CN109776310A - A kind of homogeneous catalysis rectification process preparing propionic ester by ester transesterification - Google Patents
A kind of homogeneous catalysis rectification process preparing propionic ester by ester transesterification Download PDFInfo
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Abstract
The present invention opens one using homogeneous solvable alkali or ionic liquid as catalyst methyl propionate and various esters such as Ethyl formate, propyl formate, butyl formate, ethyl acetate, the catalytic rectification process of the one-step synthesis such as propyl acetate, butyl acetate high added value, high-purity propionic ester.The process advantage is that reaction system is simple, and response path is short；Selectivity of product is high, with high purity, and complete no coupling product generates；Reaction time is short, and catalyst activity is high, and catalyst is reusable；It generally can be easily separated without azeotropic between starting ester and product ester, be of great significance to extensive, inexpensive production high added value, high-purity propionic ester.Entire reaction process green, energy-saving and environmental protection and efficiently.
Description
Technical field
Chemosynthesis technical field of the present invention, specifically (including but not limited to methyl propionate and reaction raw materials ester
Ethyl formate, propyl formate, butyl formate, ethyl acetate, propyl acetate, butyl acetate etc.) it is raw material, utilize homogeneous solvable alkali
Ionic liquid be catalyst realize continuous production high added value, the technique of high-purity propionic ester.
Background technique
Propionic ester can be applied to cellulose esters and ethers, the solvent of various natural or synthetic resins；It can be used for as fragrance
Concoct fragrant apple perfume, banana incense, plum, pineapple perfume and as butter, Western wine and other multiple eating essence.It also is used as
High-grade daily-use cosmetic essence.Such product also serves as organic synthesis intermediate.Research has shown that ethyl propionate and propyl propionate
To LiFePO4Lithium ion battery cryogenic property has certain influence.A certain amount of ethyl propionate or propyl propionate are added, carbonic acid can be improved
The ionic conductivity of ester electrolyte improves electrolyte and anode LiFePO4The compatibility of material and cathode graphite material reduces electricity
The viscosity and eutectic point for solving liquid system, are conducive to the migration of lithium ion, to improve LiFePO4The low temperature properties of lithium ion battery
Energy.At present lithium battery battery of mobile phone and in terms of, all play increasingly important role.But due to
Lithium battery electrolytes low temperature properties are poor, and under low temperature condition, the battery of electric vehicle service life is generally shorter, and in the electricity of lithium ion battery
The cryogenic property of lithium-ion battery electrolytes can be substantially improved by adding a certain amount of ethyl propionate or ethyl propionate then in solution liquid, because
This market prospects is very wide.Propionic ester can specifically be prepared by ester transesterification, and reaction raw materials can be methyl propionate and formic acid
Ethyl ester, propyl formate, butyl formate, ethyl acetate, propyl acetate, butyl acetate etc..
In traditional handicraft, production propionic ester frequently with catalyst be the concentrated sulfuric acid, reactant be propionic acid and alcohol directly into
It is prepared by row esterification.There is shortcomings for the method, and such as corrosive equipment, environment easy to pollute, side reaction is more, post-processes
It is complicated, efficiency is lower, continuous production is difficult to realize etc..With science and technology fast development, people's environmental consciousness it is universal
Raising is improved day by day with environmental regulation, and the advantage of environment-friendly type catalyst is also increasingly valued by people, and selection uses it
Its new catalyst is imperative as catalyst preparation propionic ester to substitute the concentrated sulfuric acid.
In recent years, domestic and foreign scholars had done a large amount of research work to synthesizing propionate, but really put into industrial metaplasia
The problems such as report of production is seldom, and it is inefficient to be primarily due to that there are catalysts, and preparation process is complicated, stability is poor.
