CN116459752A - A purification device for ethyl acetate production - Google Patents
A purification device for ethyl acetate production Download PDFInfo
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- CN116459752A CN116459752A CN202310463254.6A CN202310463254A CN116459752A CN 116459752 A CN116459752 A CN 116459752A CN 202310463254 A CN202310463254 A CN 202310463254A CN 116459752 A CN116459752 A CN 116459752A
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- phase
- plate
- phase separation
- ethyl acetate
- funnel
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- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 title claims abstract description 249
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- 238000000746 purification Methods 0.000 title claims abstract description 15
- 238000005191 phase separation Methods 0.000 claims abstract description 106
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 88
- 150000002148 esters Chemical class 0.000 claims abstract description 43
- 238000005452 bending Methods 0.000 claims description 14
- 230000000670 limiting effect Effects 0.000 claims description 10
- 238000007789 sealing Methods 0.000 claims description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical class [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 5
- 238000010030 laminating Methods 0.000 claims description 5
- 230000005540 biological transmission Effects 0.000 claims description 3
- 239000012071 phase Substances 0.000 abstract description 97
- 238000005886 esterification reaction Methods 0.000 abstract description 15
- 230000032050 esterification Effects 0.000 abstract description 13
- 238000004062 sedimentation Methods 0.000 abstract description 11
- 238000010924 continuous production Methods 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 4
- 238000010992 reflux Methods 0.000 abstract description 4
- 239000008346 aqueous phase Substances 0.000 abstract description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 14
- 238000000926 separation method Methods 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/58—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0208—Separation of non-miscible liquids by sedimentation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0217—Separation of non-miscible liquids by centrifugal force
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
-
- 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
- Y02P20/10—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Extraction Or Liquid Replacement (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a purification device for ethyl acetate production, which comprises a phase separation main body, wherein the phase separation main body comprises a phase separation tank, the top of the phase separation tank is fixedly communicated with a feed valve pipe which can be communicated with an external condenser, the bottom of the inner wall of the phase separation tank is respectively provided with an ester phase shell and a water phase shell, the interiors of the ester phase shell and the water phase shell are communicated with external equipment through a discharge pipe, and the phase separation component comprises a base rod. The purification device for ethyl acetate production can effectively solve the problems that in the prior art, when a phase separator is adopted for sedimentation and layering, more water is contained in an ester layer, and the preparation of ethyl acetate is a continuous process, so that the sedimentation time of ethyl acetate and water in the phase separator cannot be long enough, the obtained ester phase is not thoroughly separated from an aqueous phase, and more water can be carried in a reflux ester phase to enter an esterification tower.
Description
Technical Field
The invention relates to the technical field of ethyl acetate production, in particular to a purifying device for ethyl acetate production.
Background
Ethyl acetate is often referred to as ethyl acetate and is produced by steps including dosing, esterification, phase separation, dehydration, refining, and recovery. Because the water content in the ternary azeotrope composition of ethyl acetate, ethanol and water is less than 9%, and the water content of ethyl acetate and water produced by the reaction of acetic acid and ethanol is about 17%, in the esterification process, a reflux operation is set, and the water in the system is continuously carried out through the ternary azeotrope.
Acetic acid and ethanol are mixed according to a certain proportion and enter an esterification kettle, then concentrated sulfuric acid catalyst is added into the esterification kettle for esterification reaction, the reacted product enters an esterification tower, vapor phase ethyl acetate and water enter a phase separator for phase separation after being cooled by a tower top condenser to obtain crude ester, and the crude ester passes through a dehydration tower system and a rectifying tower system to obtain finished ethyl acetate. In the case of sedimentation and layering by using a phase separator, the ester layer contains more moisture, and the preparation of ethyl acetate is a continuous process, so that the sedimentation time of ethyl acetate and water in the phase separator cannot be long enough, the obtained ester phase is not thoroughly separated from the water phase, and more moisture is carried in the refluxed ester phase to enter the esterification tower.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects existing in the prior art, the invention provides a purifying device for ethyl acetate production, which can effectively solve the problems that in the prior art, when a phase separator is adopted for sedimentation and layering, more water is contained in an ester layer, and the preparation of ethyl acetate is a continuous process, so that the sedimentation time of ethyl acetate and water in the phase separator cannot be long enough, the obtained ester phase is not thoroughly separated from an aqueous phase, and more water is carried in a reflux ester phase to enter an esterification tower.
