CN106699566B - A kind of method of reactive distillation next door tower coproduction ethyl acetate and n-butyl acetate - Google Patents
A kind of method of reactive distillation next door tower coproduction ethyl acetate and n-butyl acetate Download PDFInfo
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- CN106699566B CN106699566B CN201710030652.3A CN201710030652A CN106699566B CN 106699566 B CN106699566 B CN 106699566B CN 201710030652 A CN201710030652 A CN 201710030652A CN 106699566 B CN106699566 B CN 106699566B
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Abstract
The present invention is the method for a kind of reactive distillation next door tower coproduction ethyl acetate and n-butyl acetate.This method uses reactive distillation next door tower, feed ethanol is fed from the bottom of conversion zone, raw material n-butanol and acetic acid are fed from the middle part of conversion zone, two reactions are placed on same conversion zone, and while preparing ethyl acetate acetic acid N-butyl, n-butyl acetate generates the entrainer of water when can function as preparing ethyl acetate, to reduce the regurgitant volume of tower top ethyl acetate, reaction conversion ratio is improved, the content of tower top ester Xiang Zhongyi alcohol and water is reduced, reduces the energy consumption of production process.The present invention can not only reduce condenser and reboiler dosage, but also can promote its thermodynamic efficiency, further decrease energy consumption of rectification, realize depth energy saving, bring good economic benefit.
Description
Technical field
The present invention relates to a kind of techniques using reactive distillation next door tower coproduction ethyl acetate and n-butyl acetate, specifically
Using ethyl alcohol, n-butanol and acetic acid as raw material, preparation and clearly separating acetic acid ethyl ester and the positive fourth of acetic acid are realized in single rectifying column
The technique of ester.
Background technique
In the production process of the industries such as petroleum, chemical industry, energy consumption of rectification accounts for about 40% or so of whole process energy consumption, therefore
Realize that the energy-saving and emission-reduction of distillation process have important social effect.Reactive distillation next door tower is a kind of by reactive distillation and next door
Tower-coupled novel thermal coupling tower has broken reaction balance and the limitation that balances each other, has reduced the back-mixing degree of intermediate species, can show
Writing reduces separating energy consumption.Ethyl acetate and n-butyl acetate are all organic solvents important in Chemical Manufacture, are widely used in oil
The industries such as paint, fragrance and weaving.Traditional reactive distillation esterification process production ethyl acetate, this method are commonly used in domestic industry at present
On the one hand a large amount of ester is needed mutually to take the water generated in tower out of in overhead reflux, water and ethyl alcohol contains in the thick ester of another aspect tower top
Amount is higher, so that subsequent separation process is needed higher vapour-liquid load, so energy consumption is higher.The production of n-butyl acetate needs simultaneously
Aqueous-phase reflux is taken to the n-butyl acetate of generation out of, therefore energy consumption is also higher.
Miguel A.Santaella et al. proposes that reactive distillation next door tower prepares ethyl acetate in the literature, in prefractionation
Duan Fasheng esterification, public rectifying section tower top distillate thick ethyl acetate, main column section tower reactor extracted waste water.But process program master
It leans on tower top ester mutually to flow back and takes the water that reaction generates out of, flow back bigger, therefore tower reactor energy consumption is also corresponding higher.Zhang Bingjian et al.
Ethyl acetate is prepared using reactive distillation, addition n-butyl acetate is that entrainer will react the water generated from side take-off, one
Determine to reduce tower top ester phase regurgitant volume and tower reactor energy consumption in degree, but due to the back-mixing problem of intermediate species, so its thermodynamics
Efficiency is lower.Tian Hui et al. proposition ethyl acetate and n-butyl acetate technique, two reactive distillation columns of the process requirement (including two
Platform condenser, two reboilers), difference preparative separation ethyl acetate and n-butyl acetate, high, process complexity that there are costs of equipment
The problems such as.
In conclusion ethyl acetate and n-butyl acetate production technology are there are process complexity, thermodynamic efficiency is low, energy consumption is high
The problems such as, therefore it is particularly important to find the process program that a kind of process is simple, thermodynamic efficiency is high, low energy consumption.
