CN102070445B - Purification method of ethyl acetate - Google Patents
Purification method of ethyl acetate Download PDFInfo
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- CN102070445B CN102070445B CN2011100058719A CN201110005871A CN102070445B CN 102070445 B CN102070445 B CN 102070445B CN 2011100058719 A CN2011100058719 A CN 2011100058719A CN 201110005871 A CN201110005871 A CN 201110005871A CN 102070445 B CN102070445 B CN 102070445B
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- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 title claims abstract description 527
- 238000000746 purification Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title abstract description 48
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 125
- 238000011084 recovery Methods 0.000 claims abstract description 76
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000000203 mixture Substances 0.000 claims abstract description 33
- 238000005265 energy consumption Methods 0.000 claims abstract description 15
- 239000002351 wastewater Substances 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000000895 extractive distillation Methods 0.000 claims abstract description 3
- 241000282326 Felis catus Species 0.000 claims description 59
- 235000019441 ethanol Nutrition 0.000 claims description 37
- 239000007792 gaseous phase Substances 0.000 claims description 37
- 239000012071 phase Substances 0.000 claims description 37
- 238000000605 extraction Methods 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 15
- 150000002148 esters Chemical class 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 8
- 238000003672 processing method Methods 0.000 claims description 8
- 238000009833 condensation Methods 0.000 claims description 6
- 230000005494 condensation Effects 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 4
- 239000002699 waste material Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- 238000007670 refining Methods 0.000 abstract description 3
- FMYHFHVAPZDDPJ-UHFFFAOYSA-N ethanol;ethyl acetate;hydrate Chemical compound O.CCO.CCOC(C)=O FMYHFHVAPZDDPJ-UHFFFAOYSA-N 0.000 abstract 1
- 230000010354 integration Effects 0.000 abstract 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 14
- 235000011941 Tilia x europaea Nutrition 0.000 description 14
- 239000004571 lime Substances 0.000 description 14
- 230000032050 esterification Effects 0.000 description 6
- 238000005886 esterification reaction Methods 0.000 description 6
- 238000005191 phase separation Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- 238000007599 discharging Methods 0.000 description 3
- 239000004149 tartrazine Substances 0.000 description 3
- 239000004229 Alkannin Substances 0.000 description 2
- 239000004231 Riboflavin-5-Sodium Phosphate Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002151 riboflavin Substances 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- 239000004230 Fast Yellow AB Substances 0.000 description 1
- 239000004234 Yellow 2G Substances 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 239000012809 cooling fluid Substances 0.000 description 1
- 235000019628 coolness Nutrition 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- MHYCRLGKOZWVEF-UHFFFAOYSA-N ethyl acetate;hydrate Chemical compound O.CCOC(C)=O MHYCRLGKOZWVEF-UHFFFAOYSA-N 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a purification method of ethyl acetate. The method comprises the following step: the ethyl acetate product is purified from ethyl acetate-ethanol-water mixture. The equipment of the method at least contains an ethyl acetate rectifying tower, an ethyl acetate recovery tower, an ethanol recovery tower and the associated equipment. The purification method is as follows: heat integration is realized between the ethyl acetate rectifying tower and the ethyl acetate recovery tower; the ethyl acetate product is obtained from the bottom of the ethyl acetate rectifying tower, wherein the ethyl acetate recovery tower uses water as extracting agent to perform extractive distillation operation; ethyl acetate is recycled from the tower top; ethanol-water mixture is discharged from the tower bottom and sent to the ethanol recovery tower; and ethanol-water mixture is obtained from the bottom of the ethanol recovery tower, a part of wastewater in the tower bottom is recycled, and the other part is discharged from the equipment. The operational energy consumption can be greatly reduced by adopting heat exchange and energy saving methods in the system. By adopting the method of the invention, the operational energy consumption can be reduced to 0.55 ton of steam for 1 ton of the ethyl acetate product, which can be reduced by more than 50% compared with the existing ethyl acetate refining method; the reaction process of returning ethyl acetate is not required, than the reaction process energy consumption can be reduced by more than 30%.