Technical proposal
In order to achieve the above purpose, the invention is realized by the following technical scheme:
the invention provides a purifying device for ethyl acetate production, which comprises:
the phase separation main body comprises a phase separation tank, the top of the phase separation tank is fixedly communicated with a feed valve pipe which can be communicated with an external condenser, the bottom of the inner wall of the phase separation tank is respectively provided with an ester phase shell and a water phase shell, and the interiors of the ester phase shell and the water phase shell are communicated with external equipment through discharge pipes;
the phase separation assembly comprises a base rod, the bottom end of the base rod is fixedly connected with the bottom of the inner wall of the phase separation tank, the top of the base rod is fixedly connected with a laminating plate, the top of the laminating plate is rotationally connected with a phase separation piece, and the top of the phase separation tank is provided with a driver which can be in transmission connection with the outer side of the phase separation piece;
the split-phase piece comprises a shaft rod, the bottom end of the shaft rod is rotationally connected with the inside of the attaching plate, the top end of the shaft rod penetrates through the split-phase tank and extends to the inside of the driver, a triangular plate is sleeved on the outer side of the shaft rod, a split-phase funnel is arranged in the triangular plate, a fan-shaped fixed plate is fixedly connected to the inner wall of the split-phase funnel, and a regulator which can be matched with the outer side of the attaching plate is rotationally connected to the bottom end of the fan-shaped fixed plate and used for opening and closing the bottom end of the split-phase funnel.
Further, the inside of the phase separation tank is a closed space, and saturated sodium carbonate solution is filled in the phase separation tank, and a collecting valve pipe is fixedly communicated with the outside of the phase separation tank.
Further, the bottom end of the feeding valve pipe is located above the phase separation funnel, a sensor is arranged on the outer side of the feeding valve pipe, and the bottom end of the sensor penetrates through the phase separation tank and extends to the position above the phase separation funnel.
Further, the laminating board includes annular plate, first arc board and second arc board outside all with annular plate outside fixed connection, annular plate top fixedly connected with draw-in groove, the set-square is through setting up slide and draw-in groove inner wall sliding connection in its bottom, first arc board is located directly over the water phase shell, the second arc board is located directly over the ester phase shell.
Further, the regulator comprises a sector moving plate, the top of the sector moving plate is rotationally connected with the bottom of the sector fixed plate through a rotating rod, and the sector moving plate is fixedly connected with a friction plate through a clamping plate arranged on the outer side of the sector moving plate.
Further, the split-phase funnel is provided with a sealing ring through a groove clamp arranged in the split-phase funnel, the outer side of the sealing ring is tightly attached to the outer side of the fan-shaped movable plate, the outer side of the friction plate is separated from the outer side of the annular plate, and the outer side of the friction plate is attached to the outer sides of the first arc plate and the second arc plate respectively.
Further, the outside fixedly connected with of phase separation funnel can with joint board outside sliding connection's track, inside stopper and the shielding plate of being provided with respectively of track.
Further, the limiting block and the shielding plate are both provided with two limiting blocks, the limiting blocks and the shielding plate are arranged in an equidistant and staggered mode, and a hard arc rod which can be in sliding connection with the inside of the clamping plate is fixedly connected to the outer side of the shielding plate.
Further, the shielding plate outside fixedly connected with bending spring, the bending spring cover is established in the stereoplasm arc pole outside, bending spring keeps away from shielding plate one end and clamping plate outside fixed connection.
Advantageous effects
Compared with the prior art, the technical scheme provided by the invention has the following beneficial effects:
the invention is provided with a feeding valve pipe, a bonding plate, a phase separation funnel and a regulator, wherein the phase separation funnel is designed with three groups, the included angle between the phase separation funnels is 120 degrees, when one phase separation funnel is transported below the sensor, the sensor regulates and controls the valve on the feeding valve pipe to be opened through an external PLC, the cooled ethyl acetate and water in the feeding valve pipe flow into the corresponding phase separation funnel through the feeding valve pipe, after the phase separation funnels filled with the ethyl acetate and the water slowly rotate for 120 degrees (the time used in the rotating period is longer, because the ethyl acetate and the water are mutually incompatible and have larger difference in density, the ethyl acetate and the water form an upper segment and a lower segment in the phase separation funnels), meanwhile, the regulator starts to contact with a first arc plate on the bonding plate, a channel can be formed between the regulator and the fan-shaped fixed plate, the water at the lower end of the phase separation funnel flows into a water phase shell, then the regulator contacts with a second arc plate, a channel is formed between the regulator and the fan-shaped fixed plate, and the ethyl acetate flows into the phase shell again. The three-component phase funnel corresponds to three conditions of ethyl acetate and water mixed liquid, ethyl acetate and water layering liquid and ethyl acetate respectively, and the phase-separating funnel is matched with a feed valve pipe, a sensor and a phase-separating assembly, so that water phase, ester phase and ethyl acetate and water layering are synchronously carried out, compared with a traditional phase-separating device, settling layering (consuming longer time) is carried out firstly, then water phase separation is carried out, finally ester phase separation is carried out, the separation time of ethyl acetate and water is greatly shortened, and meanwhile, when the regulator is matched with a phase-separating piece, the phase-separating funnel continuously rotates slowly at a constant speed, wherein the two-component phase funnel carries out water phase and ester phase separation, ethyl acetate and water in the other-component phase funnel have enough time to precipitate, mutual interference between the ethyl acetate and the water in the phase-separating device is avoided, and the obtained ester phase and water phase separation is not thorough.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It is evident that the drawings in the following description are only some embodiments of the present invention and that other drawings may be obtained from these drawings without inventive effort for a person of ordinary skill in the art.