Summary of the invention
The present invention provides the techniques of a kind of reactive distillation next door tower coproduction ethyl acetate and n-butyl acetate, it is therefore an objective to solve
Certainly traditional reactive distillation production ethyl acetate, n-butyl acetate separation process is complicated, energy consumption is high, invests the problems such as high.The technique
Two reactions are placed on same conversion zone, while preparing ethyl acetate acetic acid N-butyl, n-butyl acetate can also fill
The entrainer of water is generated when preparing ethyl acetate, to reduce the regurgitant volume of tower top ethyl acetate, improves reaction conversion ratio, drop
The content of low tower top ester Xiang Zhongyi alcohol and water, reduces the energy consumption of production process.Another aspect present invention process may be implemented in single
Rectifying column in preparation and clear separating acetic acid ethyl ester and n-butyl acetate, can not only reduce condenser and reboiler dosage, and
And its thermodynamic efficiency can be promoted, energy consumption of rectification is further decreased, depth energy saving is realized, brings good economic benefit.
The technical solution of the present invention is as follows:
A kind of method of reactive distillation next door tower coproduction ethyl acetate and n-butyl acetate, comprising the following steps:
In the reactive distillation next door tower, partition is located on the central axis in tower, and prefractionation section is located on the left of partition,
Public rectifying section is located at partition top；Main column section is located on the right side of partition, and public stripping section is located at the lower partition；Material is in prefractionation
Section middle part feeds and reacts, and is considered as conversion zone；Storng-acid cation exchange resin Amberlyst15 is housed in conversion zone,
Loadings are 0.6~1kg/L filler；
The reactive distillation next door tower is atmospheric operation；Bottom temperature is 114~117 DEG C；
(1) feed ethanol is fed from the bottom of conversion zone, and raw material n-butanol and acetic acid are fed from the middle part of conversion zone；Second
In conversion zone esterification occurs for alcohol, n-butanol and acetic acid, generates ethyl acetate and n-butyl acetate respectively, then A, B component
It is upwardly into public rectifying section, B, component C are downwardly into public stripping section；
Wherein, component A is the ternary azeotrope of ethyl acetate, second alcohol and water；B component is the binary of n-butyl acetate and water
Azeotropic mixture；Component C is the mixture of acetic acid and water, and wherein acetic acid concentration is greater than 95%wt；
(2) A, B component described in successively realize separation by the top of public rectifying section and main column section；Component A enters tower
Top is condensed into liquid phase through condenser, enters back into the first phase-splitter split-phase, and the upper layer of the first phase-splitter is that ethyl acetate content is 93
The ester phase of~95%wt, lower layer are the water phases that water content is 90~92%wt；Mutually a part extraction, a part are back in tower ester
Public rectifying section, ester phase reflux ratio are 2.5-4；The extraction of water phase a part, a part are back to public rectifying section in tower, and water phase is returned
Stream ratio is 0.4-0.65；And B component enters the top half of main column section；
(3) B, component C described in successively realize separation by the lower part of public stripping section and main column section；Wherein component C into
The bottom for entering public stripping section is produced from tower reactor；And remaining B component then enters the lower half portion of main column section, with come from king-tower
The B component of part is converged in the middle part of main column section together in section, and then sideline product produces, and sideline product is cold through side line condenser
After solidifying, the second phase-splitter split-phase is entered back into, the upper layer in the second phase-splitter is the ester that n-butyl acetate content is 89~92%wt
Phase, lower layer are the water phases that water content is 90~92%wt；
Three kinds of feedstock temperature are 40-50 DEG C；The mole of feed ratio of ethyl alcohol and n-butanol is 3-4:1；Acetic acid with
The mole of feed ratio of ethyl alcohol is 1.2-2:1；The concentration of feed ethanol is 95%wt；Raw material butanol concentration is 100%wt；Raw material
The concentration of acetic acid is 80%-100%wt；
The number of theoretical plate of the prefractionation section is 20-40；The number of theoretical plate of public rectifying section is 5-15；The reason of main column section
It is 20-40 by plate number；The number of theoretical plate of public stripping section is 5-15；Conversion zone is on prefractionation section 10-30 block theoretical plate；
The feed entrance point of the feed ethanol is 10~20 blocks of column plates of prefractionation section；The raw material n-butanol and second
The feed entrance point of acid is 15~30 blocks of column plates of prefractionation section；The extraction position of sideline product is that the 10-25 block of main column section is managed
By plate；
Proportionally 0.48-2.3:1 is allocated for two sides of the decline liquid phase of public rectifying section at the top of partition, respectively into
Enter prefractionation section and main column section；
In the two sides of partition bottom, proportionally 0.48-2.3:1 is allocated the rising vapour phase of public stripping section, respectively into
Enter prefractionation section and main column section；
The reactive distillation next door tower is preferably packed tower.
