to obtain an isopropyl acetate finished product. The continuous production method for the isopropyl acetate can be used for obviously increasing the front esterification reaction time, so that the ternary azeotropy of reaction rectification tower-top isopropanol, isopropyl acetate and water is relatively stable; the layered interface in the phase slitter is clear, so that the generated water can be automatically separated out, and therefore, a qualified product is obtained in thousand-ton level production.
Description
Technical field
The present invention relates to Iso Butyl Acetate production technical field, particularly a kind of continuous production device of Iso Butyl Acetate and method.
Background technology
Iso Butyl Acetate has another name called isopropyl acetate, and skeleton symbol is CH
3cOOCH(CH
3)
2.Iso Butyl Acetate is the fruity colourless transparent liquid of a kind of tool, can with the multiple immiscible organic solvents such as alcohol, ketone and ether, can be used for the industrial circles such as coating, plastics, spices, medicine and agricultural chemicals, range of application is comparatively extensive.At present, the production method of the industrial Iso Butyl Acetate generally adopted is with acetic acid and Virahol for raw material, is that catalyzer esterification obtains with sulfuric acid.
The synthesis technique of above-mentioned esterification generally has two kinds of modes, one is interrupter method, namely acetic acid and Virahol react under the effect of the vitriol oil, then through neutralization, dehydration and rectifying, obtained finished product, but, interrupter method is due to the restriction by molecular balance, feed stock conversion is not high, and long reaction time is unfavorable for suitability for industrialized production; Another kind is the continuous prodution adopting reaction distillation or reactive distillation, as application number continuous processing esterification disclosed in the Chinese patent literature of 02111177.4 prepares method and the device of isopropyl acetate, in pre-reaction zone bottom this device reaction rectifying column, a certain amount of Glacial acetic acid, Virahol and acidic substance catalyzer reacting by heating, described Glacial acetic acid and the ratio of Virahol are Glacial acetic acid: Virahol=(1.2 ~ 10): 1(mol ratio), the content of described acidic substance catalyzer is 0.01 ~ 1%(weight); Material in pre-reaction zone is extracted out continuously, and returns from the middle and upper part of reactive distillation post, circulates; Glacial acetic acid from the middle part of reactive distillation post, Virahol adds reactive system continuously from pre-reaction zone, through reaction, rectifying, continuous extraction isopropyl acetate finished product in rectifying tower.
Compared to interrupter method, the Measures compare that above-mentioned continuous processing esterification prepares isopropyl acetate is suitable for suitability for industrialized production, but, in the large suitability for industrialized production of ton, apply method that above-mentioned continuous processing esterification prepares isopropyl acetate when preparing Iso Butyl Acetate, phase splitter layering is unclear, and the water that reaction generates can not separate automatically, causes can not get qualified Iso Butyl Acetate product.
Summary of the invention
In order to solve above technical problem, the invention provides a kind of continuous production device and method of Iso Butyl Acetate, this device and method can obtain qualified Iso Butyl Acetate product when the large suitability for industrialized production of ton.
The invention provides a kind of continuous production device of Iso Butyl Acetate, comprising:
Reactor, described reactor lower part is provided with charging opening, and top is provided with discharge port;
The reactive distillation column that charging opening communicates with the discharge port of described reactor, the liquid exit of described reactive distillation column communicates with the charging opening of described reactor, and communicates with the charging opening of self;
The first condenser communicated with the pneumatic outlet of described reactive distillation column;
The first phase splitter communicated with described first condenser;
The finished product treating tower that charging opening communicates with the outlet in the middle part of described first phase splitter;
The second condenser communicated with the pneumatic outlet of described finished product treating tower;
The second phase splitter communicated with described second condenser;
The finished product condenser communicated with the discharge port of described finished product treating tower;
The pan tank communicated with described finished product condenser.
Preferably, also comprise:
The acetic acid tank communicated with the charging opening of described reactor;
By the Virahol storage tank that described finished product condenser communicates with the charging opening of described reactor.
The invention provides a kind of continuous production method of Iso Butyl Acetate, comprising:
A) continuously acetic acid and Virahol are fed to reactor, and carry out esterification wherein under the katalysis of the vitriol oil, obtain reaction mixture;
B) described reaction mixture is sent in reactive distillation column, carry out esterification and rectifying when its liquid level is more than 4/5, obtain mixture at the bottom of overhead mixture and tower;
C) part for mixture at the bottom of described tower is sent into described reactor, remainder returns described reactive distillation column, keeps circulation;
Described overhead mixture is carried out condensation, phase-splitting successively, obtains Iso Butyl Acetate crude product;
D) carry out rectifying by described Iso Butyl Acetate crude product feeding finished product treating tower, after condensation, obtain Iso Butyl Acetate finished product.
