CN105712873A - Control method for synthesizing ethyl acetate by using esterification method - Google Patents
Control method for synthesizing ethyl acetate by using esterification method Download PDFInfo
- Publication number
- CN105712873A CN105712873A CN201610004822.6A CN201610004822A CN105712873A CN 105712873 A CN105712873 A CN 105712873A CN 201610004822 A CN201610004822 A CN 201610004822A CN 105712873 A CN105712873 A CN 105712873A
- Authority
- CN
- China
- Prior art keywords
- esterification
- ethyl acetate
- column
- control method
- reboiler
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention belongs to the field of processing of ethyl acetate, and particularly relates to a control method for synthesizing ethyl acetate by using an esterification method. The control method comprises the following steps: a, controlling molar ratio of acetic acid to ethanol in a mixer to be 1:1, and conveying mixed materials stirred evenly to an esterification tower; b, only arranging sulfuric acid at the bottom of the esterification tower; c, heating through an esterification reboiler and carrying out esterification reaction to obtain gaseous ethyl acetate and water; and d, feeding the gaseous ethyl acetate and the water into an esterification phase splitter through an esterification condenser and an esterification cooler to obtain the ethyl acetate. An existing ethyl acetate synthesizing system is simplified, the ratio of the acetic acid, the ethanol and the sulfuric acid as a catalyst and reaction temperature are controlled, then the technical problem of low production rate of the ethyl acetate in a traditional technology is solved, meanwhile, a follow-up separating system is simplified, then consumption of steam is reduced by 50%, and the production efficiency of the product is improved.
Description
Technical field
The invention belongs to ethyl acetate manufacture field, particularly relate to the control method of a kind of method for synthetizing ethyl acetate by esterification.
Background technology
The molecular formula of ethyl acetate is C4H8O2, and No. CAS is that the hydroxyl in acetic acid is replaced by ethyoxyl and the compound that generates for 141-78-6..Colourless transparent liquid, has fruit fragrant, volatile, to air-sensitive, can absorb water and divide, and moisture can make it slowly decompose and react acid.Ethyl acetate is also known as ethyl acetate.Pure ethyl acetate is the liquid that water white transparency has penetrating odor, it it is a kind of broad-spectrum fine chemical product, there is the dissolubility of excellence, quick-drying, of many uses, it is a kind of very important Organic Chemicals and fabulous industrial solvent, is widely used in the production process of acetate fiber, ethyl cellulose, chlorinated rubber, vinyl, cellulose acetate resin, synthetic rubber, coating and paint etc..
Chemical Manufacture produces ethyl acetate frequently with continuous esterification method, in strong acid homogeneous catalyst, under uniform temperature, pressure, there is esterification by raw acetic acid and ethanol, and product is easily separated prepared ethyl acetate product by a series of rectifying columns.
Owing to esterification is a reversible reaction, and esterification process process units adopts is that reactor and ceramic packing tower use as esterification device, response system is so easily made to there is problems in that 1, owing to adopting strong acid as catalyst in the esterification reaction, easily cause the side reaction such as sulfonation, carbonization, response system in Chemical Manufacture is caused to pollute fast, cleaning frequency is frequent, and ceramic packing washes away, corrodes, it is easy to make rectification effect decline；2, use in the reactor traditional esterifications method course of reaction as esterification device use, because ethanol conversion is relatively low, higher in the alcohol content of ceramic packing top of tower, unreacted ethanol completely is caused to bring subsequent separation system into, and unreacted alcohol completely needs to be again introduced into response system after separating and participates in esterification, consequently, it is possible to the energy consumption of reaction and piece-rate system in the process of esterification certainly will be caused to increase；
3, owing to esterification is a reversible reaction, existing technique is in order to improve the productivity of ester, and General System is more complicated, and steam consumption is big, thus reducing the profit margin of product.
Summary of the invention
The present invention is directed to the technical problem existed in above-mentioned traditional handicraft, it is proposed to the control method of the method for synthetizing ethyl acetate by esterification that a kind of method is reasonable, simple to operate, easy to use and energy consumption is relatively low, conversion ratio is high.