Compared with prior art, the beneficial effects of the present invention are:
The present invention utilize reactive distillation next door tower coproduction ethyl acetate and n-butyl acetate, carry out reactive distillation next door tower and
The process intensification of joint production process in single rectifying tower, it can be achieved that prepare simultaneously clear separating acetic acid ethyl ester and n-butyl acetate.
The present invention can adjust reactant ethyl alcohol and positive fourth according to demand of the market for ethyl acetate and n-butyl acetate
The ratio of alcohol, to obtain the ethyl acetate and n-butyl acetate product for the amount of according with the demands of the market.
The present invention can flexibly handle tower reactor logistics according to the purity of acetic acid raw material, when acetic acid raw material concentration is 80-90%wt
When, present invention process can realize the purification of acetic acid by public stripping section while coproduction ethyl acetate and n-butyl acetate,
The acetic acid product that concentration is greater than 95%wt can be produced in tower reactor；When acetic acid raw material concentration is 90-100%wt, tower reactor logistics is not
Extraction, but acetic acid feed mouth is returned it by pump and is recycled.
This process program under the conditions ofs changing reactant ethyl alcohol and n-butanol charge proportion, reactant acetic acid concentration etc., with
Traditional reactive distillation process project plan comparison can be achieved to save energy consumption 30% or so.
Detailed description of the invention
Fig. 1 is the flow diagram of reactive distillation next door tower coproduction ethyl acetate acetic acid dinbutyl phthalate technology
Specific embodiment
The present invention is further described below with reference to examples and drawings.
In order to better illustrate the present invention, it is easy to understand technical solution of the present invention, of the invention is typical but non-limiting
Embodiment is as follows:
The method of reactive distillation next door tower coproduction ethyl acetate and n-butyl acetate of the present invention, as shown in Figure 1, every
Plate is located on the central axis in tower, and prefractionation section I is located on the left of partition, number of theoretical plate 30；Public rectifying section II be located at every
Plate top, number of theoretical plate 10；Main column section III is located on the right side of partition, number of theoretical plate 30；Public stripping section IV is located under partition
Portion, number of theoretical plate 10；Conversion zone V is equipped with strongly acidic cation exchange tree on the 10-20 block theoretical plate of prefractionation section I
Rouge Amberlyst15, wherein loading 0.8kg catalyst in every liter of filler.
Reactive distillation next door tower is packed tower, and filler is the Dixon ring of 3*3.Operating pressure is 101.325kPa.Feed ethanol
It is fed from the 20th block of plate of prefractionation section I, raw material n-butanol and acetic acid are fed from the 15th block of plate of prefractionation section I；Ethyl alcohol, positive fourth
Alcohol and acetic acid generate ethyl acetate and n-butyl acetate, wherein ethyl acetate, second in the generation esterification of conversion zone V respectively
The ternary azeotrope of alcohol and water is component A, and the binary azeotrope of n-butyl acetate and water is B component, the mixture of acetic acid and water
For component C, wherein acetic acid concentration is greater than 95%wt.
The specific separating step of product is as follows after reaction:
A, B component is realized in prefractionation section I with B, component C and is clearly separated, i.e., A, B enter public rectifying section II, B, C into
Enter public stripping section IV.
A, B component realizes clear separation on the top of public rectifying section II and main column section III.Wherein it is cold to enter tower top for component A
Condenser C-101 (condenser temperature is 35 DEG C) is condensed into liquid phase, enters back into phase-splitter D-101 later and carries out split-phase, upper layer is ester
Phase (ethyl acetate content is about 94%wt), lower layer are water phase (water content is about 91%wt).Ester mutually a part extraction, a part
It is back in tower；It, need to be by aqueous portion for acetic acid content in control tower top and sideline product (acetic acid content is lower than 0.03%wt)
Reflux.And remaining B component enters the top half of main column section III.