Preferably, before described acetic acid and Virahol carry out esterification in the reactor, the heat of condensation Iso Butyl Acetate finished product is utilized to preheat described Virahol.
Preferably, in described step a), the input speed of described acetic acid is 0.5m
3/ h ~ 0.6m
3/ h, the input speed of described Virahol is 0.6m
3/ h ~ 0.7m
3/ h.
Preferably, in described step b), the reflux ratio of described reactive distillation column is 9 ~ 11.
Preferably, in described step c), when the organic phase Iso Butyl Acetate content that described phase-splitting obtains is more than 92%, obtain Iso Butyl Acetate crude product.
Preferably, in described step c), by when at the bottom of described tower, a part for mixture sends into described reactor, feeding amount is 2.5m
3/ h ~ 3.5m
3/ h.
Compared with prior art, the present invention is first continuous to be sent in reactor by acetic acid and Virahol, and esterification is carried out wherein under the katalysis of the vitriol oil, then reaction mixture esterification obtained is sent in reactive distillation column, when its liquid level is more than 4/5, carry out esterification and rectifying, obtain mixture at the bottom of overhead mixture and tower, at the bottom of tower, a part for mixture returns described reactor, remainder returns described reactive distillation column, continuous circulation, and overhead mixture adopts the first condenser to carry out condensation, the first phase splitter is adopted to carry out phase-splitting again, the Iso Butyl Acetate crude product finally phase-splitting obtained is sent in finished product treating tower and is carried out rectifying, after condensation, obtain Iso Butyl Acetate finished product.Because the material of the large suitability for industrialized production of ton is more, the present invention arranges reactor before reactive distillation column, under the katalysis of the vitriol oil, acetic acid and Virahol carry out esterification in described reactor, reach certain transformation efficiency, and, the liquid level of the reaction mixture that esterification obtains in reactive distillation column more than 4/5 time, the present invention just carries out esterification and rectifying in described reactive distillation column, therefore, the present invention significantly increases the reaction time of esterification of leading portion, make isopropanol reaction complete, thus make reactive distillation column overhead Virahol, the ternary azeotropic of Iso Butyl Acetate and water is comparatively stable, in first phase splitter, layering interfaces is clear, the water that reaction generates can separate automatically, the Iso Butyl Acetate crude product obtained like this is again through rectifying, qualified Iso Butyl Acetate can be obtained.Practice shows, when apparatus and method of the present invention apply to ton large suitability for industrialized production, in gained finished product, the content of Iso Butyl Acetate is more than 99.8%.
Accompanying drawing explanation
The structural representation of the continuous production device of the Iso Butyl Acetate that Fig. 1 provides for the embodiment of the present invention.
Embodiment
In order to understand the present invention further, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these describe just for further illustrating the features and advantages of the present invention, instead of limiting to the claimed invention.
The invention provides a kind of continuous production device of Iso Butyl Acetate, comprising:
Reactor, described reactor lower part is provided with charging opening, and top is provided with discharge port;
The reactive distillation column that charging opening communicates with the discharge port of described reactor, the liquid exit of described reactive distillation column communicates with the charging opening of described reactor, and communicates with the charging opening of self;
The first condenser communicated with the pneumatic outlet of described reactive distillation column;
The first phase splitter communicated with described first condenser;
The finished product treating tower that charging opening communicates with the outlet in the middle part of described first phase splitter;
The second condenser communicated with the pneumatic outlet of described finished product treating tower;
The second phase splitter communicated with described second condenser;
The finished product condenser communicated with the discharge port of described finished product treating tower;
The pan tank communicated with described finished product condenser.
When the continuous production device of Iso Butyl Acetate provided by the invention applies to ton large suitability for industrialized production, device drives to obtain qualified product.
The continuous production device of the Iso Butyl Acetate that the embodiment of the present invention provides as shown in Figure 1, the structural representation of the continuous production device of the Iso Butyl Acetate that Fig. 1 provides for the embodiment of the present invention.
