CN110437064A - A kind of differential pressure type energy-saving processing technique of ethyl acetate - Google Patents
A kind of differential pressure type energy-saving processing technique of ethyl acetate Download PDFInfo
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- CN110437064A CN110437064A CN201910670526.3A CN201910670526A CN110437064A CN 110437064 A CN110437064 A CN 110437064A CN 201910670526 A CN201910670526 A CN 201910670526A CN 110437064 A CN110437064 A CN 110437064A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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Abstract
The invention discloses a kind of differential pressure type energy-saving processing techniques of ethyl acetate, using ethyl alcohol and acetic acid as raw material, acetic acid is reacting after the top material-heat-exchanging with esterification column into reboiler and reaction kettle with ethyl alcohol, subsequently into the Esterification separation tower of normal pressure, the taking-up of dehydrating agent side line is carried out in the tower of Esterification separation tower, discharging carries out condensation split-phase after tower top and the raw material heat exchange of Esterification separation tower, aqueous-phase reflux, heat exchange is through entering the rectifying concentration tower of pressurization after oil is mutually pressurized, in the tower reactor output acetic acid esters finished product of rectifying concentration tower；The overhead vapours of rectifying concentration tower are used to heat the material of reaction kettle and the feed material of rectifying concentration tower.The differential pressure type energy-saving processing technique of ethyl acetate of the present invention has the characteristics that the consumption that product purity is high, energy consumption is saved and unit consumption is at low cost.
Description
Technical field
The present invention relates to ethyl acetate fabricating technology field, the differential pressure type production energy-saving of especially a kind of ethyl acetate
Technique.
Background technique
Ethyl acetate is a kind of fruity solvent product, is widely used in chemical industry, is a kind of commonization
Work basic product, currently, the industrial process of ethyl acetate mainly has: esterification process, Acetaldehyde, alcohol dehydrogenase method, ethylene second
Sour addition process compares rear several production methods, and esterification process is most traditional method, but due to the factor of price, esterification process exists
The country is still main preparation method.And strong acid, especially sulfuric acid will be added when reacting in esterification process, whens other high temperature, sets metal
Standby corrosion is strong, and is also easy to produce side reaction.Reducing esterification reaction temperature has using plant maintenance and reduces raw material consumption.
And the purification process after esterification generally takes two towers or two tower process, energy consumption is larger, and industrial conventional production process is raw
The steam mono-consumption of finished product is about 1.5~2t/t.
Summary of the invention
The main differential pressure type energy-saving processing technique for being designed to provide a kind of ethyl acetate of the invention has product
The characteristics of purity is high, the consumption that energy consumption is saved and unit consumption is at low cost.
The present invention can be achieved through the following technical solutions:
The invention discloses a kind of differential pressure type energy-saving processing technique of ethyl acetate, using ethyl alcohol and acetic acid as raw material, acetic acid with
Ethyl alcohol is reacting after the top material-heat-exchanging with esterification column into reboiler and reaction kettle, and the esterification subsequently into normal pressure separates
Tower carries out the taking-up of dehydrating agent side line in the tower of Esterification separation tower, and discharging progress is cold after tower top and the raw material heat exchange of Esterification separation tower
Solidifying split-phase, aqueous-phase reflux, oil mutually enters the rectifying concentration tower of pressurization after essence heat exchange, in the tower reactor output acetic acid of rectifying concentration tower
Ester finished product；The overhead vapours of rectifying concentration tower are used to heat the material of reaction kettle and the feed material of rectifying concentration tower.
Be using differential pressure in order to make two towers carry out can matched thermal coupling, that is, utilize the tower top material steam of the high tower of pressure
The lower tower materials at bottom of tower of pressure is heated, in the present invention, if rectifying column can only be to esterification column object without differential pressure
Material is preheated, and a large amount of steam are also added and heat to esterification；Gaseous phase materials can be improved in tower in this external pressurized
Density, the production capacity of pressurizing tower can be improved from face.
Further, the pressure of Esterification separation tower is 80~120 Kpa；The pressure of rectifying concentration tower is 280~480
KPa.According to being that esterification column can be coupled with operation temperature of two tower of rectifying column in pressure limit, good heat is carried out
Coupling utilizes.
