CN102285879A - Reinforced phase splitting production device for synthesizing ethyl acetate by esterification process - Google Patents
Reinforced phase splitting production device for synthesizing ethyl acetate by esterification process Download PDFInfo
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- CN102285879A CN102285879A CN2011101789285A CN201110178928A CN102285879A CN 102285879 A CN102285879 A CN 102285879A CN 2011101789285 A CN2011101789285 A CN 2011101789285A CN 201110178928 A CN201110178928 A CN 201110178928A CN 102285879 A CN102285879 A CN 102285879A
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- esterification
- ethyl acetate
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- phase splitter
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Abstract
The invention provides a reinforced phase splitting production device for synthesizing ethyl acetate by an esterification process and belongs to a carboxylic ester preparation device. The reinforced phase splitting production device for synthesizing ethyl acetate by the esterification process comprises an esterification kettle (1), a reboiler (2), an esterification tower (3), a condenser A (4), a condenser B (5), a phase splitter (6) and a circulating pump (7), and is characterized in that a fibrous bed reinforced phase splitter (8) is arranged between the outlet pipe of the circulating pump (7) and the return pipe of the esterification tower (3). The reinforced phase splitting production device for synthesizing ethyl acetate by the esterification process, which is provided by the invention has the advantages that: the reaction speed is high; the raw material conversion rate is high; the raw materials are saved; the cost of the water treatment system is reduced; energy is saved; the production capacity of the device is improved; byproducts are reduced; and the purity of the product is improved. When the device is used, the production period of each batch of ethyl acetate is 3 hours; and the raw material conversion rate based on an acetic acid raw material is 99.95 percent. The reflux ratio of the device is 2, the ethyl acetate content is 99.5 weight percent. The production device is suitable for all esterification reactions of organic acids and alcohols for forming esters and water.
Description
Technical field
The present invention is that a kind of method for synthetizing ethyl acetate by esterification is strengthened the phase-splitting production equipment, belongs to the preparation facilities of carboxylicesters.Be particularly related to the preparation facilities of ethyl acetate.
Background technology
In esterification process production ethyl acetate technology, acetate and ethanol react the ethyl acetate that generates and carry water and the part material ethanol that generates simultaneously in esterifying kettle, be raised to the esterification cat head with ternary azeotrope in form, after condensation, mixed solution is through the phase splitter layering, lower floor obtains the bigger water of density, the upper strata obtains the less ethyl acetate phase of density, the gained ester is thick ester work in-process mutually, wherein part is delivered to the back operation and is carried out rectifying and make the finished product ethyl acetate, and another part need be delivered to the esterification column trim the top of column.Lower layer of water is sent into sewage recovering system.
Since the moisture content less than 9% during ethyl acetate, ethanol, water ternary azeotrope are formed, and in the ethyl acetate and water of the chemistry amount that acetate and ethanol synthesis produced, the content of moisture is about 17%.So in the esterification technique, reflux operation is set, the moisture in the system is constantly taken out of by ternary azeotrope.
Above-mentioned phase splitter phase process, it is the process of a free setting, utilize water, the immiscible characteristic of ester, ester, water that density is different carry out roughing out, because of production process is a successive processes, settling time can not sufficiently long, and the gained ester is not thorough with aqueous phase separation, and the middle mutually more water of ester that causes refluxing is carried and entered esterification column.
According to the esterification principle, by product is a water in the esterification reaction process, carry out to positive dirction in order to promote reaction, need in time the water sepn in the esterification products to be gone out, to improve reaction conversion ratio, reduce the ethanol content in the overhead product, reduce the internal circulating load of unreacted material in system, thereby shorten the reaction times, cut down the consumption of energy.
In the prior art, ethyl acetate that esterification generates and water and part material ethanol adopt single phase splitter sedimentation layering, and ester, water sepn are not thorough, contain more water in the ester layer, contain more product ester and feed ethanol in the water layer, cause occurring following problem:
1. contain more water in the ester layer, speed of response is slow, and feed stock conversion reduces.
2. contain more product ester and feed ethanol in the water layer, waste product and raw material, the cost of increase water treatment system.
3. be forced to increase reflux ratio, cause reaction product to be heated repeatedly, system's heat energy consumption increases, and the throughput of esterification equipment is difficult to improve.
4. by product increases, and influences product purity.
Summary of the invention
The objective of the invention is to avoid above-mentioned weak point of the prior art, a kind of speed of response is fast, feed stock conversion is high and provide, economize in raw materials, reduce the water treatment system cost, save energy, raising ethyl acetate plant capacity reduce by product, the ester that improves product purity, water sepn method for synthetizing ethyl acetate by esterification reinforcement more completely phase-splitting production equipment.
