CN105712873B - The control method of method for synthetizing ethyl acetate by esterification - Google Patents
The control method of method for synthetizing ethyl acetate by esterification Download PDFInfo
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- CN105712873B CN105712873B CN201610004822.6A CN201610004822A CN105712873B CN 105712873 B CN105712873 B CN 105712873B CN 201610004822 A CN201610004822 A CN 201610004822A CN 105712873 B CN105712873 B CN 105712873B
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- 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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Abstract
The invention belongs to ethyl acetate manufacture field more particularly to a kind of control methods of method for synthetizing ethyl acetate by esterification.Include the following steps, the molar ratio of a, the acetic acid in control mixer and ethyl alcohol are 1:1, and the mixed material stirred evenly is delivered to esterification column；B, in the bottom of esterification column and only in the bottom of esterification column setting sulfuric acid；C, esterification is heated through esterification reboiler, generates gaseous state ethyl acetate and water；D, gaseous state ethyl acetate and water enter esterification phase-splitter through esterification condensator, esterification cooler, obtain ethyl acetate；The synthesis system that the present invention passes through simplified existing ethyl acetate, by the proportion and reaction temperature that control acetic acid and ethyl alcohol and catalyst sulfuric acid, and then it solves in traditional handicraft, the low technical problem of ethyl acetate production rate, simultaneously, subsequent separation system is simplified, and then steam consumption is made to reduce 50%, improves the formation efficiency of product.
Description
Technical field
The invention belongs to ethyl acetate manufacture field more particularly to a kind of control methods of method for synthetizing ethyl acetate by esterification.
Background technique
The molecular formula of ethyl acetate is C4H8O2, No. CAS to be hydroxyl in acetic acid replaced by ethyoxyl for 141-78-6. and
The compound of generation.Colourless transparent liquid has fruit perfume, volatile, to air-sensitive, can absorb water and divide, moisture can make it slowly
It decomposes and reacts acid.Ethyl acetate is also known as ethyl acetate.Pure ethyl acetate is colorless and transparent with penetrating odor
Liquid, be a kind of widely used fine chemical product, there is excellent dissolubility, quick-drying, it is widely used, be a kind of non-
Normal important Organic Chemicals and fabulous industrial solvent, are widely used in acetate fiber, ethyl cellulose, chlorinated rubber, second
In the production process of olefine resin, cellulose acetate resin, synthetic rubber, coating and paint etc..
Produce ethyl acetate frequently with continuous esterification method in Chemical Manufacture, i.e., it is raw acetic acid and ethyl alcohol is homogeneous in strong acid
Esterification occurs in catalyst under certain temperature, pressure, and reaction product is subjected to separation system by a series of rectifying columns
Obtain ethyl acetate product.
Since esterification is a reversible reaction, and esterification process process units is using reaction kettle and ceramic packing tower
It is used as esterification device, easily has the following problems reaction system in this way: 1, urged due to using strong acid to be used as in the esterification reaction
Agent easily causes the side reactions such as sulfonation, charing, and the reaction system in Chemical Manufacture is caused to pollute fastly, and the cleaning frequency is frequent, and makes pottery
Porcelain filling washes away, corrodes, and is easy to decline rectification effect；2, the traditional esterifications method reaction for using reaction kettle to use as esterification device
In the process, higher in the alcohol content of ceramic packing top of tower because ethanol conversion is lower, cause the complete ethyl alcohol of unreacted to bring into
Subsequent separation system, and the complete alcohol of unreacted needs to be again introduced into reaction system after separation and participates in esterification, so
One, it is reacted during being bound to cause esterification and the energy consumption of separation system increases；
3, since esterification is a reversible reaction, for prior art in order to improve the yield of ester, General System is more multiple
Miscellaneous, steam consumption is big, to reduce the profit margin of product.
Summary of the invention
The present invention for technical problem present in above-mentioned traditional handicraft, propose a kind of method it is reasonable, it is easy to operate, make
With convenient and lower, high conversion rate the method for synthetizing ethyl acetate by esterification of energy consumption control method.