In order to achieve the above object, the technical solution used in the present invention is, a kind of control method of method for synthetizing ethyl acetate by esterification, including the blender being linked in sequence by pipeline and pipe fitting, esterification column, esterification condensator, esterification cooler and esterification phase separator, described esterification column is provided with esterification reboiler, arrange for loop between described esterification reboiler and esterification column, bottom in described esterification column is provided with distributor, the top of described distributor, being arranged at intervals with regular mellapak packing, described control method comprises the following steps:
The mol ratio of a, the acetic acid controlled in blender and ethanol is 1:1, stirs, the mixed material stirred is delivered to esterification column；
B, in the bottom of esterification column and only arrange catalyst sulfuric acid in the bottom of esterification column, the mixed material of a step mixing and stirring is distributed through distributor, falls within the bottom of esterification column；
C, fall within compound bottom esterification column and be delivered to esterification reboiler with sulphuric acid through pipeline, through esterification reboiler heating esterification, generate gaseous state ethyl acetate and water；
D, gaseous state ethyl acetate and water enter esterification phase separator through esterification condensator, esterification cooler, carry out liquid phase separation, obtain ethyl acetate；
Wherein, in described b step, the weight of catalyst sulfuric acid is the 1% of the weight of mixed material.
As preferably, in described step c, controlling temperature 125-128 DEG C of esterification reboiler.
As preferably, being provided with 160～170 layers of regular mellapak packing in described esterification column.
As preferably, the material of described regular mellapak packing is polypropylene.
As preferably, in described step c, it is 8:1 that control unreacted falls the mol ratio of the acetic acid in esterification column and ethanol again after rise.
As preferably, being additionally provided with tail gas condenser between described esterification condensator and esterification cooler.
As preferably, passing through pipeline communication between described esterification phase separator and esterification column.
Compared with prior art, advantages of the present invention and good effect are in that,
1, the present invention is by simplifying the synthesis system of existing ethyl acetate, by controlling proportioning and the reaction temperature of acetic acid and ethanol and catalyst sulfuric acid, and then solve in traditional handicraft, the technical problem that ethyl acetate production rate is low, simultaneously, simplify follow-up piece-rate system, and then make steam consumption reduce 50%, improve the formation efficiency of enterprise.
Accompanying drawing explanation
In order to be illustrated more clearly that the technical scheme of the embodiment of the present invention, below the accompanying drawing used required during embodiment is described is briefly described, apparently, accompanying drawing in the following describes is some embodiments of the present invention, for those of ordinary skill in the art, under the premise not paying creative work, it is also possible to obtain other accompanying drawing according to these accompanying drawings.
The operating system configuration schematic diagram of the control method of the method for synthetizing ethyl acetate by esterification that Fig. 1 provides for embodiment 1；
Above in each figure, 1, blender；11, acetic acid import；12, ethanol import；2, esterification column；21, distributor；3, esterification condensator；4, esterification cooler；5, esterification phase separator；6, waste pipe；7, ethyl acetate product pipe；8, esterification reboiler；9, regular mellapak packing；10, tail gas condenser.
Detailed description of the invention
In order to be more clearly understood that the above-mentioned purpose of the present invention, feature and advantage, below in conjunction with drawings and Examples, the present invention will be further described.It should be noted that when not conflicting, embodiments herein and the feature in embodiment can be mutually combined.
Elaborate a lot of detail in the following description so that fully understanding the present invention, but, the present invention can also adopt and be different from other modes described here and implement, and therefore, the present invention is not limited to the restriction of the specific embodiment of description described below.
Embodiment 1, the present embodiment provides the control method of a kind of method for synthetizing ethyl acetate by esterification
As shown in Figure 1, first the present embodiment simplifies the system of traditional industry method for synthetizing ethyl acetate by esterification, eliminate major part device, remain and have to use for blender 1, esterification column 2, esterification condensator 3, esterification cooler 4 and esterification phase separator 5, blender 1, esterification column 2, esterification condensator 3, esterification cooler 4 and esterification phase separator 5 are sequentially communicated by pipeline, blender 1 is provided with ethanol import 12 and acetic acid import 11, blender 1 is arranged on the material inlet of esterification column 2 also should be arranged on the bottom in esterification column 2, the concrete top being arranged on distributor 21, the material of esterification column 2 is entered from blender 1, after distributor 21 is distributed, fall within the bottom of esterification column 2, esterification column 2 is provided with the esterification reboiler 8 for heating, arrange for loop between esterification reboiler 8 and esterification column 2, bottom in esterification column 2 is provided with distributor 21, top at distributor 21, it is arranged at intervals with regular mellapak packing 9, in traditional esterification column, the material of filler is generally pottery, in the present embodiment, ceramic packing is changed into regular mellapak packing, concrete is regular Lamb wave stricture of vagina polypropylene filler, adopt the regular mellapak packing of polypropylene filler relative to traditional ceramic packing or its specific surface area of metal packing, the performances such as voidage improve very big, there is resistance little, uniform gas-liquid distribution, flux is big, the advantages such as amplification effect is inconspicuous, and then reduce the load in follow-up work, separation subsequent separation system is made to simplify, steam consumption reduces 50%, improve the conversion ratio of product, the production capacity making tower gets a promotion, reduce energy consumption, significantly improve production capacity.