Purpose of the present invention can reach by following measure:
Method for synthetizing ethyl acetate by esterification of the present invention is strengthened the phase-splitting production equipment, comprise the esterifying kettle 1, reboiler 2, esterification column 3, condenser A 4, condenser B 5 phase splitters 6 and the recycle pump 7 that are linked in sequence by pipeline and pipe fitting, it is characterized in that at recycle pump 7 outlet lines to the reflux pipeline of esterification column 3, increase at least one fibre bed and strengthen phase splitter 8; Described fibre bed is strengthened phase splitter 8 top exits and is connected by the refluxing opening of reflux pipeline with esterification column 3, and its outlet at bottom is connected with phase splitter discharge of wastewater pipeline 9 by pipeline, and its upper entrance is connected with recycle pump 7 outlet lines by pipeline.
Method for synthetizing ethyl acetate by esterification of the present invention is strengthened the phase-splitting production equipment, by on esterification column trim the top of column pipe, set up fibre bed and strengthen phase splitter (8), ester is separated more completely with water, make the moisture content in refluxing drop to minimum level, thereby improve reaction conversion ratio, reduce pure content in the cat head discharging, reduce the internal circulating load of unreacted material in system, save reaction and separating energy consumption.
Purpose of the present invention can also reach by following measure:
Method for synthetizing ethyl acetate by esterification of the present invention is strengthened the phase-splitting production equipment, and it is corrosion resistant glass fibre or Polymer Synthesizing fiber that described fibre bed is strengthened the filamentary material of loading in the phase splitter 8.
Method for synthetizing ethyl acetate by esterification of the present invention is strengthened the phase-splitting production equipment, and the filamentary materials of loading in the described fibre bed reinforcement phase splitter 8 are the sheet section bars with corrosion resistant glass fibre or the moulding of Polymer Synthesizing fiber weaving.
Method for synthetizing ethyl acetate by esterification of the present invention is strengthened the phase-splitting production equipment, it is characterized in that the number of the fibre bed reinforcement phase splitter 8 of described increase is 1～3, and use is connected in parallel to each other or is installed in series.
Method for synthetizing ethyl acetate by esterification of the present invention is strengthened the application of phase-splitting production equipment, it is characterized in that being adapted to organic acid and reacts all esterification production equipments of producing ester and water with alcohol.
Method for synthetizing ethyl acetate by esterification of the present invention is strengthened the disclosed technical scheme of phase-splitting production equipment following positively effect compared to existing technology:
1. provide that a kind of speed of response is fast, feed stock conversion is high, economize in raw materials, reduce the water treatment system cost, save energy, raising ethyl acetate plant capacity reduce by product, the ester that improves product purity, water sepn method for synthetizing ethyl acetate by esterification reinforcement more completely phase-splitting production equipment.
2. solved because of containing more water in the ester layer, speed of response is slow, the problem that feed stock conversion reduces, and the production cycle of producing a collection of ethyl acetate shortened to 3 hours by original 6 hours; Bring up to 99.95% in the feed stock conversion of raw acetic acid by original 98%.
2. solved because of containing more product ester and feed ethanol in the water layer, waste product and raw material, the problem of the cost of increase water treatment system.
3. solved and be forced to increase reflux ratio, caused reaction product to be heated repeatedly, system's heat energy consumption increases, the problem that the throughput of esterification equipment is difficult to improve.Reflux ratio drops to 2 by original 4.
4. by product reduces, and the content of product ethyl acetate reaches 95wt%.
Description of drawings
Fig. 1 is that method for synthetizing ethyl acetate by esterification of the present invention is strengthened phase-splitting production equipment synoptic diagram
Fig. 2 is a method for synthetizing ethyl acetate by esterification production equipment synoptic diagram of the prior art
Among the figure
The 1-esterifying kettle
The 2-reboiler
The 3-esterification column
4-condenser A
5-condenser B
The 6-phase splitter
The 7-recycle pump
The 8-fibre bed is strengthened phase splitter
9-phase splitter discharge of wastewater pipeline
Embodiment
The present invention will now be further detailed embodiment:
Embodiment 1
A kind of method for synthetizing ethyl acetate by esterification is strengthened the phase-splitting production equipment, comprise the esterifying kettle 1, reboiler 2, esterification column 3, condenser A 4, condenser B 5 phase splitters 6 and the recycle pump 7 that are linked in sequence by pipeline and pipe fitting, it is characterized in that at recycle pump 7 outlet lines to the reflux pipeline of esterification column 3, increase at least one fibre bed and strengthen phase splitter 8; Described fibre bed is strengthened phase splitter 8 top exits and is connected by the refluxing opening of reflux pipeline with esterification column 3, and its outlet at bottom is connected with phase splitter discharge of wastewater pipeline 9 by pipeline, and its upper entrance is connected with recycle pump 7 outlet lines by pipeline.
It is corrosion resistant glass fibre that described fibre bed is strengthened the filamentary material of loading in the phase splitter 8.
The number that the fibre bed of described increase is strengthened phase splitter 8 is 2, and use is connected in parallel to each other or is installed in series.
Produce 3 hours production cycles of a collection of ethyl acetate; Feed stock conversion 99.95% in raw acetic acid.Reflux ratio 2, ethyl acetate content 95wt%.