Description
Technical field
The present invention relates to a kind of purification process of ethyl acetate, this processing method is from the energy-saving process method of thick ester raw material (mixture of ethyl acetate, alcohol and water) by rectifying production ethyl acetate.
Background technology
The ethyl acetate process for purification (Fig. 1) that adopts at present extensively is that to react thick ester (mixture of ethyl acetate, alcohol and water) be raw material, reacts the oil phase that thick ester leaves standstill after the phase-splitting and advances the ethyl acetate treating tower, and the treating tower tower reactor obtains ethyl acetate product.The mixture for the treatment of tower overhead extraction ethyl acetate, alcohol and water, after the cooling phase-splitting, an oil phase part is returned the treating tower cat head as backflow, and extraction is back to the esterification operation to another part as hair oil.Phase-splitting gained water advances water vaporization tower, reclaims wherein ethyl acetate and ethanol.Its greatest drawback is that a large amount of ethyl acetate (account for treating tower tower reactor ethyl acetate amount 50%) circulate between treating tower and reaction process; Secondly, yield of aforesaid method ethyl acetate is low, and operation energy consumption is high.Comparatively advanced ethyl acetate treating process energy consumption is about 1.2 tons of steam/ton ethyl acetate product at present.
Summary of the invention
The purification process that the purpose of this invention is to provide a kind of ethyl acetate, this processing method is that purifying obtains ethyl acetate product from thick ester raw material (mixture of ethyl acetate, alcohol and water), overcome the shortcoming of prior art, on conventional ethyl acetate rectification process basis, differential pressure heat is integrated and extraction and distillation technology is applied in the ethyl acetate rectifying breakthroughly, significantly reduces operation energy consumption.Processing method provided by the invention has significant practicality and economic benefit.
The purification process of a kind of ethyl acetate provided by the invention is that purifying obtains ethyl acetate product from thick ester raw material (mixture of ethyl acetate, alcohol and water), it is characterized in that:
1) comprises at least ethyl acetate rectifying tower T101, ethanol recovery tower T102 and ethyl acetate recovery tower T103;
2) hot integrated operation between said ethyl acetate rectifying tower, the ethyl acetate recovery tower, ethyl acetate rectifying tower top gaseous phase are as ethyl acetate recovery tower tower reactor heat source, for the ethyl acetate recovery tower provides institute's heat requirement; Perhaps ethyl acetate recovery tower top gaseous phase is as ethyl acetate tower bottom of rectifying tower heat source, for the ethyl acetate rectifying tower provides institute's heat requirement;
3) said ethyl acetate rectifying tower cat head distillates the mixture of ethyl acetate, alcohol and water, and tower reactor obtains ethyl acetate product;
4) said ethyl acetate recovery tower is extractive distillation column, and employing water is extraction agent, and water adds between cat head or cat head and charging, and cat head distillates the mixture of ethyl acetate and water, and tower reactor is discharged the mixture of second alcohol and water;
5) said ethanol recovery tower is used for reclaiming the ethanol of ethyl acetate recovery tower tower reactor material, ethanol recovery tower overhead extraction ethanol-water mixture, tower reactor waste discharge.The waste water that tower reactor is discharged is after cooling, and a part recycles as extraction agent, and another part goes out device.
The charging of the said ethyl acetate recovery tower of the present invention is the mixture that ethyl acetate rectifying tower cat head distillates ethyl acetate, alcohol and water.
The present invention can add washing water in the raw material (mixture of ethyl acetate, alcohol and water) to promote the raw material phase-splitting, with the part alcohol extraction in the raw material to aqueous phase, thereby the difficulty of separating alcohol in the reduction ethyl acetate treating process.Washing water 19 can enter phase separation tank V100 first again after the thick ester 12 of raw material mixes, also can enter respectively V100 and then mix phase-splitting.Phase separation tank V100 can also be designed to vertical structure, washing water 19 are downward by top, the thick ester 12 of raw material is contacted by the bottom upruss, to reach the purpose of abundant washing.
The water that the said raw material of the present invention (mixture of ethyl acetate, alcohol and water) leaves standstill after the phase-splitting also enters ethyl acetate recovery tower middle part or bottom, reclaims ethyl acetate wherein.