Further, in raw material, molar ratio of alcohol to acid ethyl alcohol: acetic acid is 1.05~1.2:1.Ethyl alcohol can excessively make esterification column
The thick ester product acidity that tower top goes out, preferably control are in qualified level.
Further, rectifying concentration tower overhead reflux ratio is 0.5~2.
Further, in production of ethyl technique, esterification catalyst is acidic catalyst, acidic catalyst be sulfuric acid,
The a combination of one or more object of p-methyl benzenesulfonic acid and/or methane sulfonic acid.
Further, Esterification separation tower top material and reaction feed material carry out heat transfer coupling.
Further, rectifying tower top material steam carries out carry out heat transfer coupling with reboiler is reacted.
The differential pressure type energy-saving processing technique of ethyl acetate of the present invention has following beneficial technical effect:
The first, product purity is high, through the invention 99.5% or more the ethyl acetate finished product purity of production technology production；
The second, energy consumption is saved, and relative to conventional two tower process of normal pressure, differential pressure type technique of the invention reduces energy consumption and is greater than 40%；
Third, unit consumption are at low cost, present invention process compared to esterification column pressurization coupling rectification stripper heat mode in unit consumption
Also reduce 0.5~1.5%.
Specific embodiment
In order that those skilled in the art will better understand the technical solution of the present invention, below with reference to embodiment and to this
Invention product is described in further detail.
The invention discloses the invention discloses a kind of differential pressure type energy-saving processing techniques of ethyl acetate, with ethyl alcohol and acetic acid
As raw material, raw material and rectifying light component are being reacted after the top material-heat-exchanging with esterification column into reboiler and reaction kettle, so
Enter the Esterification separation tower of normal pressure afterwards, the taking-up of dehydrating agent side line is carried out in the tower of Esterification separation tower, using phase-splitter in esterification column
Split-phase is carried out, the tower top of Esterification separation tower discharges after exchanging heat with raw material by esterification column condenser, in esterification column overhead phase-splitter
Split-phase, partial reflux, water phase go water to recycle, and oil mutually enters pressurization through rectifying column feed preheater after the pressurization of the first pressurizing device
Rectifying concentration tower, in the tower reactor output acetic acid esters finished product of rectifying concentration tower；The overhead vapours of rectifying concentration tower are anti-for heating
Answer the material of kettle and the feed material of rectifying concentration tower.
Further, the pressure of Esterification separation tower is 80~120 Kpa；The pressure of rectifying concentration tower is 280~480
KPa。
Further, in raw material, molar ratio of alcohol to acid ethyl alcohol: acetic acid is 1.05~1.2:1.
Further, rectifying concentration tower overhead reflux ratio is 0.5~2.
Further, in production of ethyl technique, esterification catalyst is acidic catalyst, acidic catalyst be sulfuric acid,
The a combination of one or more object of p-methyl benzenesulfonic acid and/or methane sulfonic acid.
Further, Esterification separation tower top material and reaction feed material carry out heat transfer coupling.
Further, rectifying tower top material steam carries out heat transfer coupling by heat exchanger with reaction mass.
Embodiment 1
The invention discloses the invention discloses a kind of differential pressure type energy-saving processing technique of ethyl acetate, using ethyl alcohol and acetic acid as
Raw material, acetic acid is reacting after the top material-heat-exchanging with esterification column into reboiler and reaction kettle with ethyl alcohol, subsequently into normal pressure
Esterification separation tower, the taking-up of dehydrating agent side line is carried out in the tower of Esterification separation tower, after tower top and the raw material heat exchange of Esterification separation tower
Discharging carries out condensation split-phase, aqueous-phase reflux, the mutually pressurized rectifying concentration tower with after heat exchange into pressurization of oil, in rectifying concentration tower
Tower reactor output acetic acid esters finished product；The overhead vapours of rectifying concentration tower be used for heat reaction kettle material and rectifying concentration tower into
Material material.
In the present embodiment, the pressure of Esterification separation tower is 120 Kpa；The pressure of rectifying concentration tower is 380 KPa.Raw material
In, molar ratio of alcohol to acid ethyl alcohol: acetic acid 1.05:1.Rectifying concentration tower overhead reflux ratio is 2.In production of ethyl technique, ester
Change catalyst is acidic catalyst, and acidic catalyst is sulfuric acid.Esterification separation tower top material exchanges heat with reaction feed material
Coupling.Rectifying tower top material steam carries out heat transfer coupling by heat exchanger with reaction mass.