According to the production equipment of embodiment 1, difference is that it is the sheet section bar that adopts the moulding of Polymer Synthesizing fiber weaving that described fibre bed is strengthened the filamentary material of loading in the phase splitter 8, and the number that the fibre bed of described increase is strengthened phase splitter 8 is one.
Produce 2 hours production cycles of a collection of ethyl acetate; Feed stock conversion 99.95% in raw acetic acid.Reflux ratio 2, ethyl acetate content 95wt%.
Claims (5)
1. a method for synthetizing ethyl acetate by esterification is strengthened the phase-splitting production equipment, comprise the esterifying kettle (1), reboiler (2), esterification column (3), condenser A (4), condenser B (5) phase splitter (6) and the recycle pump (7) that are linked in sequence by pipeline and pipe fitting, it is characterized in that at recycle pump (7) outlet line to the reflux pipeline of esterification column (3), increase at least one fibre bed and strengthen phase splitter (8); Described fibre bed is strengthened phase splitter (8) top exit and is connected by the refluxing opening of reflux pipeline with esterification column (3), its outlet at bottom is connected with phase splitter discharge of wastewater pipeline (9) by pipeline, and its upper entrance is connected with recycle pump (7) outlet line by pipeline.
2. strengthen the phase-splitting production equipment according to the method for synthetizing ethyl acetate by esterification of claim 1, it is characterized in that it is corrosion resistant glass fibre or Polymer Synthesizing fiber that described fibre bed is strengthened the filamentary material of loading in the phase splitter (8).
3. strengthen the phase-splitting production equipment according to the method for synthetizing ethyl acetate by esterification of claim 1, it is characterized in that the filamentary material of loading in the described fibre bed reinforcement phase splitter (8) is the sheet section bar with corrosion resistant glass fibre or the moulding of Polymer Synthesizing fiber weaving.
4. strengthen the phase-splitting production equipment according to the method for synthetizing ethyl acetate by esterification of claim 1, it is characterized in that the number of the fibre bed reinforcement phase splitter (8) of described increase is 1～3, use is connected in parallel to each other or is installed in series.
5. the method for synthetizing ethyl acetate by esterification of claim 1 is strengthened the application of phase-splitting production equipment, it is characterized in that being adapted to organic acid and reacts all esterification production equipments of producing ester and water with alcohol.
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| CN2011101789285A CN102285879B (en) | 2011-06-29 | 2011-06-29 | Reinforced phase splitting production device for synthesizing ethyl acetate by esterification process |
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| CN2011101789285A CN102285879B (en) | 2011-06-29 | 2011-06-29 | Reinforced phase splitting production device for synthesizing ethyl acetate by esterification process |
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| CN102285879A true CN102285879A (en) | 2011-12-21 |
| CN102285879B CN102285879B (en) | 2013-07-17 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105622405A (en) * | 2016-02-29 | 2016-06-01 | 薛晶 | Ethyl acetate production device |
| CN105712873A (en) * | 2016-01-04 | 2016-06-29 | 金沂蒙集团有限公司 | Control method for synthesizing ethyl acetate by using esterification method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1526692A (en) * | 2003-09-22 | 2004-09-08 | ����ʦ����ѧ | Composite extracting and rectifying separation process of ethyl acetate |
| CN201175593Y (en) * | 2008-04-18 | 2009-01-07 | 上海安赐机械设备有限公司 | Wild-phase separator |
| CN101830799A (en) * | 2010-05-25 | 2010-09-15 | 张超 | Single-tower rectifying method for synthetizing ethyl acetate by esterification method |
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2011
- 2011-06-29 CN CN2011101789285A patent/CN102285879B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1526692A (en) * | 2003-09-22 | 2004-09-08 | ����ʦ����ѧ | Composite extracting and rectifying separation process of ethyl acetate |
| CN201175593Y (en) * | 2008-04-18 | 2009-01-07 | 上海安赐机械设备有限公司 | Wild-phase separator |
| CN101830799A (en) * | 2010-05-25 | 2010-09-15 | 张超 | Single-tower rectifying method for synthetizing ethyl acetate by esterification method |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105712873A (en) * | 2016-01-04 | 2016-06-29 | 金沂蒙集团有限公司 | Control method for synthesizing ethyl acetate by using esterification method |
| CN105712873B (en) * | 2016-01-04 | 2019-02-22 | 金沂蒙集团有限公司 | The control method of method for synthetizing ethyl acetate by esterification |
| CN105622405A (en) * | 2016-02-29 | 2016-06-01 | 薛晶 | Ethyl acetate production device |
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| CN102285879B (en) | 2013-07-17 |
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Owner name: LINYI GOLDEN YIMENG BIOTECHNOLOGY CO., LTD. Free format text: FORMER OWNER: ZHANG CHAO Effective date: 20120320 |
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Effective date of registration: 20120320 Address after: 276700 No. 99 Da Xing West Street, Linshu County, Shandong, Linyi Applicant after: Linyi Jinximeng Biological Technology Co., Ltd. Address before: 276700 No. 99 Da Xing West Street, Linshu County, Shandong, Linyi Applicant before: Zhang Chao |
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