Propionic ester is only esterified in existing literature and patent and prepared by carbonyl process.Esterification process be using propionic acid and alcohol as raw material,
Use the inorganic acid such as concentrated sulfuric acid for catalyst, alcoholic acid esterification method energy consumption is high, consumes a large amount of soda acids, and production technology cost is high, and
There is very big pollution to environment, it is difficult to meet the needs of modern chemical industry development and the requirement of environmental protection.Carbonylation rule is anti-
Condition is answered to require high, and there are side reactions.The support type Rh catalyst of Zhang Zhixian et al. research, with C2H5I is co-catalyst,
240 DEG C, under 1.5MPa, ethanol conversion contains propionic acid 64% in product, ethyl propionate is only 34%, and there are 3% second up to 97%
Ether.The Ni-Cu/ activated-carbon catalyst of Deng Guixiang et al. research, with C2H2I is co-catalyst, at 300 DEG C, 0.1MPa, is carried out
The reaction of gas-solid phase ethanol carbonylation, product only have ethyl propionate, and yield is 50~60%, but catalyst activity is lower.Ge Qingxiu
It is propionic acid and ethyl alcohol and certain solvent composition is non-aqueous when specific method Deng utilizing alkaline fat Enzyme catalyzed synthesis ethyl propionate
Phase esterification system.The optimal reaction temperature of the method is 32~36 DEG C, more harsh to temperature requirement, therefore utilizes alkalinity
Lipase is not satisfactory to catalyze and synthesize ethyl propionate.Propionic ester is prepared by esterification process and carbonyl process, has by-product, and produce
There are alcohols in object, lithium electricity grade propionic ester requires purity is high, cannot have other trace impurities, therefore, pass through esterification and carbonyl
Changing reaction, lithium-ion battery electrolytes low temperature properties are not satisfactory for improving to obtain ethyl propionate, open up a new reaction road
Line and the high-purity propionic ester of technique large scale preparation are of great significance.
There is the report of numerous studies ester exchange reaction in the country, as propene carbonate and methanol transesterification prepare carbonic acid diformazan
Ester, dimethyl carbonate and ethyl alcohol transesterification prepare methyl ethyl carbonate etc., but several by the report of ester transesterification synthesizing propionate
Do not have.The technique that we propose a kind of homogeneous catalysis synthesizing propionate herein.
Summary of the invention
The purpose of the present invention is open up one it is completely new it is heterogeneous using high-performance solid alkali be catalyst methyl propionate with
Various esters such as Ethyl formate, propyl formate, butyl formate, ethyl acetate, the one-step synthesis propionic acid such as propyl acetate, butyl acetate
The catalytic rectification process of ester.
The present invention is achieved by the following technical solutions.
A kind of homogeneous catalysis rectification process preparing propionic ester by ester transesterification is with homogeneous solvable alkali or ionic liquid
Body is that catalyst methyl propionate and reaction raw materials ester one-step synthesis propionic ester, reaction equation are as follows:
C4H8O2+R1COOR2→C2H5COOR2+R1COOCH3。
Specifically, the cation of the ionic liquid of the homogeneous solvable alkali is any one in quaternary ammonium or quaternary phosphonium cations
Kind, anion is any one in acid or basic functionality.
Specifically, the reaction raw materials ester and methyl propionate molar ratio 0.5:1~1:20, the complete raw material propionic acid first of unreacted
Ester returns to reaction zone and carries out conversion and cycle.
Specifically, the concrete operations of above-mentioned catalytic rectification process are as follows:
A) excessive methyl propionate and reaction raw materials ester are reacted under certain reaction condition, product propionic acid ester and certain acid
Methyl esters；
B) the sour methyl esters boiling point of product is minimum, separates out reaction system from rectifying tower top part, driving a reaction carries out to the right；
C) excessive methyl propionate raw material is added, by catalytic rectification process, makes certain sour methyl esters fully reacting；
D) mixture methyl propionate boiling point is lower than propionic acid ester, and rectifying is isolated methyl propionate and used as feedstock circulation,
Higher boiling propionic acid ester rectification and purification in product tower.
Specifically, in above-mentioned steps a), excessive methyl propionate, reaction raw materials ester and solvable alkali or ionic liquid are by counting
After the preheated device V-1 preheating of amount pump P-1, enter rectifying column from middle and upper part, rectifying tower bottom persistently supplements methyl propionate, reflux ratio
For 1:1, in rectifying column, excessive methyl propionate is sufficiently reacted with propyl acetate.