In FIG, 1 is acetic acid tank, and 2 is Virahol storage tank, 3 is reactor, and 4 is reactive distillation column, and 5 is the first reboiler, 6 is the first condenser, and 7 is the first phase splitter, and 8 is wastewater trough, 9 is crude product groove, and 10 is finished product treating tower, and 11 is the second condenser, 12 is the second phase splitter, and 13 is the first finished product condenser, and 14 is the second finished product condenser, 15 is the second reboiler, and 16 is pan tank, and 17 is light constituent groove.
In the present invention, described continuous production device comprises reactor 3, and its underpart is provided with charging opening, and top is provided with discharge port.The type of the present invention to described reactor is not particularly limited, and raw material acetic acid and Virahol enter reactor 3 from charging opening continuously, and the catalyzer vitriol oil is disposable puts into reactor 3, carries out esterification wherein.
Described continuous production device comprises reactive distillation column 4, comprises the first condenser 6 communicated with its pneumatic outlet and the first phase splitter 7 communicated with the first condenser 6 accordingly; Described pneumatic outlet is positioned at the top of reactive distillation column 4.
Be provided with charging opening in the middle part of reactive distillation column 4, bottom is provided with liquid exit, and top is provided with liquid inlet.The charging opening of reactive distillation column 4 communicates with the discharge port of reactor 3, and liquid exit communicates with the charging opening of reactor 3, and communicates with the charging opening of self.The present invention is not particularly limited described reactive distillation column, and reactive distillation column 4 can be heated by the first reboiler 5.The material that esterification obtains in reactor 3 is from reactor 3 Base top contact, in the middle part of reactive distillation column 4, enter reactive distillation column 4, when its liquid level is more than 4/5, open the first reboiler 5 steam valve, heating is started to material, heats up and carry out esterification and rectifying.Meanwhile, a part of material Returning reactor 3 bottom reactive distillation column 4, constantly circulates, and another part material is squeezed in the middle part of reactive distillation column 4 and circulated.
Along with constantly carrying out of reaction, the reaction mass in reactive distillation column 4 is from top after the first condenser 6 cools, and enter the first phase splitter 7 and carry out phase-splitting, the outlet in the middle part of the first phase splitter 7 communicates with the liquid inlet of reactive distillation column 4.In the first phase splitter 7, water, from discharging bottom it, can enter wastewater trough 8; Organic phase outlet from the center separates, when obviously there being water in the first phase splitter 7, reactive distillation column 4 head temperature is stabilized in 75 DEG C, upper organic phase turns back in reactive distillation column 4 and refluxes, when reactive distillation column 4 head temperature is more than 80 DEG C, when organic phase Iso Butyl Acetate content is more than 92%, obtain Iso Butyl Acetate crude product, it can enter crude product groove 9.
Because the material of the large suitability for industrialized production of ton is more, the present invention arranges reactor before reactive distillation column, under the katalysis of the vitriol oil, acetic acid and Virahol carry out esterification in described reactor, reach certain transformation efficiency, and, the liquid level of the reaction mixture that esterification obtains in reactive distillation column more than 4/5 time, the present invention just carries out esterification and rectifying in described reactive distillation column, therefore, the present invention significantly increases the reaction time of esterification of leading portion, make isopropanol reaction complete, thus make reactive distillation column overhead Virahol, the ternary azeotropic of Iso Butyl Acetate and water is comparatively stable, in first phase splitter, layering interfaces is clear, the water that reaction generates can separate automatically, the Iso Butyl Acetate crude product obtained like this is again through rectifying, qualified Iso Butyl Acetate can be obtained.
In the present invention, in order to crude product is refined, described continuous production device comprises finished product treating tower 10, comprise the second condenser 11 communicated with its pneumatic outlet and the second phase splitter 12 communicated with the second condenser 11 accordingly, and the finished product condenser communicated with the discharge port of finished product treating tower 10.Described pneumatic outlet is positioned at the top of finished product treating tower 10, and discharge port is positioned at the middle and lower part of finished product treating tower 10; Described finished product condenser is connected with pan tank 16.
Be provided with charging opening in the middle part of finished product treating tower 10, top is provided with liquid inlet.The charging opening of finished product treating tower 10 communicates with the outlet in the middle part of the first phase splitter 7, and the present invention is not particularly limited described finished product treating tower, and it can be heated by the second reboiler 15.The Iso Butyl Acetate crude product obtained through the first phase splitter 7 phase-splitting enters finished product treating tower 10, opens the second reboiler 15, carries out rectifying work.