Embodiment 2
The invention discloses the invention discloses a kind of differential pressure type energy-saving processing technique of ethyl acetate, using ethyl alcohol and acetic acid as
Raw material, acetic acid is reacting after the top material-heat-exchanging with esterification column into reboiler and reaction kettle with ethyl alcohol, subsequently into normal pressure
Esterification separation tower, the taking-up of dehydrating agent side line is carried out in the tower of Esterification separation tower, after tower top and the raw material heat exchange of Esterification separation tower
Discharging carries out condensation split-phase, aqueous-phase reflux, the mutually pressurized rectifying concentration tower with after heat exchange into pressurization of oil, in rectifying concentration tower
Tower reactor output acetic acid esters finished product；The overhead vapours of rectifying concentration tower be used for heat reaction kettle material and rectifying concentration tower into
Material material.
In the present embodiment, the pressure of Esterification separation tower is 100 Kpa；The pressure of rectifying concentration tower is 280KPa.Raw material
In, molar ratio of alcohol to acid ethyl alcohol: acetic acid 1.2:1.Rectifying concentration tower overhead reflux ratio is 1.25.In production of ethyl technique,
Esterification catalyst is acidic catalyst, and acidic catalyst is p-methyl benzenesulfonic acid.Esterification separation tower top material and reaction feed object
Material carries out heat transfer coupling.Rectifying tower top material steam carries out heat transfer coupling by heat exchanger with reaction mass.
Embodiment 3
The invention discloses the invention discloses a kind of differential pressure type energy-saving processing technique of ethyl acetate, using ethyl alcohol and acetic acid as
Raw material, acetic acid is reacting after the top material-heat-exchanging with esterification column into reboiler and reaction kettle with ethyl alcohol, subsequently into normal pressure
Esterification separation tower, the taking-up of dehydrating agent side line is carried out in the tower of Esterification separation tower, after tower top and the raw material heat exchange of Esterification separation tower
Discharging carries out condensation split-phase, aqueous-phase reflux, the mutually pressurized rectifying concentration tower with after heat exchange into pressurization of oil, in rectifying concentration tower
Tower reactor output acetic acid esters finished product；The overhead vapours of rectifying concentration tower be used for heat reaction kettle material and rectifying concentration tower into
Material material.
In the present embodiment, the pressure of Esterification separation tower is 80 Kpa；The pressure of rectifying concentration tower is 480 KPa.Raw material
In, molar ratio of alcohol to acid ethyl alcohol: acetic acid 1.12:1.Rectifying concentration tower overhead reflux ratio is 0.5.In production of ethyl technique,
Esterification catalyst is acidic catalyst, and acidic catalyst is methane sulfonic acid.Esterification separation tower top material and reaction feed material into
Row heat transfer coupling.Rectifying tower top material steam carries out heat transfer coupling by heat exchanger with reaction mass.
Embodiment 4
The invention discloses the invention discloses a kind of differential pressure type energy-saving processing technique of ethyl acetate, using ethyl alcohol and acetic acid as
Raw material, acetic acid is reacting after the top material-heat-exchanging with esterification column into reboiler and reaction kettle with ethyl alcohol, subsequently into normal pressure
Esterification separation tower, the taking-up of dehydrating agent side line is carried out in the tower of Esterification separation tower, after tower top and the raw material heat exchange of Esterification separation tower
Discharging carries out condensation split-phase, aqueous-phase reflux, the mutually pressurized rectifying concentration tower with after heat exchange into pressurization of oil, in rectifying concentration tower
Tower reactor output acetic acid esters finished product；The overhead vapours of rectifying concentration tower be used for heat reaction kettle material and rectifying concentration tower into
Material material.
In the present embodiment, the pressure of Esterification separation tower is 80~120 Kpa；The pressure of rectifying concentration tower is 320KPa.
