CN103214367A - Continuous production device and method for isopropyl acetate - Google Patents
Continuous production device and method for isopropyl acetate Download PDFInfo
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- CN103214367A CN103214367A CN2013101683186A CN201310168318A CN103214367A CN 103214367 A CN103214367 A CN 103214367A CN 2013101683186 A CN2013101683186 A CN 2013101683186A CN 201310168318 A CN201310168318 A CN 201310168318A CN 103214367 A CN103214367 A CN 103214367A
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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 the Iso Butyl Acetate production technical field, particularly a kind of serialization production equipment and method of Iso Butyl Acetate.
Background technology
Iso Butyl Acetate has another name called isopropyl acetate, and skeleton symbol is CH
3COOCH(CH
3)
2Iso Butyl Acetate is a kind of colourless transparent liquid with fruit aroma, can with multiple immiscible organic solvents such as alcohol, ketone and ether, can be used for 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 that generally adopts is to be raw material with acetic acid and Virahol, makes for the catalyzer esterification with sulfuric acid.
The synthesis technique of above-mentioned esterification generally has dual mode, a kind of is interrupter method, be that acetic acid and Virahol react under the effect of the vitriol oil, through neutralization, dehydration and rectifying, make finished product then, still, interrupter method is owing to be subjected to the restriction of molecular balance, feed stock conversion is not high, and long reaction time is unfavorable for suitability for industrialized production; Another kind is the serialization production of adopting reaction distillation or reactive distillation, as application number is method and the device that 02111177.4 the disclosed continuous processing esterification of Chinese patent literature prepares isopropyl acetate, in the pre-reaction zone of this device reaction rectifying column bottom, a certain amount of Glacial acetic acid, Virahol and acidic substance catalyzer reacting by heating, the ratio of described Glacial acetic acid and Virahol is a Glacial acetic acid: Virahol=(1.2～10): the 1(mol ratio), the content of described acidic substance catalyzer is 0.01～1%(weight); Material in the pre-reaction zone is extracted out continuously, and returns from the middle and upper part of reactive distillation post, circulates; Glacial acetic acid adds reactive system from middle part, the Virahol of reactive distillation post continuously from pre-reaction zone, through reaction, rectifying, and continuous extraction isopropyl acetate finished product in rectifying tower.
Than interrupter method, the method that above-mentioned continuous processing esterification prepares isopropyl acetate relatively is suitable for suitability for industrialized production, but, in the big suitability for industrialized production of ton, when using method that above-mentioned continuous processing esterification prepares isopropyl acetate and preparing Iso Butyl Acetate, the phase splitter layering is unclear, and the water that reaction generates can not be told 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 serialization production equipment and method of Iso Butyl Acetate, this device and method can obtain qualified Iso Butyl Acetate product when the big suitability for industrialized production of ton.
The invention provides a kind of serialization production equipment of Iso Butyl Acetate, comprising:
Reactor, described reactor lower part is provided with charging opening, and the top is provided with discharge port;
The reaction fractionating tower that charging opening communicates with the discharge port of described reactor, the liquid exit of described reaction fractionating tower communicates with the charging opening of described reactor, and communicates with the charging opening of self;
First condenser that communicates with the pneumatic outlet of described reaction fractionating tower;
First phase splitter that communicates with described first condenser;
The finished product treating tower that charging opening communicates with the outlet at described first phase splitter middle part;
Second condenser that communicates with the pneumatic outlet of described finished product treating tower;
Second phase splitter that communicates with described second condenser;
The finished product condenser that communicates with the discharge port of described finished product treating tower;
The pan tank that communicates with described finished product condenser.
Preferably, also comprise:
The acetic acid tank that communicates with the charging opening of described reactor;
The Virahol storage tank that communicates with the charging opening of described reactor by described finished product condenser.
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 under the katalysis of the vitriol oil, carry out esterification therein, obtain reaction mixture;
B) described reaction mixture is sent in the reaction fractionating tower, when its liquid level surpasses 4/5, carried out esterification and rectifying, obtain mixture at the bottom of overhead mixture and the tower;
C) part of mixture at the bottom of the described tower is sent into described reactor, remainder returns described reaction fractionating tower, keeps circulation;
Described overhead mixture is carried out condensation, phase-splitting successively, obtain the Iso Butyl Acetate crude product;
D) described Iso Butyl Acetate crude product is sent into carried out rectifying in the finished product treating tower, after condensation, obtain the Iso Butyl Acetate finished product.