In finished product treating tower 10, from finished product treating tower 10 top out, after the second condenser 11 cools, enter the second phase splitter 12 carries out phase-splitting to small portion isopropyl alcohol and water etc., and water, from discharging bottom it, also can enter wastewater trough 8; Organic phase separates from the outlet at middle part, and the light constituents such as Virahol can enter light constituent groove 17, then returns to finished product treating tower 10 top through pump major part and reflux, and small portion can turn back in crude product groove 9.
Iso Butyl Acetate finished product is extracted out from finished product treating tower 10 middle and lower part, after described finished product condenser cooling, obtains finished product, enters pan tank 16.Wherein, described finished product condenser preferably includes the first finished product condenser 13 and the second finished product condenser 14, and cooling performance is better.
The present invention is not particularly limited described condenser, phase splitter, pan tank etc., adopts the equipment that this area is conventional.
Practice shows, when device of the present invention applies to ton large suitability for industrialized production, in gained finished product, the content of Iso Butyl Acetate is more than 99.8%.
In the present invention, described continuous production device preferably also comprises the acetic acid tank 1 communicated with the charging opening of reactor 3, the Virahol storage tank 2 communicated with the charging opening of reactor 3 by finished product condenser, for the storage of raw materials, and by pump to reactor 3 charging.Wherein, the Virahol that Virahol storage tank 2 exports preferably is preheated as the first finished product condenser 13 by described finished product condenser, which reduces the consumption of heating raw steam used, decreases the consumption of the required water of finished product cooling, energy-saving and cost-reducing, is beneficial to application.
Present invention also offers a kind of continuous production method of Iso Butyl Acetate, comprising:
A) continuously acetic acid and Virahol are fed to reactor, and carry out esterification wherein under the katalysis of the vitriol oil, obtain reaction mixture;
B) described reaction mixture is sent in reactive distillation column, carry out esterification and rectifying when its liquid level is more than 4/5, obtain mixture at the bottom of overhead mixture and tower;
C) part for mixture at the bottom of described tower is sent into described reactor, remainder returns described reactive distillation column, keeps circulation;
Described overhead mixture is carried out condensation, phase-splitting successively, obtains Iso Butyl Acetate crude product;
D) carry out rectifying by described Iso Butyl Acetate crude product feeding finished product treating tower, after condensation, obtain Iso Butyl Acetate finished product.
When the continuous production method of Iso Butyl Acetate provided by the invention applies to ton large suitability for industrialized production, device is made to obtain qualified product.
The present invention first by acetic acid and Virahol continuously to charging in reactor, and carry out esterification under the katalysis of the vitriol oil, obtain reaction mixture.
The present invention for raw material with acetic acid and Virahol, is catalyzer with the vitriol oil, prepares Iso Butyl Acetate by esterification.By raw material in reactor during charging, the input speed of described acetic acid is preferably 0.5m
3/ h ~ 0.6m
3/ h, the input speed of described Virahol is preferably 0.6m
3/ h ~ 0.7m
3/ h.Described acetic acid and Virahol are about the ratio of 1:1 according to mol ratio, squeeze in reactor by pump and flow control valve; The described vitriol oil adopts conventional catalyst levels, as being 0.3% ~ 1% of raw material gross weight.
Before described acetic acid and Virahol carry out esterification in the reactor, the present invention preferably utilizes the heat of condensation Iso Butyl Acetate finished product to preheat described Virahol, which reduce the consumption of heating raw steam used, decrease the consumption of the required water of finished product cooling, energy-saving and cost-reducing, be beneficial to application.
Described raw material enters reactor from bottom feed mouth and reacts, and the temperature of described reaction is preferably 80 DEG C ~ 100 DEG C; After reaction from reactor head discharge port out, enter reactive distillation column, carry out esterification rectifying when described reactive distillation column liquid level is more than 4/5, obtain mixture at the bottom of overhead mixture and tower.
Along with constantly carrying out of reaction, in described reactive distillation column, a part of material of mixture at the bottom of tower is squeezed in described reactor by pump and is kept circulation, and internal circulating load is preferably 2.5m
3/ h ~ 3.5m
3/ h; Another part material is squeezed in the middle part of self by pump, and keep circulation, internal circulating load is preferably 2.5m
3/ h ~ 3.5m
3/ h; Overhead mixture from described reactive distillation top of tower, enters the first phase splitter and carries out phase-splitting after the first condenser condenses.