From the above technical scheme, it can be seen that the beneficial effects of the present invention are:
The production technology for the synthesizing propionate that the present invention opens up, it is advantageous that reaction system is simple, response path is short；It produces
Object selectivity is high, with high purity, and complete no coupling product generates；Reaction time is short, and catalyst activity is high, and catalyst is reusable；
It generally can be easily separated without azeotropic between reaction raw materials ester and product ester, to extensive, inexpensive production high added value, high-purity
Propionic ester is of great significance, entire reaction process green, energy-saving and environmental protection and efficiently.The technique used catalyst is solvable alkali
Or ionic liquid, catalytic activity is high, catalyst performance stabilised non-inactivation, and usage amount is the 0.3- of the total mass of raw material
5wt%, it is at low cost.
Detailed description of the invention
Fig. 1 is ester transesterification synthesizing propionate homogeneous catalysis process flow chart
Specific embodiment
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.Reality used in the examples
The condition of applying can be for further adjustments according to the condition of producer, and unaccounted implementation condition is usually conventional laboratory conditions.
By taking methyl propionate and propyl acetate prepare propyl propionate as an example, reaction equation is as follows:
C4H8O2+C5H10O2→C6H12O2+C3H6O2
A) be that raw material reacts under certain reaction condition by excessive methyl propionate and propyl acetate, product propyl propionate and
Methyl acetate；
B) acetic acid product methyl esters boiling point is minimum, separates out reaction system from rectifying tower top part, driving a reaction carries out to the right；
C) by catalytic rectification process, make propyl acetate fully reacting as far as possible；
D) target product propyl propionate boiling point highest and excessive methyl propionate remain in catalytic rectifying tower tower reactor.
E) methyl propionate isolated is used as feedstock circulation.
The homogeneous catalyst is KOH, and excessive methyl propionate, propyl acetate and KOH mixture are by metering pump P-1 through pre-
After hot device V-1 preheating, entering rectifying column T1 from middle and upper part, T1 rectifying tower bottom persistently supplements methyl propionate, reflux ratio 1:1,
In rectifying column, excessive methyl propionate is sufficiently reacted with propyl acetate, and product is propyl propionate and methyl acetate, raw acetic acid
Propyl ester is consumed significantly, and closer to T1 rectifying tower bottom, methyl propionate concentration is higher, and propyl acetate concentration is lower.
It is 55-70 DEG C that T1 rectifying column, which produces temperature, and the main component of extraction is 80wt% methyl acetate and 20wt% propionic acid
Methyl esters, methyl propionate and methyl acetate not azeotropic, into T2 rectifying tower bottom, overhead extraction temperature is 56-58 DEG C, and reflux ratio is
The top of the distillation column 2:1, T2 production be methyl acetate, bottom temperature be 75-80 DEG C, tower reactor residue be mainly methyl propionate and
Small part methyl acetate, is recycled to reaction raw materials.
T1 rectifying tower reactor group become 0.03wt% methyl acetate, 0.5wt% propyl acetate, 40wt% methyl propionate and
60wt% propyl propionate, tower reactor mix products are washed with the distilled water of its mass fraction 5wt%, and after stratification, upper layer is to have
Machine ester layer, lower layer are the water layer of the catalyst containing KOH, and upper layer ester layer goes T3 rectifying tower bottom, overhead extraction temperature after repetition is washed 3-5 times
Degree is 78-80 DEG C, and the main component of extraction is methyl propionate, is recycled as reaction raw materials, T3 tower bottom of rectifying tower residue
Into T4 rectifying column, overhead extraction temperature is 122-124 DEG C, obtains high-purity propyl propionate.
