Method for synthetizing ethyl acetate by esterification is strengthened the phase-splitting production equipment
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, acetic acid 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.
Because 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 acetic acid and ethanol synthesis produce, the content of moisture is about 17%.So in the esterification technique, reflux operation is set, by ternary azeotrope the moisture in the system is constantly taken out of.
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 production process is a successive processes, settling time can not sufficiently long, and the gained ester is not thorough with aqueous phase separation, cause the ester that refluxes mutually middle more water carry and enter esterification column.
According to the esterification principle, by product is 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, the 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.
The utility model content
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 A4, condenser B5 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 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 containing more water in the ester layer, speed of response is slow, and the problem that feed stock conversion reduces is produced the production cycle of a collection of ethyl acetate by original 6 hours, shortens to 3 hours; Bring up to 99.95% in the feed stock conversion of raw acetic acid by original 98%.
2. solved because 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 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 A4, condenser B5 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 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%.
Embodiment 2
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%.