The control method that the present embodiment provides, first traditional production system is proposed improvement, simplify traditional production system, additionally on it controls, it is also proposed improvement, first, the acetic acid controlled in blender 1 is that 1:1 mixes with the mol ratio of ethanol, stir, the mixed material stirred is delivered to esterification column 2, in esterification column 2 and only at the inside of esterification column 2 placement catalyst sulfuric acid, the placement amount of sulphuric acid is the 1% of the acetic acid total amount with ethanol, compound is after distributor 21 is distributed, fall within the bottom of esterification column 2, after being sufficiently mixed with the material bottom esterification column 2, through esterification reboiler 8 steam heating, control reaction temperature 125 DEG C-128 DEG C, carry out esterification, reaction generates the azeotropic mixture of ethyl acetate and water, after the rectification of regular mellapak packing 9, enter esterification condensator 3, esterification cooler 4, finally carry out liquid phase separation through esterification phase separator 5, obtain ethyl acetate.When reaction, in order to ensure the productivity of ethyl acetate, temperature 80～95 DEG C in the tower of esterification column 2 should be controlled, tower top temperature 70～75 DEG C, system pressure 0.01～0.05Mpa, and the mol ratio that need to control the acetic acid at the bottom of esterification column tower and ethanol should control at 8:1, the temperature of timely adjustment esterification reboiler 8, to control esterification reaction temperature.
By above-mentioned control method and with simplified system after cooperate, and then finally make native system esterification column eject material containing alcohol less than 0.05%, containing acid less than 0.004%, later separation simplifies, and energy consumption declines, simultaneously, guaranteeing that the mol ratio of the acetic acid at the bottom of esterification column and ethanol should control at 8:1, and then bed material uses the time long, the clear still frequency reduces more than 50%, finally making esterification reaction rate improve, production capacity improves more than 20%.After actually used, productivity >=97% of the final ethyl acetate of control method of the method for synthetizing ethyl acetate by esterification that the present embodiment provides.
In order to further reduce energy consumption, in the present embodiment, it is additionally provided with tail gas condenser 10 between esterification condensator 3 and esterification cooler 4, in esterification condensator 3, the azeotropic mixture of a part of uncooled ethyl acetate and water enters tail gas condenser 10, and then the condensation effect of raising esterification condensator 3, the condensed product of final esterification condensator 3 and tail gas condenser 10 enters esterification cooler 4 jointly.
Ethyl acetate and water after esterification cooler 4 cooling eventually enter into esterification phase separator 5, carry out liquid phase separation, water after separation enters waste pipe 6, now, and containing alcohol less than 0.05% in waste water, containing acid less than 0.004%, ethyl acetate is partly into ethyl acetate product pipe 7 as product extraction, and another part reenters esterification column 2, such setting as backflow, be conducive to economizing on resources, reduce energy expenditure during follow-up wastewater treatment.
In order to better ensure that it reacts, obtain higher productivity, esterification column planted agent controls liquid level well, preferably should equipped with far transmission level meter bottom esterification column 2, should control material liquid level height from the bottom of tower to distributor 21 height 2/3 place, such control, is conducive to material to mix fully, and then better reacts.
The above; it it is only presently preferred embodiments of the present invention; it is not the restriction that the present invention is made other form; the Equivalent embodiments that any those skilled in the art were changed or be modified as equivalent variations possibly also with the technology contents of the disclosure above is applied to other field; but it is every without departing from technical solution of the present invention content; according to any simple modification, equivalent variations and remodeling that above example is made by the technical spirit of the present invention, still fall within the protection domain of technical solution of the present invention.
Claims (7)
1. the control method of a method for synthetizing ethyl acetate by esterification, including the blender being linked in sequence by pipeline and pipe fitting, esterification column, esterification condensator, esterification cooler and esterification phase separator, described esterification column is provided with esterification reboiler, arrange for loop between described esterification reboiler and esterification column, bottom in described esterification column is provided with distributor, it is characterised in that the top of described esterification column, being arranged at intervals with the regular mellapak packing of some layers, described control method comprises the following steps:
The mol ratio of a, the acetic acid controlled in blender and ethanol is 1:1, stirs；The mixed material stirred is delivered to esterification column；
B, in the bottom of esterification column and only arrange catalyst sulfuric acid in the bottom of esterification column, the mixed material of a step mixing and stirring is distributed through distributor, falls within the bottom of esterification column；
C, fall within compound bottom esterification column and be delivered to esterification reboiler with sulphuric acid through pipeline, carry out esterification through esterification reboiler heating, generate gaseous state ethyl acetate and water；
D, gaseous state ethyl acetate and water enter esterification phase separator through esterification condensator, esterification cooler, carry out liquid phase separation, obtain ethyl acetate；
Wherein, in described 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, it is characterised in that in described step c, controls temperature 125-128 DEG C of esterification reboiler.