Water layer contains catalyst, a small amount of methyl propionate and propyl propionate, into T5 tower bottom of rectifying tower.The top of the distillation column T5 temperature
Degree is 72-75 DEG C, and extraction group is divided into 3.9wt% water and 96.1wt% methyl propionate；Overhead extraction temperature is then improved to 100-
110 DEG C, remaining hydromining is gone out and (is recycled as water recently distilled), tower reactor residual is catalyst, and being recycled to reaction raw materials makes
With.For homogeneous catalysis process flow diagram as shown in Figure 1, the present invention produces the technique of propionic ester, reaction raw materials are excessive third
Sour methyl esters and other esters (including but not limited to Ethyl formate, propyl formate, butyl formate, ethyl acetate, propyl acetates, second
Acid butyl ester etc.) mixture, the two enters T1 rectifying column together, and the latter's esters are reacted completely, and finally obtained product is propionic acid
Ester and other esters.The synthesis technology reactive distillation enormously simplifies the process flow of conventional propionic acid Lipase absobed, and separation purity
It is high.
The technique that the present invention produces propionic ester has following additional technical characteristic:
The device of present invention production propionic ester, comprising: T1 rectifying column, the T1 rectifying column centre have first charging aperture,
The tower bottom of the T1 rectifying column has the first discharge port connecting with T2 rectifying column, and the T1 rectifying column has and water washing device
Second discharge port of connection；T2 rectifying column, the T2 rectifying column middle part have second charging aperture, described the top of the distillation column T2 top
With third discharge port, the tower bottom of the T2 rectifying column has the 4th discharge port connecting with T1 rectifying column；T3 rectifying column, institute
Stating T3 rectifying column has the third feed inlet connecting with water washing device top, has and T1 rectifying column at the top of the T3 rectifying tower
5th discharge port of connection, the T3 tower bottom have the 6th discharge port connecting with T4；T4 rectifying column, the T4 rectifying column tool
There is the 4th feed inlet connecting with T3, there is the 7th discharge port at the top of the T4 rectifying column；T5 rectifying column, the T5 rectifying column tool
There is the 5th feed inlet connecting with water washing device, the T5 rectifier bottoms have the 8th discharge port connecting with T1 rectifying column,
There are the nine, the tenth discharge ports at the top of the T5 rectifying column.
Absolute pressure is 0.1MPa-5MPa in the tower of the T1 rectifying column, and tower top temperature is 55 DEG C -70 DEG C, column bottom temperature
It is 55-79.9 DEG C；The tower pressure interior force of the rectifying column T2 is 0.1-0.5MPa, and tower top temperature is 56-58 DEG C, and column bottom temperature is
75-80℃；The T3 rectifying column tower pressure interior force is 0.1-5MPa, and tower top temperature is 70-80 DEG C, the T4 rectifying column tower pressure interior force
For 0.1-5MPa, tower top temperature is 122-124 DEG C, and the T5 rectifying column tower pressure interior force is 0.1-5MPa, tower top temperature 72-
110℃。
The partition of heretofore described reactor and rectifying column is arranged to make the cross-sectional area of the fore-running section and the side
The ratio between cross-sectional area of line segment is 1:1-3:1.
The number of plates of fore-running section is 1~30 piece, and the side line section number of plates is 1~30 piece, the number of plates of public rectifying section is 1~
30 pieces, the number of plates of public stripping section is 1~30 piece.
T1 rectifying column, T2 rectifying column, T3 rectifying column, T4 rectifying column and T5 rectifying column are plate column, packed tower in the present invention
Or board-like-filler mixing column.
Embodiment 1
Using methyl propionate and propyl acetate as raw material, reaction generates propyl propionate and methyl acetate the mass ratio of the material is
1:1, excessive methyl propionate recycle.
Catalyst KOH dosage is the 0.3-5wt% of total mass of raw material sum, and the ratio between fore-running section and the cross-sectional area of side line section are
1:1.
Operating condition is as follows:
Rectifying column T1: tower diameter 1000mm；Tower height 19000mm；Public rectifying section, fore-running section, side line section, public stripping section
The number of plates is respectively 10,20,30,15；Tower pressure interior force 1MPa；60 DEG C of tower top temperature；71 DEG C of the column bottom temperature of public stripping section；Side
74 DEG C of the column bottom temperature of line segment.
Rectifying column T2: tower diameter 3000mm；Tower height 40000mm；Public rectifying section, fore-running section, side line section, public stripping section
The number of plates is respectively 10,20,30,15；Tower pressure interior force 1MPa；80 DEG C of tower top temperature, 85 DEG C of the column bottom temperature of public stripping section；Side