The said ethyl acetate recovery tower of the present invention cat head is established condenser and phase splitter, and ethyl acetate recovery tower cat head distillates gas phase after condensation, phase-splitting, and an oil phase part is back to ethyl acetate recovery tower cat head as backflow, also can not reflux; Another part oil phase is back to the charging of ethyl acetate rectifying tower; Water after the phase-splitting returns the ethyl acetate recovery tower.When ethyl acetate recovery tower cat head oil phase did not reflux, extraction water was fed to ethyl acetate recovery tower cat head, and perhaps ethyl acetate recovery tower cat head water is fed to ethyl acetate recovery tower cat head.
Ethanol recovery tower cat head of the present invention obtains ethanol-water mixture; The waste water that tower reactor is discharged is after cooling, and a part recycles as extraction agent, and another part goes out device.
The said ethanol recovery tower of the present invention top gaseous phase can adopt circulating water; Perhaps ethanol recovery tower top gaseous phase is as ethyl acetate tower bottom of rectifying tower heat source; Perhaps ethanol recovery tower top gaseous phase is as ethyl acetate recovery tower heat source; Perhaps be used for other cryogens in the heating system, to reduce operation energy consumption.
Operational condition of the present invention be the ethyl acetate rectifying tower top gaseous phase as ethyl acetate recovery tower tower reactor heat source, the cat head working pressure of ethyl acetate rectifying tower is 90～900kPa; The cat head working pressure of ethyl acetate recovery tower is 30～400kPa; The cat head working pressure of ethanol recovery tower is 90～1200kPa.Except specified otherwise, all pressure all refer to absolute pressure among the present invention.
A kind of typical operational condition of the present invention is: ethyl acetate recovery tower top gaseous phase is as ethyl acetate tower bottom of rectifying tower heat source, and the cat head working pressure of ethyl acetate rectifying tower is 30～400kPa; The cat head working pressure of ethyl acetate recovery tower is 90～900kPa; The cat head working pressure of ethanol recovery tower is 90～1200kPa.
The said ethanol recovery tower of the present invention top gaseous phase can adopt circulating water; Perhaps ethanol recovery tower top gaseous phase is as ethyl acetate tower bottom of rectifying tower heat source; Perhaps ethanol recovery tower top gaseous phase is as ethyl acetate recovery tower heat source; Perhaps be used for other cryogens in the heating system, to reduce operation energy consumption.For example: ethanol recovery tower top gaseous phase is used for adding the charging of hot ethyl acetate rectifying tower; Ethanol recovery tower top gaseous phase is used for adding hot ethyl acetate recovery tower phegma, and ethanol recovery tower top gaseous phase is as esterification operation esterification column heat source.
Processing method provided by the invention, recovered energy, reduce steam consumption, the energy-saving process method that reduces recirculated water consumption includes but not limited to following methods, the energy-saving process method that adopts can be following whole or their various possible combination:
(1) ethyl acetate product 2 is given T101 charging 20 preheatings.
(2) ethyl acetate product 2 is given T102 charging 30 preheatings.
(3) ethyl acetate product 2 is given 26 preheatings of phase splitter V101 oil phase.
(4) ethyl acetate product 2 is given 29 preheatings of phase splitter V101 water.
(5) ethyl acetate product 2 is given 27 preheatings of T103 phegma.
(6) T102 still liquid 35 is given T101 charging 20 preheatings.
(7) T102 still liquid 35 is given 26 preheatings of phase splitter V101 oil phase.
(8) T102 still liquid 35 is given 29 preheatings of phase splitter V101 water.
(9) T102 still liquid 35 is given 27 preheatings of T103 phegma.
(10) T102 still liquid 35 is given T102 charging 30 preheatings.
(11) T103 top gaseous phase 23 is given T101 charging 20 preheatings.
(12) T103 top gaseous phase 23 is given 26 preheatings of phase splitter V101 oil phase.
(13) T103 top gaseous phase 23 is given 29 preheatings of phase splitter V101 water.