Preferably, described acetic acid and Virahol carry out in reactor before the esterification, utilize the heat of condensation Iso Butyl Acetate finished product that described Virahol is preheated.
Preferably, in the 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 the described step b), the reflux ratio of described reaction fractionating tower is 9～11.
Preferably, in the described step c), the organic phase Iso Butyl Acetate content that described phase-splitting obtains surpasses at 92% o'clock, obtains the Iso Butyl Acetate crude product.
Preferably, in the described step c), when the part of mixture at the bottom of the described tower was sent into described reactor, the amount of sending into was 2.5m
3/ h～3.5m
3/ h.
Compared with prior art, the present invention sends into acetic acid and Virahol in the reactor at first continuously, and under the katalysis of the vitriol oil, carry out esterification therein, the reaction mixture that esterification is obtained is sent in the reaction fractionating tower then, when its liquid level surpasses 4/5, carry out esterification and rectifying, obtain mixture at the bottom of overhead mixture and the tower, the part of mixture is returned described reactor at the bottom of the tower, remainder returns described reaction fractionating tower, constantly circulation, and overhead mixture adopts first condenser to carry out condensation, adopts first phase splitter to carry out phase-splitting again, and the Iso Butyl Acetate crude product that at last phase-splitting is obtained is sent into and carried out rectifying in the finished product treating tower, after condensation, obtain the Iso Butyl Acetate finished product.Because the material of the big suitability for industrialized production of ton is more, the present invention is provided with reactor before reaction fractionating tower, 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 reaction mixture in reaction fractionating tower that obtains in esterification was above 4/5 o'clock, the present invention just carries out esterification and rectifying in described reaction fractionating tower, therefore, the present invention has obviously increased the reaction time of esterification of leading portion, makes isopropanol reaction complete, thereby makes reactive distillation column overhead Virahol, the ternary azeotropic of Iso Butyl Acetate and water is comparatively stable, layering interfaces is clear in first phase splitter, the water that reaction generates can be told automatically, and the Iso Butyl Acetate crude product that obtains like this passes through rectifying again, can obtain qualified Iso Butyl Acetate.Practice shows, when apparatus and method of the present invention applied to the big suitability for industrialized production of ton, the content of Iso Butyl Acetate was more than 99.8% in the gained finished product.
Description of drawings
The structural representation of the serialization production equipment of the Iso Butyl Acetate that Fig. 1 provides for the embodiment of the invention.
Embodiment
In order further to understand the present invention, below in conjunction with embodiment the preferred embodiment of the invention is described, but should be appreciated that these describe just to further specifying the features and advantages of the present invention, rather than to the restriction of claim of the present invention.
The invention provides a kind of serialization production equipment of Iso Butyl Acetate, comprising:
Reactor, described reactor lower part is provided with charging opening, and the top is provided with discharge port;
The reaction fractionating tower that charging opening communicates with the discharge port of described reactor, the liquid exit of described reaction fractionating tower communicates with the charging opening of described reactor, and communicates with the charging opening of self;
First condenser that communicates with the pneumatic outlet of described reaction fractionating tower;
First phase splitter that communicates with described first condenser;
The finished product treating tower that charging opening communicates with the outlet at described first phase splitter middle part;
Second condenser that communicates with the pneumatic outlet of described finished product treating tower;
Second phase splitter that communicates with described second condenser;
The finished product condenser that communicates with the discharge port of described finished product treating tower;
The pan tank that communicates with described finished product condenser.
When the serialization production equipment of Iso Butyl Acetate provided by the invention applied to the big suitability for industrialized production of ton, device drove to obtain qualified product.
The serialization production equipment of the Iso Butyl Acetate that the embodiment of the invention provides as shown in Figure 1, the structural representation of the serialization production equipment of the Iso Butyl Acetate that Fig. 1 provides for the embodiment of the invention.
In Fig. 1,1 is acetic acid tank, and 2 is the Virahol storage tank, 3 is reactor, and 4 is reaction fractionating tower, and 5 is first reboiler, 6 is first condenser, and 7 is first phase splitter, and 8 is wastewater trough, 9 is the crude product groove, and 10 is the finished product treating tower, and 11 is second condenser, 12 is second phase splitter, and 13 is the first finished product condenser, and 14 is the second finished product condenser, 15 is second reboiler, and 16 is pan tank, and 17 is the light constituent groove.