3. the control method of method for synthetizing ethyl acetate by esterification according to claim 1, it is characterised in that be provided with 160～170 layers of regular mellapak packing in described esterification column.
4. the control method of method for synthetizing ethyl acetate by esterification according to claim 3, it is characterised in that the material of described regular mellapak packing is polypropylene.
5. the control method of method for synthetizing ethyl acetate by esterification according to claim 4, it is characterised in that in described step c, it is 8:1 that control unreacted falls the mol ratio of the acetic acid in esterification column and ethanol again after rise.
6. the control method of method for synthetizing ethyl acetate by esterification according to claim 5, it is characterised in that be additionally provided with tail gas condenser between described esterification condensator and esterification cooler.
7. the control method of method for synthetizing ethyl acetate by esterification according to claim 6, it is characterised in that pass through pipeline communication between described esterification phase separator and esterification column.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610004822.6A CN105712873B (en) | 2016-01-04 | 2016-01-04 | The control method of method for synthetizing ethyl acetate by esterification |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610004822.6A CN105712873B (en) | 2016-01-04 | 2016-01-04 | The control method of method for synthetizing ethyl acetate by esterification |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105712873A true CN105712873A (en) | 2016-06-29 |
| CN105712873B CN105712873B (en) | 2019-02-22 |
Family
ID=56147638
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610004822.6A Active CN105712873B (en) | 2016-01-04 | 2016-01-04 | The control method of method for synthetizing ethyl acetate by esterification |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105712873B (en) |
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 |
-
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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105712873B (en) | 2019-02-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP4049748A1 (en) | Gas-liquid bubbling bed reactor, reaction system and method for synthesizing carbonate | |
| CN106631684A (en) | Method for preparing SBA(sec-butyl alcohol) through hydrolysis with sec-butyl acetate | |
| CN102557932B (en) | Method for producing isobutyl acetate | |
| CN106928021A (en) | A kind of method of preparing ethylene glycol by using dimethyl oxalate plus hydrogen | |
| CN110407779A (en) | The method for preparing 5 hydroxymethyl furfural as raw material using biomass | |
| CN104557524A (en) | Production method of ethyl acetate | |
| CN109865493A (en) | A kind of twin drum bubble column reaction unit and reaction process for p xylene oxidation | |
| CN106349473A (en) | Method for preparing dipolyethylene glycol maleate by using ionic liquid | |
| CN102964248B (en) | Method for producing nitric oxide and synthesizing dimethyl oxalate through carbonylation | |
| CN105384629B (en) | A kind of energy-conserving and environment-protective production technology of the different monooctyl ester of lactic acid | |
| CN105712873A (en) | Control method for synthesizing ethyl acetate by using esterification method | |
| CN103193636A (en) | Method for synthetizing 2,3-butanediol ester | |
| CN103387495A (en) | Method for the continuous production of carboxylic acid esters | |
| CN206188686U (en) | Device of butyraldehyde oxidation preparation butyric acid | |
| CN203212506U (en) | Efficient ethyl acetate reaction rectification device | |
| CN102219679B (en) | Method for producing oxalic acid ester through CO gas phase coupling | |
| CN108083982A (en) | A kind of preparation method of methylallyl alcohol | |
| CN102992973B (en) | Industrial method for synthesizing p-hydroxy benzaldehyde in jet flow manner | |
| CN110498782B (en) | Continuous preparation method of 2, 5-dimethyl-4-hydroxy-3 (2H) furanone | |
| CN102060816A (en) | Synthesis method of gamma-nonalactone | |
| CN102260170B (en) | Method for microwave pipeline production of butyl acetate | |
| CN106995359A (en) | A kind of isobutene polymerisation prepares the method and device of triisobutylene sum | |
| CN113233983A (en) | Method for catalytically synthesizing linalyl acetate by using acidic deep eutectic solvent | |
| CN207537372U (en) | Continuous reaction rectification production cyanoacetate compound, malonate compound device | |
| CN1184187C (en) | Gas phase catalytic esterification process and equipment |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
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. |
|
| TR01 | Transfer of patent right |