89 DEG C of the column bottom temperature of line segment.
Rectifying column T3: tower diameter 3000mm；Tower height 40000mm；Public rectifying section, fore-running section, side line section, public stripping section
The number of plates is respectively 10,20,30,15；Tower pressure interior force 1MPa；80 DEG C of tower top temperature, 75 DEG C of the column bottom temperature of public stripping section；Side
79 DEG C of the column bottom temperature of line segment.
Rectifying column T4: tower diameter 3000mm；Tower height 40000mm；Public rectifying section, fore-running section, side line section, public stripping section
The number of plates is respectively 10,20,30,15；Tower pressure interior force 1MPa；80 DEG C of tower top temperature, 85 DEG C of the column bottom temperature of public stripping section；Side
The charging of 89 DEG C of first reactive distillation column T1 of column bottom temperature of line segment and tower top composition result are as shown in the table
Influence of the different total raw material mass flows of table 1 to T1 the first reactive distillation column overhead each component mass fraction
Table 1 can be seen that, with the increase of total feed, tower top methyl acetate content first increases and then decreases, ethyl acetate, third
Sour methyl esters and ethyl propionate content are very low always.Reason is that inlet amount is bigger, causes material shorter in dwell time in the tower,
Reaction carries out insufficient.It is optimal total raw material mass flow when total raw material mass flow is 5000kg/h.
Embodiment 2
Under the operating condition of embodiment 1, when total raw material mass flow is 5000kg/h, change the first reactive distillation column of T1
Material molar ratio, the variation of tower top each component mass fraction are as shown in table 2.
Influence of the 2 different material molar ratio of table to T1 the first reactive distillation column overhead each component mass fraction
As can be seen from Table 2, with the increase of material molar ratio, tower top methyl acetate mass fraction is gradually reduced, second third
Ester mass fraction gradually increases, and is optimum feed stock ratio when propyl acetate and methyl propionate molar ratio are 1:2.
Embodiment 3
Under the operating condition of embodiment 2, total raw material mass flow is 5000kg/h, propyl acetate and methyl propionate mole
When than for 1:2, change the first reactive distillation column of T1 reflux ratio, the variation of tower top each component mass fraction is as shown in table 3.
The influence that the different reflux ratios of table 3 change T1 the first reactive distillation column overhead each component mass fraction
As can be seen from Table 3, with the increase of reflux ratio, tower top methyl acetate mass fraction is gradually increased, methyl propionate,
Propyl propionate and propyl acetate content reduce, it is seen that the increase of reflux ratio facilitates more tower top light component methyl acetates and returns to tower
Reaction is inside participated in again, improves the conversion ratio of reactant.
Embodiment 4
Due to the difference of raw material esters boiling point, temperature controlled difference in caused art production process.Now probe into use
Methyl propionate and ethyl acetate are as raw material, and reaction generates ethyl propionate and the technique of methyl acetate is as follows:
It is 55-70 DEG C that T1 rectifying column, which produces temperature, and the main component of extraction is 80wt% methyl acetate and 20wt% propionic acid
Methyl esters.Methyl propionate and methyl acetate not azeotropic, into T2 rectifying tower bottom, overhead extraction temperature is 56-58 DEG C, and reflux ratio is
The top of the distillation column 2:1, T2 production is methyl acetate.Bottom temperature be 75-80 DEG C, tower reactor residue be mainly methyl propionate and
Small part methyl acetate, is recycled to reaction raw materials.
T1 rectifying tower reactor group become 0.03wt% methyl acetate, 0.5wt% propyl acetate, 40wt% methyl propionate and
60wt% ethyl propionate.Tower reactor mix products are washed with the distilled water of its mass fraction 5wt%, and after stratification, upper layer is to have
Machine ester layer, lower layer are the water layer of the catalyst containing KOH, and upper layer ester layer goes T3 rectifying tower bottom, overhead extraction temperature after repetition is washed 3-5 times
Degree is 78-80 DEG C, and the main component of extraction is methyl propionate, is recycled as reaction raw materials, T3 tower bottom of rectifying tower residue
Into T4 rectifying column, overhead extraction temperature is 99.1-100 DEG C, obtains high-purity ethyl propionate.