(14) T103 top gaseous phase 23 is given 27 preheatings of T103 phegma.
(15) T102 top gaseous phase 31 is given the heating of T101 tower reactor.
(16) T102 top gaseous phase 31 is given the heating of T103 tower reactor.
(17) T102 top gaseous phase 31 is given T101 charging 20 preheatings.
(18) T102 top gaseous phase 31 is given 26 preheatings of phase splitter V101 oil phase.
(19) T102 top gaseous phase 31 is given 29 preheatings of phase splitter V101 water.
(20) T102 top gaseous phase 31 is given 27 preheatings of T103 phegma.
(21) heating steam lime set is to T101 charging 20 preheatings.
(22) heating steam lime set is to T102 charging 30 preheatings.
(23) heating steam lime set is to T103 charging 22 preheatings.
(24) heating steam lime set is to 26 preheatings of V101 oil phase.
(25) heating steam lime set is to 27 preheatings of T103 phegma.
(26) lime set 24 of T103 top gaseous phase 23 is given 26 preheatings of V101 oil phase.
(27) lime set 24 of T103 top gaseous phase 23 is given 27 preheatings of T103 phegma.
The present invention has overcome the shortcoming of prior art, with respect to thick ester raw material, and processing method provided by the invention, yield of ethyl acetate treating process is almost 100%, has avoided a large amount of ethyl acetate at system's internal recycle.Because the application of differential pressure heat integrated technique and extraction rectification technique, processing method provided by the invention is down to 0.55 ton of steam/ton ethyl acetate product with ethyl acetate treating process operation energy consumption, and advanced ethyl acetate process for purification reduces operation energy consumption more than 50% at present.Add without ethyl acetate and return reaction process, can make the reaction process Energy Intensity Reduction more than 30%.Therefore, Refine Process for Ethyl Acetate method provided by the invention has significant practicality and economic benefit.
Description of drawings
Fig. 1 is the Refine Process for Ethyl Acetate method flow diagram that prior art adopts.
Fig. 2 is a kind of Refine Process for Ethyl Acetate method provided by the invention, and T101 and T102 cat head material steam are respectively as T103 tower reactor reboiler heat source.
Fig. 3 is a kind of Refine Process for Ethyl Acetate method provided by the invention, and T101 cat head material steam is as T103 tower reactor reboiler heat source.T102 cat head material steam is as reaction process esterification column heat source.
Embodiment
Specific embodiments of the present invention is described in detail as follows with reference to accompanying drawing, but for illustrative purposes only rather than the restriction the present invention.
As shown in Figure 1, what prior art adopted is to leave standstill phase-splitting with thick ester (mixture of ethyl acetate, alcohol and water) raw material 12 in phase separation tank V100, and oil phase 1 advances ethyl acetate treating tower C101, and the C101 tower reactor obtains ethyl acetate product 2.C101 top gaseous phase 3 is through condenser E102 condensation, and lime set 4 is cooled off laggard phase separation tank V101 through E103.V101 oil phase 6 is divided into two strands, and one oil phase returns the C101 cat head as C101 phegma 7, and another strand oil phase is as hair oil 8 extraction, and hair oil 8 is back to the esterification operation.V100 water 13 and V101 water 9 all enter water vaporization tower C102, and C102 top gaseous phase 10 also advances the E102 condensation.C102 tower reactor waste discharge 11.
The greatest drawback of this common process method is that a large amount of ethyl acetate (account for treating tower tower reactor ethyl acetate amount 50%) circulate between treating tower and reaction process; Cause yield of ethyl acetate very low, operation energy consumption is high.By processing method shown in Figure 1, comparatively advanced ethyl acetate treating process energy consumption is about 1.2 tons of steam/ton ethyl acetate product at present.