In the present invention, described serialization production equipment comprises reactor 3, and its underpart is provided with charging opening, and the top is provided with discharge port.The present invention does not have particular restriction to the type of described reactor, and raw material acetic acid and Virahol enter reactor 3 from charging opening continuously, and the disposable reactor 3 of putting into of the catalyzer vitriol oil carries out esterification therein.
Described serialization production equipment comprises reaction fractionating tower 4, comprises first condenser 6 that communicates with its pneumatic outlet and first phase splitter 7 that communicates with first condenser 6 accordingly; Described pneumatic outlet is positioned at the top of reaction fractionating tower 4.
Reaction fractionating tower 4 middle parts are provided with charging opening, and the bottom is provided with liquid exit, and top is provided with the liquid inlet.The charging opening of reaction fractionating tower 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 does not have particular restriction to described reaction fractionating tower, and reaction fractionating tower 4 can be heated by first reboiler 5.The material that esterification obtains in reactor 3 is drawn from reactor 3 tops, enter reaction fractionating tower 4 from reaction fractionating tower 4 middle parts, when its liquid level surpasses 4/5, open first reboiler, 5 steam valves, material is begun heating, heat up and carry out esterification and rectifying.Simultaneously, a part of material Returning reactor 3 of reaction fractionating tower 4 bottoms, constantly circulation, another part material is squeezed into reaction fractionating tower 4 middle parts and is circulated.
Along with constantly carrying out of reaction, the reaction mass in the reaction fractionating tower 4, enters first phase splitter 7 and carries out phase-splitting after 6 coolings of first condenser from the top, and the outlet at first phase splitter, 7 middle parts communicates with the liquid inlet of reaction fractionating tower 4.In first phase splitter 7, water is discharged from its bottom, can enter wastewater trough 8; Organic phase outlet is from the center told, when obviously water being arranged in first phase splitter 7, reaction fractionating tower 4 head temperature are stabilized in 75 ℃, upper organic phase turns back in the reaction fractionating tower 4 and refluxes, when reaction fractionating tower 4 head temperature above 80 ℃, organic phase Iso Butyl Acetate content surpasses at 92% o'clock, obtains the Iso Butyl Acetate crude product, and it can enter crude product groove 9.
Because the material of the big suitability for industrialized production of ton is more, the present invention is provided with reactor before reaction fractionating tower, 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 reaction mixture in reaction fractionating tower that obtains in esterification was above 4/5 o'clock, the present invention just carries out esterification and rectifying in described reaction fractionating tower, therefore, the present invention has obviously increased the reaction time of esterification of leading portion, makes isopropanol reaction complete, thereby makes reactive distillation column overhead Virahol, the ternary azeotropic of Iso Butyl Acetate and water is comparatively stable, layering interfaces is clear in first phase splitter, the water that reaction generates can be told automatically, and the Iso Butyl Acetate crude product that obtains like this passes through rectifying again, can obtain qualified Iso Butyl Acetate.
In the present invention, for crude product is made with extra care, described serialization production equipment comprises finished product treating tower 10, comprise second condenser 11 that communicates with its pneumatic outlet and second phase splitter 12 that communicates with second condenser 11 accordingly, and the finished product condenser that communicates 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.
Finished product treating tower 10 middle parts are provided with charging opening, and top is provided with the liquid inlet.The charging opening of finished product treating tower 10 communicates with the outlet at first phase splitter, 7 middle parts, and the present invention does not have particular restriction to described finished product treating tower, and it can be heated by second reboiler 15.The Iso Butyl Acetate crude product that obtains through 7 phase-splittings of first phase splitter enters finished product treating tower 10, opens second reboiler 15, carries out rectifying work.
In finished product treating tower 10, small portion Virahol and water etc. come out from finished product treating tower 10 tops, and after 11 coolings of second condenser, entering second phase splitter 12 carries out phase-splitting, and water is discharged from its bottom, also can enter wastewater trough 8; Organic phase is told from the outlet at middle part, and light constituents such as Virahol can enter light constituent groove 17, returns finished product treating tower 10 tops through the pump major part again and refluxes, and small portion can turn back in the crude product groove 9.