FIG. 1 is a schematic view of a three-dimensional structure of the present invention;
FIG. 2 is a schematic view of a three-dimensional partial cross-section of the present invention;
FIG. 3 is a schematic view of a multi-angle three-dimensional partial cross-section of the present invention;
FIG. 4 is a schematic view of a split-phase member according to the present invention;
FIG. 5 is a schematic diagram of a three-dimensional separation structure of a phase separation member according to the present invention;
FIG. 6 is a schematic view showing a three-dimensional combination of a phase separation funnel and a regulator according to the present invention;
FIG. 7 is a schematic view of a regulator according to the present invention;
fig. 8 is a schematic view of a three-dimensional exploded structure of the regulator of the present invention.
Reference numerals in the drawings represent respectively: 1. a split-phase main body; 11. a split-phase tank; 12. a feed valve tube; 13. an ester phase shell; 14. a water phase shell; 15. a collection valve tube; 16. a sensor; 2. a phase separation assembly; 21. a base rod; 22. bonding plates; 221. a ring plate; 222. a first arc plate; 223. a second arc plate; 224. a clamping groove; 23. a split-phase member; 231. a shaft lever; 232. a triangle; 233. a split-phase funnel; 2331. a groove; 234. a fan-shaped fixed plate; 235. a regulator; 2351. a fan-shaped movable plate; 2352. a clamping plate; 2353. a friction plate; 2354. a track; 2355. a limiting block; 2356. a shielding plate; 2357. a hard arc rod; 2358. a bending spring; 236. a seal ring; 24. a driver.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. It will be apparent that the described embodiments are some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention is further described below with reference to examples.
Examples:
referring to fig. 1-8, the present invention provides a technical solution: a purification device for ethyl acetate production, comprising:
the device comprises a phase separation main body 1, wherein the phase separation main body 1 comprises a phase separation tank 11, a feed valve pipe 12 which can be communicated with an external condenser is fixedly communicated with the top of the phase separation tank 11, an ester phase shell 13 and a water phase shell 14 are respectively arranged at the bottom of the inner wall of the phase separation tank 11, and the interiors of the ester phase shell 13 and the water phase shell 14 are communicated with external equipment through discharge pipes;
the phase separation assembly 2 comprises a base rod 21, the bottom end of the base rod 21 is fixedly connected with the bottom of the inner wall of the phase separation tank 11, the top of the base rod 21 is fixedly connected with a bonding plate 22, the top of the bonding plate 22 is rotationally connected with a phase separation piece 23, and the top of the phase separation tank 11 is provided with a driver 24 which can be in transmission connection with the outer side of the phase separation piece 23;
the split-phase piece 23 comprises a shaft lever 231, the bottom end of the shaft lever 231 is rotationally connected with the inside of the attaching plate 22, the top end of the shaft lever 231 penetrates through the split-phase tank 11 and extends to the inside of the driver 24, a triangular plate 232 is sleeved outside the shaft lever 231, a split-phase funnel 233 is arranged inside the triangular plate 232, a fan-shaped fixed plate 234 is fixedly connected to the inner wall of the split-phase funnel 233, and a regulator 235 which can be matched with the outside of the attaching plate 22 is rotationally connected to the bottom of the fan-shaped fixed plate 234 and used for opening and closing the bottom end of the split-phase funnel 233.
The inside of the phase-splitting tank 11 is a closed space, the inside of the phase-splitting tank 11 is filled with saturated sodium carbonate solution, the outside of the phase-splitting tank 11 is fixedly communicated with a collecting valve pipe 15, volatilized acetic acid is absorbed by the saturated sodium carbonate solution, meanwhile, ethanol is easily dissolved in the saturated sodium carbonate solution, separation of ethyl acetate from acetic acid and ethanol is facilitated, the inside of the phase-splitting tank 11 is a closed space, volatilized ethyl acetate is reserved in the inside of the phase-splitting tank 11, and unified collection is facilitated through the collecting valve pipe 15.