The present invention such as Fig. 2, shown in Figure 3, the purification process that the invention provides a kind of ethyl acetate is that purifying obtains ethyl acetate product from thick ester raw material (mixture of ethyl acetate, alcohol and water).Whole ethyl acetate refining system comprises that at least ethyl acetate rectifying tower T101, ethanol recovery tower T102 and ethyl acetate recovery tower T103 and support equipment thereof form.The integrated operation of differential pressure heat obtains ethyl acetate product by the ethyl acetate tower bottom of rectifying tower between T101, the T103.The method of the integrated operation of differential pressure heat can be that T101 cat head material steam 3 is to T103 tower reactor reboiler E106 heating between T101, the T103; Or T103 cat head material steam 23 is given T101 tower reactor reboiler E101 heating.Two towers of T101 and T103 only have a tower wherein to need the external steam heating, and another tower does not need to input outer for steam, effectively reduces operation energy consumption.
Water of the present invention is as extraction agent, adopts the method for extracting rectifying to separate the mixture of the ethyl acetate, alcohol and water that the T101 cat head distillates at the T103 tower.Because the extraction of water, the ethanol that polarity is stronger is extracted to the T103 tower reactor by water, and the T103 cat head distillates the mixture 23 of ethyl acetate-water, only contains micro ethanol.The laggard phase splitter V101 of 23 phlegmas, 24 coolings, a part of oil phase 27 refluxes as T103 and returns the T103 cat head, also can not return; All the other oil phase 28 extraction are also returned the T101 tower.The isolated water 29 of V101 enters T103 top or top.T103 tower tower reactor is discharged the mixture of alcohol-water, only contains the micro-acetic acid ethyl ester, removes the T102 tower.The extraction of T102 column overhead is ethanol, water mixture, contains the micro-acetic acid ethyl ester.The T102 tower reactor is waste water 35, and a part of waste water 36 returns T103 and recycles as extraction agent after heat exchange, cooling, and another part waste water 37 goes out device.
The invention provides a kind of Refine Process for Ethyl Acetate method is described in detail as follows:
Application Example 1
Fig. 2, T101 and T102 cat head material steam are respectively as T103 tower reactor reboiler heat source.
The first tower is ethyl acetate rectifying tower T101, and the second tower is that ethanol recovery tower T102, the 3rd tower are ethyl acetate recovery tower T103.
Add washing water 19 in thick ester (mixture of the ethyl acetate, alcohol and water) raw material 12, enter after the mixing among the phase separation tank V100 and leave standstill phase-splitting, oil phase 1 (or respectively) after mixing from T103 cat head oil phase discharging 28 enters the T101 middle part.The T101 tower reactor is by reboiler E101 steam heating, and the T101 tower reactor obtains ethyl acetate product 2.T101 top gaseous phase 3 is through hot integrated heat exchanger E106 condensation, and lime set 4 is through advancing return tank V103.Lime set 4 is divided into two strands, and a part is returned the T101 cat head as T101 phegma 21, and the T103 middle part is gone in another burst 22 extraction.
T103 top gaseous phase 23 is through condenser E102 condensation, and lime set 24 is through the E103 cooling, and lime set cooling fluid 25 is advanced phase separation tank V101 phase-splitting, oil phase 26 is divided into two strands, one oil phase returns the T103 cat head as T103 phegma 27, and another strand oil phase 28 is as the discharging of T103 cat head, and the T101 charging is returned in logistics 28.V100 water 13 enters T103 tower bottom or middle part.V101 water 29 enters T103 tower top or top.The T102 middle part is entered in T103 tower reactor discharging 30.
T102 top gaseous phase 31 is also given the heating of T103 tower reactor by hot integrated heat exchanger E105, and logistics 31 lime sets 32 are advanced return tank V102.Lime set 32 is divided into two strands, and a part is returned the T102 cat head as T102 phegma 33, and another strand 34 is Recycled ethanol.The T102 tower bottoms is waste water 35, and logistics 35 is divided into two strands, one waste water 36 through enter the T103 top of tower after the water cooler E107 cooling as cycling extraction agent 38 or enter the T103 cat head and logistics 22 feed entrance points between; Another strand waste water 37 goes out device.
Below provided a kind of typical operation conditions of embodiment 1 each major equipment:
T101 cat head working pressure 500kPa, the cat head service temperature is 121 ℃, 139 ℃ of tower reactor service temperatures.