The Iso Butyl Acetate finished product is extracted out from finished product treating tower 10 middle and lower parts, 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 does not have particular restriction to described condenser, phase splitter, pan tank etc., adopts this area equipment commonly used to get final product.
Practice shows, when device of the present invention applied to the big suitability for industrialized production of ton, the content of Iso Butyl Acetate was more than 99.8% in the gained finished product.
In the present invention, the Virahol storage tank 2 that described serialization production equipment preferably also comprises the acetic acid tank 1 that communicates with the charging opening of reactor 3, communicates with the charging opening of reactor 3 by the finished product condenser, be used for the storage of raw materials, and can be by pump to reactor 3 chargings.Wherein, the Virahol of Virahol storage tank 2 outputs is preferably preheated as the first finished product condenser 13 by described finished product condenser, has reduced the consumption of the used steam of heating raw like this, has also reduced the consumption that finished product cools off required water, and is energy-saving and cost-reducing, is beneficial to application.
The present invention also provides a kind of continuous production method of Iso Butyl Acetate, comprising:
A) continuously acetic acid and Virahol are fed to reactor, and under the katalysis of the vitriol oil, carry out esterification therein, obtain reaction mixture;
B) described reaction mixture is sent in the reaction fractionating tower, when its liquid level surpasses 4/5, carried out esterification and rectifying, obtain mixture at the bottom of overhead mixture and the tower;
C) part of mixture at the bottom of the described tower is sent into described reactor, remainder returns described reaction fractionating tower, keeps circulation;
Described overhead mixture is carried out condensation, phase-splitting successively, obtain the Iso Butyl Acetate crude product;
D) described Iso Butyl Acetate crude product is sent into carried out rectifying in the finished product treating tower, after condensation, obtain the Iso Butyl Acetate finished product.
When the continuous production method of Iso Butyl Acetate provided by the invention applies to the big suitability for industrialized production of ton, make device obtain qualified product.
The present invention is at first with acetic acid and Virahol charging in reactor continuously, and carries out esterification under the katalysis of the vitriol oil, obtains reaction mixture.
The present invention is a raw material with acetic acid and Virahol, is catalyzer with the vitriol oil, prepares Iso Butyl Acetate by esterification.In reactor during charging, the input speed of described acetic acid is preferably 0.5m with raw material
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 the reactor by pump and flow control valve; The described vitriol oil adopts catalyst levels commonly used, as is that 0.3%～1% of raw material gross weight gets final product.
Described acetic acid and Virahol carry out before the esterification in reactor, the present invention preferably utilizes the heat of condensation Iso Butyl Acetate finished product that described Virahol is preheated, reduced the consumption of the used steam of heating raw like this, also reduced the consumption that finished product cools off required water, energy-saving and cost-reducing, be beneficial to application.
Described raw material enters the reactor from the bottom feed mouth and reacts, and the temperature of described reaction is preferably 80 ℃～100 ℃; Coming out from the reactor head discharge port in reaction back, enters reaction fractionating tower, carries out esterification rectifying when described reaction fractionating tower liquid level surpasses 4/5, obtains mixture at the bottom of overhead mixture and the tower.
Along with constantly carrying out of reaction, in the described reaction fractionating tower at the bottom of the tower a part of material of mixture squeeze in the described reactor by pump and keep circulation, internal circulating load is preferably 2.5m
3/ h～3.5m
3/ h; Another part material is squeezed into self middle part by pump, keeps circulation, and internal circulating load is preferably 2.5m
3/ h～3.5m
3/ h; Overhead mixture, enters first phase splitter and carries out phase-splitting after first condenser condenses from described reactive distillation top of tower.
When obviously water being arranged in described first phase splitter, described reaction fractionating tower tower top temperature is stabilized in 75 ℃, divide and anhydrate, can enter wastewater trough, upper organic phase turns back in the described reaction fractionating tower, and the reflux ratio of described reaction fractionating tower is preferably 9～11, and the present invention adds heat and reflux ratio by control, control the temperature of cat head, prevent that acetic acid from running out of from cat head;
Constantly enter described reaction fractionating tower at Virahol and acetic acid, and keep in the round-robin process, when described reaction fractionating tower head temperature above 80 ℃, organic phase Iso Butyl Acetate content in described first phase splitter is preferably above 92% o'clock, when being Virahol 3%, Iso Butyl Acetate 93%, water 4% as organic phase composite, obtain the Iso Butyl Acetate crude product, can enter the crude product groove.