In order to achieve the above object, the technical solution adopted by the present invention is a kind of control of method for synthetizing ethyl acetate by esterification
Method, including mixer, esterification column, esterification condensator, esterification cooler and the esterification being linked in sequence by pipeline and pipe fitting
Phase-splitter is provided with esterification reboiler on the esterification column, is arranged between esterification reboiler and the esterification column for loop, described
Bottom in esterification column is provided with distributor, and the top of the distributor is arranged at intervals with regular mellapak packing, the control
Method the following steps are included:
A, the molar ratio for controlling acetic acid and ethyl alcohol in mixer is 1:1, is stirred evenly, the mixed material that will be stirred evenly
It is delivered to esterification column；
B, in the bottom of esterification column and only in the bottom of esterification column setting catalyst sulfuric acid, a step is mixed evenly
Mixed material is distributed through distributor, falls within the bottom of esterification column；
C, the mixture for being esterified tower bottom and sulfuric acid are fallen within through pipeline to reboiler is esterified, through esterification reboiler heating
Esterification generates gaseous state ethyl acetate and water；
D, gaseous state ethyl acetate and water enter esterification phase-splitter through esterification condensator, esterification cooler, carry out liquid phase separation,
Obtain ethyl acetate；
Wherein, in the b step, the weight of catalyst sulfuric acid is the 1% of the weight of mixed material.
Preferably, in the step c, 125-128 DEG C of temperature of control esterification reboiler.
Preferably, being provided with 160~170 layers of regular mellapak packing in the esterification column.
Preferably, the material of the regular mellapak packing is polypropylene.
Preferably, control unreacted is fallen after rise again in the molar ratio of acetic acid and ethyl alcohol in esterification column in the step c
For 8:1.
Preferably, being additionally provided with tail gas condenser between the esterification condensator and esterification cooler.
Preferably, being connected between esterification phase-splitter and the esterification column by pipeline.
Compared with prior art, the advantages and positive effects of the present invention are,
1, the present invention passes through control acetic acid and ethyl alcohol and catalyst by the synthesis system of simplified existing ethyl acetate
The proportion and reaction temperature of sulfuric acid, and then solve in traditional handicraft, the low technical problem of ethyl acetate production rate, meanwhile,
Subsequent separation system is simplified, and then steam consumption is made to reduce 50%, improves the formation efficiency of enterprise.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, required use in being described below to embodiment
Attached drawing be briefly described, it should be apparent that, drawings in the following description are some embodiments of the invention, for ability
For the those of ordinary skill of domain, without any creative labor, it can also be obtained according to these attached drawings others
Attached drawing.
Fig. 1 is the operating system configuration schematic diagram of the control method for the method for synthetizing ethyl acetate by esterification that embodiment 1 provides；
In above each figure, 1, mixer；11, acetic acid import；12, ethyl alcohol import；2, esterification column；21, distributor；3, it is esterified
Condenser；4, it is esterified cooler；5, it is esterified phase-splitter；6, waste pipe；7, ethyl acetate product pipe；8, it is esterified reboiler；9, it advises
Whole plate ripple packing；10, tail gas condenser.
Specific embodiment
To better understand the objects, features and advantages of the present invention, with reference to the accompanying drawings and examples
The present invention will be further described.It should be noted that in the absence of conflict, in embodiments herein and embodiment
Feature can be combined with each other.
In the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention, still, the present invention may be used also
To be implemented using other modes described herein are different from, therefore, the present invention is not limited to the specific of specification is described below
The limitation of embodiment.
Embodiment 1, the present embodiment provides a kind of control methods of method for synthetizing ethyl acetate by esterification
As shown in Figure 1, the system that the present embodiment simplifies traditional industry method for synthetizing ethyl acetate by esterification first, eliminates big
Partial devices remain the mixer 1 that must be used, esterification column 2, esterification condensator 3, esterification cooler 4 and esterification split-phase
Device 5, mixer 1, esterification column 2, esterification condensator 3, esterification cooler 4 and esterification phase-splitter 5 are sequentially communicated by pipeline,
Ethyl alcohol import 12 and acetic acid import 11 are provided on mixer 1, the material inlet that esterification column 2 is arranged in mixer 1 should also be set
The lower part in esterification column 2 is set, the top of distributor 21 is specifically set, the material of esterification column 2, warp are entered from mixer 1
After distributor 21 is distributed, the bottom of esterification column 2 is fallen within, esterification reboiler 8 for heating is provided on esterification column 2, is esterified
It is arranged between reboiler 8 and esterification column 2 for loop, the bottom in esterification column 2 is provided with distributor 21, on the top of distributor 21
Portion is arranged at intervals with regular mellapak packing 9, and in traditional esterification column, the material of filler is generally ceramics, in the present embodiment
In, ceramic packing is changed to regular mellapak packing, is specifically regular Lamb wave line polypropylene filler, using polypropylene filler
Regular mellapak packing improved relative to the performances such as traditional ceramic packing or metal packing its specific surface area, voidage it is very big,
Have many advantages, such as that small resistance, uniform gas-liquid distribution, flux are big, amplification effect is unobvious, and then reduces negative in follow-up work
Lotus simplifies separation subsequent separation system, and steam consumption reduces 50%, improves the conversion ratio of product, obtains the production capacity of tower
To promotion, energy consumption is reduced, production capacity is significantly improved.