In raw material, molar ratio of alcohol to acid ethyl alcohol: acetic acid 1.08:1.Rectifying concentration tower overhead reflux ratio is 1.Production of ethyl technique
In, esterification catalyst is acidic catalyst, and acidic catalyst is sulfuric acid, p-methyl benzenesulfonic acid and methane sulfonic acid.Esterification separation tower
It pushes up material and reaction feed material carries out heat transfer coupling.Rectifying tower top material steam is exchanged heat with reaction mass by heat exchanger
Coupling.
Embodiment 5
The invention discloses the invention discloses a kind of differential pressure type energy-saving processing technique of ethyl acetate, using ethyl alcohol and acetic acid as
Raw material, acetic acid is reacting after the top material-heat-exchanging with esterification column into reboiler and reaction kettle with ethyl alcohol, subsequently into normal pressure
Esterification separation tower, the taking-up of dehydrating agent side line is carried out in the tower of Esterification separation tower, after tower top and the raw material heat exchange of Esterification separation tower
Discharging carries out condensation split-phase, aqueous-phase reflux, the mutually pressurized rectifying concentration tower with after heat exchange into pressurization of oil, in rectifying concentration tower
Tower reactor output acetic acid esters finished product；Rectifying tower top material steam carries out heat transfer coupling by heat exchanger with reaction mass.
In the present embodiment, the pressure of Esterification separation tower is 110 Kpa；The pressure of rectifying concentration tower is 420 KPa.Raw material
In, molar ratio of alcohol to acid ethyl alcohol: acetic acid 1.12:1.Rectifying concentration tower overhead reflux ratio is 1.5.In production of ethyl technique,
Esterification catalyst is acidic catalyst, and acidic catalyst is sulfuric acid and methane sulfonic acid.Esterification separation tower top material and reaction feed
Material carries out heat transfer coupling.Rectifying tower top material steam carries out carry out heat transfer coupling with reboiler is reacted.
Application Example 1
The invention discloses a kind of differential pressure type energy-saving processing technique of ethyl acetate, 95 ethyl alcohol (and recycling ethyl alcohol) of 100kg/h
Enter reaction system with the acetic acid of 112kg/h, be in 58 DEG C of entrance reaction kettle R1, R1 after E3 is preheated using sulfuric acid as catalyst,
Content keeps being about 0.5%(w/w), dehydrating agent is butyl acetate, and content remains 10~13% (w/w).It is reacted to react kettle liquid
After kettle and reboiler reaction and gasification (114 DEG C), it is cooling after side line in tower is collected and taken out to enter Esterification separation tower from T1 tower bottom
Layering, water phase go recyclable device, organic phase logistics infinite reflux after taking out logistics heat exchange with side line.Overhead stream is through heat exchanger E3
Split-phase afterwards, organic phase reflux ratio are 1.8:1, and organic phase is pressurizeed after E4 exchanges heat into the tower (350kpa) of pressurization, tower top temperature
It is 110-112 DEG C, lighter component tank S3, reflux ratio 1.20:1 is entered after top gaseous phase and reaction kettle material Coupling Thermal.Tower bottom goes out
Ethyl acetate finished product, purity is up to 99.59%.Steam mono-consumption 1.16t/t, compared to atmospheric processes steam mono-consumption 1.85t/t, consumption reduction
37%。
Application Example 2
The invention discloses a kind of differential pressure type energy-saving processing technique of ethyl acetate, 95 ethyl alcohol (and recycling ethyl alcohol) of 100kg/h
Enter reaction system with the acetic acid of 108kg/h, be in 58 DEG C of entrance reaction kettle R1, R1 after E3 is preheated using sulfuric acid as catalyst,
Content keeps being about 0.8%(w/w), dehydrating agent is butyl acetate, and content remains 8-10% (w/w).React the reacted kettle of kettle liquid
After reacting and gasify with reboiler (114 DEG C), enter Esterification separation tower cooling point after side line in tower is collected and taken out from T1 tower bottom
Layer, water phase go recyclable device, organic phase logistics infinite reflux after taking out logistics heat exchange with side line.Overhead stream is after heat exchanger E3
Split-phase, organic phase reflux ratio are 1.8:1, and organic phase is pressurizeed after E4 exchanges heat into the tower (480kpa) of pressurization, and tower top temperature is
119-120 DEG C, enter lighter component tank S3, reflux ratio 1.21:1 after top gaseous phase and reaction kettle material Coupling Thermal.Tower bottom goes out second