Because the material of the big suitability for industrialized production of ton is more, the present invention is provided with reactor before reaction fractionating tower, 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 reaction mixture in reaction fractionating tower that obtains in esterification was above 4/5 o'clock, the present invention just carries out esterification and rectifying in described reaction fractionating tower, therefore, the present invention has obviously increased the reaction time of esterification of leading portion, makes isopropanol reaction complete, thereby makes reactive distillation column overhead Virahol, the ternary azeotropic of Iso Butyl Acetate and water is comparatively stable, layering interfaces is clear in first phase splitter, the water that reaction generates can be told automatically, and the Iso Butyl Acetate crude product that obtains like this passes through rectifying again, can obtain qualified Iso Butyl Acetate.
After obtaining the Iso Butyl Acetate crude product, it is returned in the described reaction fractionating tower by a pump part reflux, another part enters and carries out rectifying in the finished product treating tower, and inlet amount is preferably 1m
3/ h～2m
3/ h after condensation, obtains the Iso Butyl Acetate finished product.
Described Iso Butyl Acetate crude product adds heat by its second reboiler control in described finished product treating tower, carry out rectifying work.Wherein, reflux ratio is preferably 11～13; Tower top temperature is preferably 76 ℃～80 ℃.
Virahol and water etc. come out from described finished product treater cat head, after the cooling of second condenser, enter second phase splitter and carry out phase-splitting, water can enter wastewater trough from the bottom, organic phase can enter the light constituent groove, returns cat head through the pump major part again and refluxes, and small portion can turn back to the crude product groove;
The 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, when method of the present invention applied to the big suitability for industrialized production of ton, the content of Iso Butyl Acetate was more than 99.8% in the gained finished product.
In order further to understand the present invention, the serialization production equipment and the method for Iso Butyl Acetate provided by the invention are specifically described below in conjunction with embodiment.
Embodiment 1
The serialization production equipment of the Iso Butyl Acetate that the embodiment of the invention provides as shown in Figure 1.
Open acetic acid tank 1 bottom metering valve, by pump continuously with acetic acid according to 0.55m
3Virahol storage tank 2 bottom metering valves are opened in the charging in reactor 3 of the speed of/h simultaneously, by pump continuously with Virahol according to 0.65m
3The charging in reactor 3 of the speed of/h, described Virahol were preheated by the heat of the first finished product condenser, 13 condensation finished products before charging, and in reactor 3 the disposable input 30kg vitriol oil.
Acetic acid after the charging and Virahol carry out esterification in reactor 3 under the katalysis of the vitriol oil, temperature is 80 ℃～100 ℃.Along with material constantly gathers in reactor 3, after long-pending expiring, draw, slowly enter wherein by reaction fractionating tower 4 middle part charging openings from reactor 3 top discharge mouths, when reaction fractionating tower 4 liquid levels surpass 4/5, open first reboiler, 5 steam valves, material is begun heating, carry out esterification and rectifying, open the recycle pump of reaction fractionating tower 4 bottoms simultaneously, a part of material at the bottom of the tower in the reaction fractionating tower 4 is squeezed in the reactor 3, constantly circulation, internal circulating load is 3m
3/ h.
Along with constantly carrying out of reaction, reaction mass is from first condenser, 6 condensations of reaction fractionating tower 4 tops, enter first phase splitter 7 and carry out phase-splitting, when obviously water being arranged in first phase splitter 7, reaction fractionating tower 4 tower top temperatures are stabilized in 75 ℃, and branch anhydrates, water is discharged from first phase splitter, 7 bottoms, enter wastewater trough 8, upper organic phase turns back in the reaction fractionating tower 4, and the reflux ratio of reaction fractionating tower 4 is 10; Constantly enter reaction fractionating tower 4 at Virahol and acetic acid, and keep in the round-robin process, when reaction fractionating tower 4 head temperature above 80 ℃, organic phase Iso Butyl Acetate content in first phase splitter 7 was above 92% o'clock, obtain the Iso Butyl Acetate crude product, enter crude product groove 9, organic phase consists of Virahol 3%, Iso Butyl Acetate 93%, water 4%.