Water layer contains catalyst, a small amount of methyl propionate and propyl propionate, into T5 tower bottom of rectifying tower.The top of the distillation column T5 temperature
Degree is 72-75 DEG C, and extraction group is divided into 3.9wt% water and 96.1wt% methyl propionate；Overhead extraction temperature is then improved to 100-
110 DEG C, remaining hydromining is gone out and (is recycled as water recently distilled), tower reactor residual is catalyst, and being recycled to reaction raw materials makes
With.
Absolute pressure is 0.1MPa-5MPa in the tower of first reactive distillation column of T1, and tower top temperature is 55 DEG C -70 DEG C,
Column bottom temperature is 55-79.9 DEG C；The tower pressure interior force of the rectifying column T2 is 0.1MPa-05MPa, and tower top temperature is 56-58 DEG C, tower
Bottom temperature is 75 DEG C -80 DEG C；It is 70-80 DEG C that the T3 rectifying column tower pressure interior force, which is 0.1MPa-5MPa tower top temperature,；The T5 essence
Evaporating tower tower pressure interior force is 0.1MPa-5MPa, and tower top temperature is 72-110 DEG C.
The above is only several embodiments of the application, not does any type of limitation to the application, although this Shen
Please disclosed as above with preferred embodiment, however not to limit the application, any person skilled in the art is not taking off
In the range of technical scheme, a little variation or modification are made using the technology contents of the disclosure above and is equal to
Case study on implementation is imitated, is belonged in technical proposal scope.
Claims (5)
1. a kind of homogeneous catalysis rectification process for preparing propionic ester by ester transesterification, which is characterized in that with homogeneous solvable alkali or
Person's ionic liquid is that catalyst methyl propionate and reaction raw materials ester one-step synthesis propionic ester, reaction equation are as follows:
C4H8O2+R1COOR2→C2H5COOR2+R1COOCH3。
2. a kind of homogeneous catalysis rectification process for preparing propionic ester by ester transesterification according to claim 1, feature
It is, the cation of the homogeneous solvable alkali or ionic liquid is any one in quaternary ammonium or quaternary phosphonium cations, anion
For any one in acid or basic functionality.
3. a kind of homogeneous catalysis rectification process for preparing propionic ester by ester transesterification according to claim 1, feature
It is, the reaction raw materials ester and methyl propionate molar ratio 0.5:1~1:20, the complete raw material methyl propionate of unreacted returns to reaction
Area carries out conversion and cycle.
4. a kind of homogeneous catalysis rectification process for preparing propionic ester by ester transesterification according to claim 1, feature
It is, the concrete operations of the technique are as follows:
A) excessive methyl propionate and reaction raw materials ester are reacted under certain reaction condition, product propionic acid ester and certain sour first
Ester；
B) the sour methyl esters boiling point of product is minimum, separates out reaction system from rectifying tower top part, driving a reaction carries out to the right；
C) excessive methyl propionate raw material is added, by catalytic rectification process, makes certain sour methyl esters fully reacting；
D) mixture methyl propionate boiling point is lower than propionic acid ester, and rectifying is isolated methyl propionate and used as feedstock circulation, high boiling
Point propionic acid ester rectification and purification in product tower.
5. a kind of homogeneous catalysis rectification process for preparing propionic ester by ester transesterification according to claim 4, feature
It is, in above-mentioned steps a), the ionic liquid of excessive methyl propionate, reaction raw materials ester and homogeneous solvable alkali is by metering pump P-1
After preheated device V-1 preheating, entering rectifying column from middle and upper part, rectifying tower bottom persistently supplements methyl propionate, reflux ratio 1:1,
In rectifying column, excessive methyl propionate is sufficiently reacted with propyl acetate.
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| CN104276949A (en) * | 2005-05-20 | 2015-01-14 | 赢创罗姆有限责任公司 | Transesterification Methods |
| WO2007125069A1 (en) * | 2006-04-28 | 2007-11-08 | Krause-Röhm-Systeme Ag | Method for transesterification of esters |
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