T102 cat head working pressure 400kPa, 119 ℃ of cat head service temperatures, 146 ℃ of tower reactor service temperatures.
T103 cat head working pressure is normal pressure, 84 ℃ of cat head service temperatures, 98 ℃ of tower reactor service temperatures.
The V100 working pressure is normal pressure, 38 ℃ of service temperatures.
The V101 working pressure is normal pressure, 38 ℃ of service temperatures.
Application Example 2:
The invention provides a kind of Refine Process for Ethyl Acetate method, T101 cat head material steam is as T103 tower reactor reboiler heat source.T102 cat head material steam is as reaction process esterification column heat source (Fig. 3).
The typical operation conditions of embodiment 2 each major equipment is identical with embodiment 1.
Adopt ethyl acetate purification process provided by the invention and extensively adopt at present the contrast of two tower Refine Process for Ethyl Acetate operation energy consumptions as follows:
The routine two tower Refine Process for Ethyl Acetate that extensively adopt at present, the steam consumption quantity of production ethyl acetate is 1.2 tons of steam/ton ethyl acetate product approximately.
Adopt ethyl acetate purification process provided by the invention, steam consumption quantity is 0.55 ton of steam/ton ethyl acetate product approximately.
Adopt ethyl acetate purification process provided by the invention and the routine two tower Refine Process for Ethyl Acetate methods contrast of extensively adopting at present, calculate (ethyl acetate output is 12.5 tons/hour, and year operation hours was by 8000 hours) by 100,000 ton/years of Ethyl Acetate Plants:
Ethyl acetate treating process Energy Intensity Reduction
(1.2-0.55)/1.2×100％≈54％。
Can save steam every year
(1.2-0.55) ton/ton x10 is ten thousand ton/years=0.65 ton/ton * 100,000 ton/years=6.5 ten thousand ton/years
By 150 yuan of calculating of steam per ton, can save the steam expense every year:
6.5 ten thousand ton/years * 150 yuan/tons=9,750,000 yuan/year.
Above-mentioned cost saving does not also count the Energy Intensity Reduction benefit of bringing in the circulation of reaction process and refining step because reducing a large amount of ethyl acetate.If count above-mentioned Energy Intensity Reduction economic benefit, annual energy-saving benefit will reach more than 1,500 ten thousand yuan.
The invention provides a kind of purification process of ethyl acetate, have extremely distinct economic.Specified in conjunction with the embodiments, the personnel of association area fully can suitably change or change and make up according to the method that this patent provides, and realize the art of this patent.Of particular note, all these carry out similar change or change and combination by the technical process that this patent is provided, and are apparent to those skilled in the art, all are regarded as in spirit of the present invention, scope and content.
Claims (9)
1. the purification process of an ethyl acetate, this processing method be thick ester take the mixture of ethyl acetate, alcohol and water as feed purification obtains ethyl acetate product, it is characterized in that:
1) comprises at least ethyl acetate rectifying tower (T101), ethanol recovery tower (T102) and ethyl acetate recovery tower (T103);
2) hot integrated operation between said ethyl acetate rectifying tower, the ethyl acetate recovery tower, ethyl acetate rectifying tower top gaseous phase are as ethyl acetate recovery tower tower reactor heat source, for the ethyl acetate recovery tower provides institute's heat requirement; Perhaps ethyl acetate recovery tower top gaseous phase is as ethyl acetate tower bottom of rectifying tower heat source, for the ethyl acetate rectifying tower provides institute's heat requirement;
3) said ethyl acetate rectifying tower cat head distillates the mixture of ethyl acetate, alcohol and water, and tower reactor obtains ethyl acetate product;
4) said ethyl acetate recovery tower is extractive distillation column, and employing water is extraction agent, and water adds between cat head or cat head and feed entrance point, and cat head distillates the mixture of ethyl acetate and water, and tower reactor is got rid of the mixture of second alcohol and water;
5) said ethanol recovery tower is used for reclaiming the ethanol of ethyl acetate recovery tower tower reactor material, ethanol recovery tower overhead extraction ethanol-water mixture, tower reactor waste discharge.