When obviously there being water in described first phase splitter, described reactive distillation column overhead temperatures is stabilized in 75 DEG C, divide and anhydrate, wastewater trough can be entered, upper organic phase turns back in described reactive distillation column, and the reflux ratio of described reactive distillation column is preferably 9 ~ 11, and the present invention adds heat and reflux ratio by control, control the temperature of tower top, prevent acetic acid from running out of from tower top;
Described reactive distillation column is constantly entered at Virahol and acetic acid, and keep in the process of circulation, when described reactive distillation column head temperature is more than 80 DEG C, organic phase Iso Butyl Acetate content in described first phase splitter preferably greater than 92% time, as organic phase composite be Virahol 3%, Iso Butyl Acetate 93%, water 4% time, obtain Iso Butyl Acetate crude product, crude product groove can be entered.
Because the material of the large suitability for industrialized production of ton is more, the present invention arranges reactor before reactive distillation column, under the katalysis of the vitriol oil, acetic acid and Virahol carry out esterification in described reactor, reach certain transformation efficiency, and, the liquid level of the reaction mixture that esterification obtains in reactive distillation column more than 4/5 time, the present invention just carries out esterification and rectifying in described reactive distillation column, therefore, the present invention significantly increases the reaction time of esterification of leading portion, make isopropanol reaction complete, thus make reactive distillation column overhead Virahol, the ternary azeotropic of Iso Butyl Acetate and water is comparatively stable, in first phase splitter, layering interfaces is clear, the water that reaction generates can separate automatically, the Iso Butyl Acetate crude product obtained like this is again through rectifying, qualified Iso Butyl Acetate can be obtained.
After obtaining Iso Butyl Acetate crude product, it returned in described reactive distillation column by a pump part and reflux, another part enters in finished product treating tower and carries out rectifying, and inlet amount is preferably 1m
3/ h ~ 2m
3/ h, after condensation, obtains Iso Butyl Acetate finished product.
Described Iso Butyl Acetate crude product, in described finished product treating tower, controls to add heat by its second reboiler, carries out rectifying work.Wherein, reflux ratio is preferably 11 ~ 13; Tower top temperature is preferably 76 DEG C ~ 80 DEG C.
From described finished product treater tower top out, after the second condenser cooling, enter the second phase splitter carries out phase-splitting to isopropyl alcohol and waters etc., water can enter wastewater trough from bottom, organic phase can enter light constituent groove, then returns tower top through pump major part and reflux, and small portion can turn back to crude product groove;
Iso Butyl Acetate finished product is extracted out from described finished product treating tower middle and lower part, after the cooling of finished product condenser, obtains finished product, enters pan tank.
Practice shows, during approach application of the present invention suitability for industrialized production large to ton, in gained finished product, the content of Iso Butyl Acetate is more than 99.8%.
In order to understand the present invention further, below in conjunction with embodiment, the continuous production device of Iso Butyl Acetate provided by the invention and method are specifically described.
Embodiment 1
The continuous production device of the Iso Butyl Acetate that the embodiment of the present invention provides as shown in Figure 1.
Open metering valve bottom acetic acid tank 1, by pump continuously by acetic acid according to 0.55m
3the speed of/h, to charging in reactor 3, opens metering valve bottom Virahol storage tank 2 simultaneously, by pump continuously by Virahol according to 0.65m
3the speed of/h is to charging in reactor 3, and described Virahol was preheated by the heat of the first finished product condenser 13 condensation finished product before charging, and in reactor 3 the disposable input 30kg vitriol oil.
Acetic acid after charging and Virahol, under the katalysis of the vitriol oil, carry out esterification in reactor 3, and temperature is 80 DEG C ~ 100 DEG C.Along with material constantly gathers in reactor 3, amass completely, draw from reactor 3 top discharge mouth, slowly entered wherein by charging opening in the middle part of reactive distillation column 4, when reactive distillation column 4 liquid level is more than 4/5, open the first reboiler 5 steam valve, heating is started to material, carries out esterification and rectifying, open the recycle pump bottom reactive distillation column 4 simultaneously, a part of material in reactive distillation column 4 at the bottom of tower is squeezed in reactor 3, constantly circulates, internal circulating load is 3m
3/ h.
Along with constantly carrying out of reaction, reaction mass is from condenser 6 condensation of reactive distillation column 4 top first, enter the first phase splitter 7 and carry out phase-splitting, when obviously there being water in the first phase splitter 7, reactive distillation column 4 tower top temperature is stabilized in 75 DEG C, divides and anhydrates, water is discharged bottom the first phase splitter 7, enter wastewater trough 8, upper organic phase turns back in reactive distillation column 4, and the reflux ratio of reactive distillation column 4 is 10; Reactive distillation column 4 is constantly entered at Virahol and acetic acid, and keep in the process of circulation, when reactive distillation column 4 head temperature is more than 80 DEG C, when organic phase Iso Butyl Acetate content in first phase splitter 7 is more than 92%, obtain Iso Butyl Acetate crude product, enter crude product groove 9, organic phase consists of Virahol 3%, Iso Butyl Acetate 93%, water 4%.