B, component C realizes clear separation in the lower part of public stripping section IV and main column section III.Wherein component C is from public stripping
The bottom extraction (acetic acid content is greater than 95%wt) of section IV, and remaining B component then enters lower half portion and the master of main column section III
The B component of part produces (n-butyl acetate content is about 78%wt) together as sideline product in tower section III.Sideline product B group
After lease making condenser C-102 (condenser temperature is 35 DEG C) condensation, phase-splitter D-102 split-phase is entered back into, upper layer is the positive fourth of acetic acid
Ester crude product (n-butyl acetate content is about 90%wt), lower layer are water phase (water content is about 90%wt).
Feedstock temperature is between 40-50 DEG C；The mole of feed ratio of ethyl alcohol and n-butanol is 3-4:1；Acetic acid and second
The raw materials components mole ratio example of alcohol is 1.2-2:1；The concentration of feed ethanol is 95%wt；Raw material butanol concentration is 100%wt；Raw material second
The concentration of acid is 80%-100%wt.
The decline liquid phase of public rectifying section and the risings vapour phase of public stripping section are divided in portion pre- point in partition two sides
It evaporates in section and main column section, carries out reverse contact and realize mass transfer separation process.Wherein through control swinging funnel two at the top of partition
The duration of oscillation of side come control liquid phase distribution ratio be 0.3-0.7, wherein liquid phase distribution ratio be into prefractionation section liquid phase flow
With the ratio of total liquid phase flow；It is 0.3-0.7 that vapour phase distribution ratio is controlled by balance partition two sides pressure drop, and wherein vapour phase is distributed
Than for into the ratio of the vapour phase flow of prefractionation section and total vapour phase flow.
Ester phase reflux ratio is 2.5-4；Wherein ester phase reflux ratio is the ratio of tower top ester phase produced quantity and regurgitant volume.
Aqueous-phase reflux ratio is 0.4-0.65；Wherein aqueous-phase reflux ratio is tower top water phase produced quantity and water phase total flow
Ratio.
Acetic acid raw material concentration depends on factory's actual production situation, when acetic acid raw material concentration is 80%-90%wt, makes anti-
It answers object acetic acid with respect to ethyl alcohol and butanol excess 20%-100%, does not participate in the acetic acid of reaction through prefractionation section I and public stripping section
IV purification directly produces the acetic acid product that concentration is greater than 95%wt in tower reactor, that is, realizes the purification concentrate of raw acetic acid.Work as second
When acid starting material concentration is 90%-100%wt, then makes reactant ethyl alcohol with respect to acetic acid excess 3%, through prefractionation section I and public mention
The separation of section IV is evaporated, tower reactor is the acetic acid stream that concentration is greater than 95%wt, which does not produce but return it into second by pump
Sour feed cycle uses.
Case study on implementation 1
Reactive distillation next door tower is packed tower, and tower diameter 0.43m, partition is located on the central axis in tower, prefractionation section I
Number of theoretical plate be 30, the number of theoretical plate of public rectifying section II is 10, the number of theoretical plate of main column section III is 30, public stripping section IV
Number of theoretical plate be 10,10-20 block theoretical plate of the conversion zone V in prefractionation section I.The operating pressure of reactive distillation next door tower
For 101.325kPa, bottom temperature is 115 DEG C.Feed ethanol is fed from the 20th block of plate of prefractionation section I, raw material n-butanol and second
Acid is fed from the 15th block of plate of prefractionation section I, and side take-off position is the 15th piece of theoretical plate of main column section.Feeding temperature is in 40-
Between 50 DEG C.The concentration of acetic acid raw material is 100%wt, feed rate 5kmol/h.Ethanol raw material concentration is 95%wt, charging
Flow is 4kmol/h；N-butanol material concentration is 100%wt, feed rate 1kmol/h.Liquid phase distribution ratio is 0.6；Vapour phase
Distribution ratio is 0.5；Tower top ester phase reflux ratio is 3；Tower top water phase reflux ratio example is 0.45.Ethyl acetate in tower top ester phase product
Mass concentration is 93.8%；The mass concentration of water is 91.4% in tower top water phase；The matter of n-butyl acetate in side line ester phase product
Measuring concentration is 90.2%；The mass concentration of water is 90.7% in side line water phase.Tower reactor energy consumption is 280kw, is reacted compared to tradition
Rectifying column prepares ethyl acetate technique and saves tower reactor energy consumption 34%.