Control method provided in this embodiment proposes improvement to traditional production system first, simplifies traditional life
In addition production system also proposed improvement in its control, firstly, the molar ratio of acetic acid and ethyl alcohol in control mixer 1 is 1:1
It is mixed, is stirred evenly, the mixed material stirred evenly is delivered to esterification column 2, in esterification column 2 and only in esterification column 2
Inside place catalyst sulfuric acid, the placement amount of sulfuric acid is the 1% of the total amount of acetic acid and ethyl alcohol, and mixture is distributed through distributor 21
Afterwards, the bottom for falling within esterification column 2, after being sufficiently mixed with the material of 2 bottom of esterification column, through esterification 8 steam of reboiler heating, control
125 DEG C -128 DEG C of reaction temperature, esterification is carried out, reaction generates the azeotropic mixture of ethyl acetate and water, fills out through regular Lamb wave line
After expecting 9 rectifying, into esterification condensator 3, esterification cooler 4, liquid phase separation finally is carried out through esterification phase-splitter 5, obtains acetic acid
Ethyl ester.In reaction, in order to guarantee the yield of ethyl acetate, 80~95 DEG C of temperature, tower top temperature in the tower of esterification column 2 should be controlled
70~75 DEG C, 0.01~0.05Mpa of system pressure, and the molar ratio for the acetic acid and ethyl alcohol that need to control esterification column tower bottom should control
8:1, timely adjustment is esterified the temperature of reboiler 8, to control esterification reaction temperature.
By above-mentioned control method and with simplify system after cooperate, and then finally eject this system esterification column
Alcohol-containing 0.05% is expected hereinafter, energy consumption declines, simultaneously, it is ensured that the second at esterification column bottom containing acid 0.004% hereinafter, later separation simplifies
The molar ratio of acid and ethyl alcohol should be controlled in 8:1, and then bottom material is long using the time, and the clear kettle frequency reduces 50% or more, finally make ester
Change reaction rate to improve, production capacity improves 20% or more.After actually using, method for synthetizing ethyl acetate by esterification provided in this embodiment
The final ethyl acetate of control method yield >=97%.
In order to further reduce energy consumption, in the present embodiment, also set between esterification condensator 3 and esterification cooler 4
It is equipped with tail gas condenser 10, it is cold to enter tail gas for the azeotropic mixture of a part of uncooled ethyl acetate and water in esterification condensator 3
Condenser 10, and then improve the condensation effect of esterification condensator 3, final esterification condensator 3 and tail gas condenser 10 it is condensed
Product enters esterification cooler 4 jointly.
Esterification phase-splitter 5 is eventually entered into through the esterification ethyl acetate after cooling of cooler 4 and water, carries out liquid phase separation, point
Water from after enters waste pipe 6, at this point, alcohol-containing 0.05% is hereinafter, containing acid 0.004% hereinafter, ethyl acetate is a part of in waste water
It is produced into ethyl acetate product pipe 7 as product, another part reenters esterification column 2 as reflux, and such setting has
Conducive to economizing on resources, energy consumption when subsequent wastewater treatment is reduced.
In order to preferably guarantee its reaction, higher yield is obtained, liquid level should be controlled in esterification column, preferably in esterification column
2 bottoms should be equipped with far transmission level meter, should control material liquid level height from tower bottom at the 2/3 of 21 height of distributor, such control
System, is conducive to material and adequately mixes, and then preferably react.
The above described is only a preferred embodiment of the present invention, being not that the invention has other forms of limitations, appoint
What those skilled in the art changed or be modified as possibly also with the technology contents of the disclosure above equivalent variations etc.
It imitates embodiment and is applied to other fields, but without departing from the technical solutions of the present invention, according to the technical essence of the invention
Any simple modification, equivalent variations and remodeling to the above embodiments, still fall within the protection scope of technical solution of the present invention.