The Iso Butyl Acetate crude product that obtains returned in the reaction fractionating tower 4 by a pump part reflux, another part is according to 1.5m
3The inlet amount of/h is sent constantly in the finished product treating tower 10, opens second reboiler 15 of finished product treating tower 10, carries out rectifying work, and reflux ratio is 12, and tower top temperature is 76 ℃～80 ℃.The organic phase of finished product treating tower 10 cat head extraction is through 11 condensations of second condenser, 12 phase-splittings of second phase splitter, water enters wastewater trough 8 from the bottom, organic phase is introduced into light constituent groove 17, returns through the pump major part that finished product treating tower 10 cats head do to reflux, small portion turns back in the crude product groove 9 again; Finished product treating tower 10 middle and lower part discharge hole for discharge, after the first finished product condenser 13,14 condensations of the second finished product condenser, but extraction 1m per hour
3The Iso Butyl Acetate finished product, enter pan tank 16, Iso Butyl Acetate content 〉=99.9% in the finished product, acetic acid content≤0.005%.
As seen from the above embodiment, when apparatus and method of the present invention applied to the big suitability for industrialized production of ton, the content of Iso Butyl Acetate was more than 99.8% in the gained finished product, i.e. the present invention can obtain qualified Iso Butyl Acetate product.
The explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of claim of the present invention.
Claims (8)
1. the serialization production equipment of an Iso Butyl Acetate comprises:
Reactor, described reactor lower part is provided with charging opening, and the top is provided with discharge port;
The reaction fractionating tower that charging opening communicates with the discharge port of described reactor, the liquid exit of described reaction fractionating tower communicates with the charging opening of described reactor, and communicates with the charging opening of self;
First condenser that communicates with the pneumatic outlet of described reaction fractionating tower;
First phase splitter that communicates with described first condenser;
The finished product treating tower that charging opening communicates with the outlet at described first phase splitter middle part;
Second condenser that communicates with the pneumatic outlet of described finished product treating tower;
Second phase splitter that communicates with described second condenser;
The finished product condenser that communicates with the discharge port of described finished product treating tower;
The pan tank that communicates with described finished product condenser.
2. serialization production equipment according to claim 1 is characterized in that, also comprises:
The acetic acid tank that communicates with the charging opening of described reactor;
The Virahol storage tank that communicates with the charging opening of described reactor by described finished product condenser.
3. the continuous production method of an Iso Butyl Acetate comprises:
A) continuously acetic acid and Virahol are fed to reactor, and under the katalysis of the vitriol oil, carry out esterification therein, obtain reaction mixture;
B) described reaction mixture is sent in the reaction fractionating tower, when its liquid level surpasses 4/5, carried out esterification and rectifying, obtain mixture at the bottom of overhead mixture and the tower;
C) part of mixture at the bottom of the described tower is sent into described reactor, remainder returns described reaction fractionating tower, keeps circulation;
Described overhead mixture is carried out condensation, phase-splitting successively, obtain the Iso Butyl Acetate crude product;
D) described Iso Butyl Acetate crude product is sent into carried out rectifying in the finished product treating tower, after condensation, obtain the Iso Butyl Acetate finished product.
4. continuous production method according to claim 3 is characterized in that, described acetic acid and Virahol carry out in reactor before the esterification, utilizes the heat of condensation Iso Butyl Acetate finished product that described Virahol is preheated.
5. continuous production method according to claim 3 is characterized in that, in the 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.
6. continuous production method according to claim 3 is characterized in that, in the described step b), the reflux ratio of described reaction fractionating tower is 9～11.
7. continuous production method according to claim 3 is characterized in that, in the described step c), the organic phase Iso Butyl Acetate content that described phase-splitting obtains surpasses at 92% o'clock, obtains the Iso Butyl Acetate crude product.
8. continuous production method according to claim 3 is characterized in that, in the described step c), when the part of mixture at the bottom of the described tower was sent into described reactor, the amount of sending into was 2.5m
3/ h～3.5m
3/ h.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| 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 |
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| 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104592018A (en) * | 2015-01-04 | 2015-05-06 | 烟台四通橡胶有限责任公司 | Method for synthesizing isopropyl acetate by means of reaction-reaction reinforcement |
| 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 |
| CN106955500A (en) * | 2017-04-05 | 2017-07-18 | 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 |
| 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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