Case study on implementation 2
Reactive distillation next door tower is packed tower, and tower diameter 0.43m, partition is located on the central axis in tower, prefractionation section I
Number of theoretical plate be 30, the number of theoretical plate of public rectifying section II is 10, the number of theoretical plate of main column section III is 30, public stripping section IV
Number of theoretical plate be 10,10-20 block theoretical plate of the conversion zone V in prefractionation section I.The operating pressure of reactive distillation next door tower
For 101.325kPa, bottom temperature is 117 DEG C.Feed ethanol is fed from the 20th block of plate of prefractionation section I, raw material n-butanol and second
Acid is fed from the 15th block of plate of prefractionation section I, and side take-off position is the 15th piece of theoretical plate of main column section.Feeding temperature is in 40-
Between 50 DEG C；The concentration of acetic acid raw material is 85%wt, feed rate 8kmol/h.Ethanol raw material concentration is 95%wt, feeding flow
Amount is 4kmol/h；N-butanol material concentration is 100%wt, feed rate 1kmol/h.Liquid phase distribution ratio is 0.63；Vapour phase point
Proportion is 0.5；Tower top ester phase reflux ratio is 2.8；Tower top water phase reflux ratio example is 0.42.Ethyl acetate in tower top ester phase product
Mass concentration is 93.1%；The mass concentration of water is 90.8% in tower top water phase；The matter of n-butyl acetate in side line ester phase product
Measuring concentration is 89.9%；The mass concentration of water is 90.1% in side line water phase.Tower reactor energy consumption is 302kw, is reacted compared to tradition
Rectifying column prepares ethyl acetate technique and saves tower reactor energy consumption 29%.
Case study on implementation 3
Reactive distillation next door tower is packed tower, and tower diameter 0.38m, partition is located on the central axis in tower, prefractionation section I
Number of theoretical plate be 30, the number of theoretical plate of public rectifying section II is 10, the number of theoretical plate of main column section III is 30, public stripping section IV
Number of theoretical plate be 10,10-20 block theoretical plate of the conversion zone V in prefractionation section I.The operating pressure of reactive distillation next door tower
For 101.325kPa, bottom temperature is 117 DEG C.Feed ethanol is fed from the 20th block of plate of prefractionation section I, raw material n-butanol and second
Acid is fed from the 15th block of plate of prefractionation section I, and side take-off position is the 15th piece of theoretical plate of main column section.Feeding temperature is in 40-
Between 50 DEG C；The concentration of acetic acid raw material is 85%wt, feed rate 6kmol/h.Ethanol raw material concentration is 95%wt, feeding flow
Amount is 3kmol/h；N-butanol material concentration is 100%wt, feed rate 1kmol/h.Liquid phase distribution ratio is 0.66；Vapour phase point
Proportion is 0.5；Tower top ester phase reflux ratio is 3.1；Tower top water phase reflux ratio example is 0.51.N-butyl acetate in tower top ester phase product
Mass concentration be 93.9%；The mass concentration of water is 91.7% in tower top water phase；The matter of ethyl acetate in side line ester phase product
Measuring concentration is 91.3%；The mass concentration of water is 91.6% in side line water phase.Tower reactor energy consumption is 264kw, is reacted compared to tradition
Rectifying column prepares ethyl acetate technique and saves tower reactor energy consumption 37.8%.
The present invention does not address place and is suitable for the prior art.