Claims (7)
1. a kind of control method of method for synthetizing ethyl acetate by esterification, including mixer, the ester being linked in sequence by pipeline and pipe fitting
Change tower, esterification condensator, esterification cooler and esterification phase-splitter, is provided with esterification reboiler, the ester on the esterification column
Change and be arranged between reboiler and esterification column for loop, the bottom in the esterification column is provided with distributor, which is characterized in that described
The top of esterification column is arranged at intervals with the regular mellapak packing of several layers, the control method the following steps are included:
A, the molar ratio for controlling acetic acid and ethyl alcohol in mixer is 1:1, is stirred evenly；The mixed material stirred evenly is conveyed
To esterification column；
B, in the bottom of esterification column and only in the bottom of esterification column setting catalyst sulfuric acid, the mixing that a step is mixed evenly
Material is distributed through distributor, falls within the bottom of esterification column；
C, the mixture for being esterified tower bottom and sulfuric acid are fallen within through pipeline to reboiler is esterified, is carried out through esterification reboiler heating
Esterification generates gaseous state ethyl acetate and water；
D, gaseous state ethyl acetate and water enter esterification phase-splitter through esterification condensator, esterification cooler, carry out liquid phase separation, obtain
Ethyl acetate；
Wherein, in the b step, the weight of catalyst sulfuric acid is the 1% of the weight of mixed material.
2. the control method of method for synthetizing ethyl acetate by esterification according to claim 1, which is characterized in that in the step c,
125-128 DEG C of temperature of control esterification reboiler.
3. the control method of method for synthetizing ethyl acetate by esterification according to claim 1, which is characterized in that in the esterification column
It is provided with 160~170 layers of regular mellapak packing.
4. the control method of method for synthetizing ethyl acetate by esterification according to claim 3, which is characterized in that the regular Lamb wave
The material of line filler is polypropylene.
5. the control method of method for synthetizing ethyl acetate by esterification according to claim 4, which is characterized in that in the step c,
Control unreacted fall after rise again in acetic acid and ethyl alcohol in esterification column molar ratio be 8:1.
6. the control method of method for synthetizing ethyl acetate by esterification according to claim 5, which is characterized in that the esterification condensation
Tail gas condenser is additionally provided between device and esterification cooler.
7. the control method of method for synthetizing ethyl acetate by esterification according to claim 6, which is characterized in that the esterification split-phase
It is connected between device and esterification column by pipeline.
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| CN201610004822.6A CN105712873B (en) | 2016-01-04 | 2016-01-04 | The control method of method for synthetizing ethyl acetate by esterification |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7253307B1 (en) * | 2002-05-01 | 2007-08-07 | Rohm And Haas Company | Process for production of methacrylic acid |
| CN102285879A (en) * | 2011-06-29 | 2011-12-21 | 张超 | Reinforced phase splitting production device for synthesizing ethyl acetate by esterification process |
| CN203212506U (en) * | 2013-04-10 | 2013-09-25 | 临沂市金沂蒙生物科技有限公司 | Efficient ethyl acetate reaction rectification device |
| CN103467285A (en) * | 2013-06-09 | 2013-12-25 | 百川化工(如皋)有限公司 | Method for reducing acidity of acetate |
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2016
- 2016-01-04 CN CN201610004822.6A patent/CN105712873B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7253307B1 (en) * | 2002-05-01 | 2007-08-07 | Rohm And Haas Company | Process for production of methacrylic acid |
| CN102285879A (en) * | 2011-06-29 | 2011-12-21 | 张超 | Reinforced phase splitting production device for synthesizing ethyl acetate by esterification process |
| CN203212506U (en) * | 2013-04-10 | 2013-09-25 | 临沂市金沂蒙生物科技有限公司 | Efficient ethyl acetate reaction rectification device |
| CN103467285A (en) * | 2013-06-09 | 2013-12-25 | 百川化工(如皋)有限公司 | Method for reducing acidity of acetate |
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Effective date of registration: 20200319 Address after: 276000, No. 99, Da Xing West Street, Linshu County, Linyi, Shandong Patentee after: LINYI JINYIMENG BIOTECHNOLOGY Co.,Ltd. Address before: 276017, No. 99, Da Xing West Street, Linshu County, Linyi, Shandong Patentee before: JINYIMENG GROUP Co.,Ltd. |