2. according to the said purification process of claim 1, it is characterized in that the charging of said ethyl acetate recovery tower is the mixture that ethyl acetate rectifying tower cat head distillates ethyl acetate, alcohol and water.
3. according to the said purification process of claim 1, it is characterized in that in the mixture of raw acetic acid ethyl ester-alcohol-water, adding washing water to promote the raw material phase-splitting.
4. according to the said purification process of claim 1, the water that the mixture that it is characterized in that said raw acetic acid ethyl ester-alcohol-water leaves standstill after the phase-splitting also enters the ethyl acetate recovery tower, reclaims ethyl acetate wherein.
5. according to the said purification process of claim 1, it is characterized in that said ethyl acetate recovery tower cat head establishes condenser and phase splitter, ethyl acetate recovery tower cat head distillates gas phase after condensation, phase-splitting, and an oil phase part is back to ethyl acetate recovery tower cat head as backflow, or does not reflux; Another part oil phase is back to the charging of ethyl acetate rectifying tower; Water after the phase-splitting returns the ethyl acetate recovery tower.
6. according to the said purification process of claim 1, it is characterized in that ethanol recovery tower cat head obtains ethanol-water mixture; The waste water that tower reactor is discharged is after cooling, and a part recycles as extraction agent, and another part goes out device.
7. according to the said purification process of claim 1, it is characterized in that said ethanol recovery tower top gaseous phase adopts circulating water; Perhaps ethanol recovery tower top gaseous phase is as ethyl acetate tower bottom of rectifying tower heat source; Perhaps ethanol recovery tower top gaseous phase is as ethyl acetate recovery tower heat source; Perhaps be used for other cryogens in the heating system, to reduce operation energy consumption.
8. according to the said purification process of claim 1, it is characterized in that operational condition is: the ethyl acetate rectifying tower top gaseous phase is as ethyl acetate recovery tower tower reactor heat source, and the cat head working pressure of ethyl acetate rectifying tower is 90～900kPa; The cat head working pressure of ethyl acetate recovery tower is 30～400kPa; The cat head working pressure of ethanol recovery tower is 90～1200kPa.
9. according to the said purification process of claim 1, it is characterized in that operational condition is; Ethyl acetate recovery tower top gaseous phase is as ethyl acetate tower bottom of rectifying tower heat source, and the cat head working pressure of ethyl acetate rectifying tower is 30～400kPa; The cat head working pressure of ethyl acetate recovery tower is 90～900kPa; The cat head working pressure of ethanol recovery tower is 90～1200kPa.
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| CN110743276A (en) * | 2019-12-20 | 2020-02-04 | 山东万圣博化工有限公司 | Adhesive industrial waste gas treatment method |
| CN112409172B (en) * | 2020-11-19 | 2023-04-07 | 江门谦信化工发展有限公司 | Method and system for producing ethyl acetate |
| CN115490594B (en) * | 2022-08-29 | 2023-09-26 | 泰兴金江化学工业有限公司 | Purification equipment and purification method of high-purity ethyl acetate |
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| CN1526692A (en) * | 2003-09-22 | 2004-09-08 | ����ʦ����ѧ | Composite extracting and rectifying separation process of ethyl acetate |
| CN101486642A (en) * | 2009-02-16 | 2009-07-22 | 江门天诚溶剂制品有限公司 | Heat pump production method of ethyl acetate and production apparatus thereof |
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| CN1526692A (en) * | 2003-09-22 | 2004-09-08 | ����ʦ����ѧ | Composite extracting and rectifying separation process of ethyl acetate |
| CN101486642A (en) * | 2009-02-16 | 2009-07-22 | 江门天诚溶剂制品有限公司 | Heat pump production method of ethyl acetate and production apparatus thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106699560A (en) * | 2015-11-18 | 2017-05-24 | 上海浦景化工技术股份有限公司 | Separation device and separation method of material flow containing methyl methacrylate |
| CN106699560B (en) * | 2015-11-18 | 2020-08-14 | 上海浦景化工技术股份有限公司 | Separation equipment and separation method for methyl methacrylate-containing material flow |
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| CN102070445A (en) | 2011-05-25 |
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