Acetoacetic ester finished product, purity is up to 99.53%.Steam mono-consumption 1.12t/t, compared to atmospheric processes steam mono-consumption 1.85t/t, consumption reduction
40%。
Application Example 3
The invention discloses a kind of differential pressure type energy-saving processing technique of ethyl acetate, 95 ethyl alcohol (and recycling ethyl alcohol) of 100kg/h
Enter reaction system with the acetic acid of 103kg/h, is with methane sulfonic acid after E3 is preheated in 58 DEG C of entrance reaction kettle R1, R1 for catalysis
Agent, content keep being about 1.2%(w/w), dehydrating agent is butyl acetate, and content remains 7-9% (w/w).It is reacted to react kettle liquid
After kettle and reboiler reaction and gasification (114 DEG C), it is cooling after side line in tower is collected and taken out to enter Esterification separation tower from T1 tower bottom
Layering, water phase go recyclable device, organic phase logistics infinite reflux after taking out logistics heat exchange with side line.Overhead stream is through heat exchanger E3
Split-phase afterwards, organic phase reflux ratio are 1.8:1, and organic phase is pressurizeed after E4 exchanges heat into the tower (280kpa) of pressurization, tower top temperature
It is 102 DEG C, lighter component tank S3, reflux ratio 1.98:1 is entered after top gaseous phase and reaction kettle material Coupling Thermal.Tower bottom goes out acetic acid
Ethyl ester finished product, purity is up to 99.66%.Steam mono-consumption is 1.29t/t, compared to atmospheric processes steam mono-consumption 1.85t/t, consumption reduction
30%。
More than, only presently preferred embodiments of the present invention is not intended to limit the present invention in any form；All current rows
The those of ordinary skill of industry can be shown in by specification and above and swimmingly implement the present invention；But all it is familiar with this profession
Technical staff without departing from the scope of the present invention, made using disclosed above technology contents it is a little more
Dynamic, modification and the equivalent variations developed, are equivalent embodiment of the invention；Meanwhile all substantial technologicals pair according to the present invention
The variation, modification and evolution etc. of any equivalent variations made by above embodiments, still fall within the guarantor of technical solution of the present invention
Within the scope of shield.
Claims (6)
1. a kind of differential pressure type energy-saving processing technique of ethyl acetate, using ethyl alcohol and acetic acid as raw material, it is characterised in that: acetic acid with
Ethyl alcohol is reacting after the top material-heat-exchanging with esterification column into reboiler and reaction kettle, and the esterification subsequently into normal pressure separates
Tower carries out the taking-up of dehydrating agent side line in the tower of Esterification separation tower, and discharging progress is cold after tower top and the raw material heat exchange of Esterification separation tower
Solidifying split-phase, aqueous-phase reflux, heat exchange enters the rectifying concentration tower of pressurization after oil is mutually pressurized, in the tower reactor output second of rectifying concentration tower
Acid esters finished product；The overhead vapours of the rectifying concentration tower are used to heat the material of reaction kettle and the feed material of rectifying concentration tower.
2. the differential pressure type energy-saving processing technique of ethyl acetate according to claim 1, it is characterised in that: the esterification point
Pressure from tower is 80~120 Kpa；The pressure of the rectifying concentration tower is 280~480 KPa.
3. the differential pressure type energy-saving processing technique of ethyl acetate according to claim 1 or 2, it is characterised in that: the raw material
In, molar ratio of alcohol to acid ethyl alcohol: acetic acid is 1.05~1.2:1.
4. the differential pressure type energy-saving processing technique of ethyl acetate according to claim 3, it is characterised in that: the rectifying concentrate
Column overhead reflux ratio is 0.5~2.
5. the differential pressure type energy-saving processing technique of ethyl acetate according to claim 4, it is characterised in that: production of ethyl
In technique, esterification catalyst is acidic catalyst, and the acidic catalyst is sulfuric acid, p-methyl benzenesulfonic acid and/or methane sulfonic acid
A combination of one or more object.
6. the differential pressure type energy-saving processing technique of ethyl acetate according to claim 5, it is characterised in that: rectifying tower top material
Steam carries out carry out heat transfer coupling with reboiler is reacted.
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Application publication date: 20191112 |