Returned in reactive distillation column 4 by a pump part by the Iso Butyl Acetate crude product obtained and reflux, another part is according to 1.5m
3the inlet amount of/h, sends constantly in finished product treating tower 10, and open the second reboiler 15 of finished product treating tower 10, carry out rectifying work, reflux ratio is 12, and tower top temperature is 76 DEG C ~ 80 DEG C.The organic phase of finished product treating tower 10 overhead extraction is through the second condenser 11 condensation, the second phase splitter 12 phase-splitting, water enters wastewater trough 8 from bottom, organic phase is introduced into light constituent groove 17, then returns through pump major part that finished product treating tower 10 tower top refluxes, small portion turns back in crude product groove 9; Finished product treating tower 10 middle and lower part discharge hole for discharge, after the first finished product condenser 13, second finished product condenser 14 condensation, per hour can extraction 1m
3iso Butyl Acetate finished product, enter pan tank 16, Iso Butyl Acetate content>=99.9% in finished product, acetic acid content≤0.005%.
As seen from the above embodiment, when apparatus and method of the present invention apply to ton large suitability for industrialized production, in gained finished product, the content of Iso Butyl Acetate is more than 99.8%, and namely the present invention can obtain qualified Iso Butyl Acetate product.
The explanation of above embodiment just understands method of the present invention and core concept thereof for helping.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improve and modify and also fall in the protection domain of the claims in the present invention.
Claims (6)
1. a continuous production method for Iso Butyl Acetate, comprising:
A) continuously acetic acid and Virahol are fed to reactor, and carry out esterification wherein under the katalysis of the vitriol oil, obtain reaction mixture;
B) described reaction mixture is sent in reactive distillation column, carry out esterification and rectifying when its liquid level is more than 4/5, obtain mixture at the bottom of overhead mixture and tower;
C) part for mixture at the bottom of described tower is sent into described reactor, remainder returns described reactive distillation column, keeps circulation;
Described overhead mixture is carried out condensation, phase-splitting successively, obtains Iso Butyl Acetate crude product;
D) carry out rectifying by described Iso Butyl Acetate crude product feeding finished product treating tower, after condensation, obtain Iso Butyl Acetate finished product.
2. continuous production method according to claim 1, is characterized in that, before described acetic acid and Virahol carry out esterification in the reactor, utilizes the heat of condensation Iso Butyl Acetate finished product to preheat described Virahol.
3. continuous production method according to claim 1, is characterized in that, described step a) in, the input speed of described acetic acid is 0.5m
3/ h ~ 0.6m
3/ h, the input speed of described Virahol is 0.6m
3/ h ~ 0.7m
3/ h.
4. continuous production method according to claim 1, is characterized in that, described step b) in, the reflux ratio of described reactive distillation column is 9 ~ 11.
5. continuous production method according to claim 1, is characterized in that, described step c) in, when the organic phase Iso Butyl Acetate content that described phase-splitting obtains is more than 92%, obtain Iso Butyl Acetate crude product.
6. continuous production method according to claim 1, is characterized in that, described step c) in, by when at the bottom of described tower, a part for mixture sends into described reactor, feeding amount is 2.5m
3/ h ~ 3.5m
3/ h.
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| CN104592018B (en) * | 2015-01-04 | 2016-06-29 | 烟台四通橡胶有限责任公司 | A kind of method of reaction-reaction strengthening synthesis of acetic acid isopropyl ester |
| CN105061147A (en) * | 2015-07-17 | 2015-11-18 | 济南大学 | Batch distillation process for separating isopropanol-isopropyl acetate azeotrope through mixed extraction agent |
| CN106955500B (en) * | 2017-04-05 | 2019-07-02 | 青岛科技大学 | A kind of three tower is thermally integrated the method and device of variable-pressure rectification purifying acetic acid isopropyl ester |
| CN111807959A (en) * | 2020-07-21 | 2020-10-23 | 浙江建业化工股份有限公司 | Energy-saving process and process equipment for n-propyl acetate |
| CN115322219A (en) * | 2022-08-22 | 2022-11-11 | 青岛科技大学 | Continuous production system and method for isopropyl titanate |
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