Claims (2)
1. a kind of method of reactive distillation next door tower coproduction ethyl acetate and n-butyl acetate, it is characterized in that this method includes following
Step:
In the reactive distillation next door tower, partition is located on the central axis in tower, and prefractionation section is located on the left of partition, public
Rectifying section is located at partition top, and main column section is located on the right side of partition, and public stripping section is located at the lower partition；Material is in prefractionation section
Portion feeds and reacts, and is considered as conversion zone；Storng-acid cation exchange resin Amberlyst15, filling are housed in conversion zone
Amount is 0.6~1kg/L filler；
The reactive distillation next door tower is atmospheric operation；Bottom temperature is 114~117 DEG C；
(1) feed ethanol is fed from the bottom of conversion zone, and raw material n-butanol and acetic acid are fed from the middle part of conversion zone；Ethyl alcohol, just
In conversion zone esterification occurs for butanol and acetic acid, generates ethyl acetate and n-butyl acetate respectively, and then A, B component are to enterprising
Enter public rectifying section, B, component C are downwardly into public stripping section；
Wherein, component A is the ternary azeotrope of ethyl acetate, second alcohol and water；B component is the binary azeotropic of n-butyl acetate and water
Object；Component C is the mixture of acetic acid and water, and wherein acetic acid concentration is greater than 95%wt；
(2) A, B component described in successively realize separation by the top of public rectifying section and main column section；Component A enters tower top warp
Condenser is condensed into liquid phase, enters back into the first phase-splitter split-phase, the upper layer of the first phase-splitter be ethyl acetate content be 94~
The ester phase of 96%wt, lower layer are the water phases that water content is 90~92%wt；Ester mutually a part extraction, a part is back in tower public
Rectifying section altogether, ester phase reflux ratio are 2.5-4；The extraction of water phase a part, a part are back to public rectifying section, aqueous-phase reflux in tower
Ratio is 0.4-0.65；And B component enters the top half of main column section；
(3) B, component C described in successively realize separation by the lower part of public stripping section and main column section；Wherein component C enters public affairs
The bottom of stripping section altogether is produced from tower reactor；And remaining B component then enters the lower half portion of main column section, and in the main column section
Partial B component is converged in the middle part of main column section together, and then sideline product produces, and sideline product is condensed through side line condenser
Afterwards, the second phase-splitter split-phase is entered back into, the upper layer in the second phase-splitter is the ester phase that n-butyl acetate content is 89~92%wt,
Lower layer is the water phase that water content is 90~92%wt；
Three kinds of feedstock temperature are 40-50 DEG C；The mole of feed ratio of ethyl alcohol and n-butanol is 3-4:1；Acetic acid
Mole of feed ratio with ethyl alcohol is 1.2-2:1；The concentration of feed ethanol is 95%wt；Raw material butanol concentration is 100%wt；It is former
The concentration for expecting acetic acid is 80%-100%wt；
The number of theoretical plate of the prefractionation section is 20-40；The number of theoretical plate of public rectifying section is 5-15；The theoretical plate of main column section
Number is 20-40；The number of theoretical plate of public stripping section is 5-15；Conversion zone is on prefractionation section 10-30 block theoretical plate；
The feed entrance point of the feed ethanol is 10~20 pieces of theoretical plates of prefractionation section；The raw material n-butanol and acetic acid
Feed entrance point be prefractionation section 15~30 blocks of column plates；The extraction position of sideline product is that the 10-25 block of main column section is theoretical
Plate；
Proportionally 0.48-2.3:1 is allocated for two sides of the decline liquid phase of the public rectifying section at the top of partition, respectively
Into prefractionation section and main column section；The rising vapour phase of public stripping section partition bottom two sides proportionally 0.48-2.3:1 into
Row distribution, respectively enters prefractionation section and main column section.
2. the method for reactive distillation next door tower coproduction ethyl acetate and n-butyl acetate as described in claim 1, it is characterized in that
The reactive distillation next door tower is packed tower.
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| CN109663375A (en) * | 2017-10-13 | 2019-04-23 | 中国石油化工集团公司 | A kind of separation method of next door rectifying column and hydrocarbon mixture |
| CN108467744B (en) * | 2018-03-27 | 2020-04-24 | 天津大学 | Five-line-reducing product quality improvement method for lubricating oil type pressure-reducing partition plate tower |
| US10377690B1 (en) * | 2018-08-22 | 2019-08-13 | Eastman Chemical Company | Method for catalytic production of refined enal products from an aldehyde feed stream using a single enclosed unit |
| CN113956149B (en) * | 2020-07-21 | 2024-03-15 | 中国石油大学(华东) | Separation method of glyceric acid product prepared by glycerol oxidation |
| CN113230682A (en) * | 2021-05-08 | 2021-08-10 | 北京化工大学 | Double-partition-wall reaction rectification structure and design method |
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| Design and control of a reactive-distillation process for esterification of an alcohol mixture containing ethanol and n-butanol;Yi-Chang Wu等;《Computers and Chemical Engineering》;20130125;第57卷;第63-77页 * |
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