The bottom end of the feed valve pipe 12 is located above the phase separation funnel 233, and a sensor 16 is arranged outside the feed valve pipe 12, and the bottom end of the sensor 16 penetrates through the phase separation tank 11 and extends to above the phase separation funnel 233. The separating funnels 233 are designed to be three groups, the included angle between the separating funnels 233 is 120 degrees, when one separating funnel 233 is transported to the lower part of the sensor 16, the sensor 16 regulates and controls the valve on the feeding valve pipe 12 to be opened through an external PLC, ethyl acetate and water cooled in the feeding valve pipe 12 flow into the corresponding separating funnel 233 through the feeding valve pipe 12, the three-group separating funnels 233 respectively correspond to three conditions of ethyl acetate and water mixed liquid, ethyl acetate and water layering liquid and ethyl acetate, and the separating funnel 233 is matched with the feeding valve pipe 12, the sensor 16 and the separating assembly 2, water phase, ester phase and ethyl acetate and water layering are synchronously carried out, compared with the traditional separator, sedimentation layering is carried out firstly (time is longer), then water phase separation is carried out, finally ester phase separation is carried out, the separation time of ethyl acetate and water is greatly shortened, simultaneously, when the regulator 235 is matched with the separating element 23, the two-group separating funnels 233 continuously rotate slowly, ethyl acetate and water phase separation are carried out at a uniform speed, the other-group separating funnels 233 have enough time to interfere with ethyl acetate and water phase, and the water phase sedimentation situation of the ethyl acetate phase and the water phase separation are not carried out thoroughly, and the sedimentation time of the ethyl acetate phase and the water phase separation are not carried out thoroughly.
The laminating plate 22 comprises a ring plate 221, a first arc plate 222 and a second arc plate 223, wherein the outer sides of the first arc plate 222 and the second arc plate 223 are fixedly connected with the outer side of the ring plate 221, the top of the ring plate 221 is fixedly connected with a clamping groove 224, a triangular plate 232 is slidably connected with the inner wall of the clamping groove 224 through a sliding plate arranged at the bottom of the triangular plate 232, the first arc plate 222 is positioned right above the water phase shell 14, the second arc plate 223 is positioned right above the ester phase shell 13, the effective length of the first arc plate 222 is smaller than the length of the water phase shell 14, and the effective length of the second arc plate 223 is smaller than the length of the ester phase shell 13.
The regulator 235 includes a sector moving plate 2351, the top of the sector moving plate 2351 is rotatably connected to the bottom of the sector fixed plate 234 through a rotating rod, and the sector moving plate 2351 is fixedly connected to a friction plate 2353 through a clamping plate 2352 provided at the outer side thereof.
The separating funnel 233 is provided with a sealing ring 236 by clamping a groove 2331 formed in the separating funnel 233, the outer side of the sealing ring 236 is tightly attached to the outer side of the sector moving plate 2351, and the sealing ring is used for sealing between the sector moving plate 2351 and the separating funnel 233, the outer side of the friction plate 2353 is separated from the outer side of the annular plate 221, and the outer sides of the friction plates 2353 are attached to the outer sides of the first arc plate 222 and the second arc plate 223 respectively.
The outside fixedly connected with of separating funnel 233 can with joint board 2352 outside sliding connection's track 2354, track 2354 inside is provided with stopper 2355 and shielding plate 2356 respectively.
Stopper 2355 and shielding plate 2356 all are provided with two, and equidistant crisscross setting between stopper 2355 and the shielding plate 2356, shielding plate 2356 outside fixedly connected with can with the inside sliding connection's of joint board 2352 stereoplasm arc pole 2357.
The outside fixedly connected with bending spring 2358 of shielding plate 2356, bending spring 2358 cover is established in the stereoplasm arc pole 2357 outside, and bending spring 2358 keeps away from shielding plate 2356 one end and clamping plate 2352 outside fixed connection. Friction plate 2353 on regulator 235 starts to contact first arc plate 222, first arc plate 222 produces frictional force to friction plate 2353, drive friction plate 2353 to rotate clockwise, because the length of first arc plate 222 and second arc plate 223 is far longer than the length of friction plate 2353, friction plate 2353 moves along the outside of first arc plate 222 for a very short time, friction plate 2353 drives joint plate 2352 to be fast attached to the outside of limiting block 2355, joint plate 2352 slides along the outside of hard arc rod 2357, and extrudes bending spring 2358, drive sector plate 2351 to rotate clockwise 90 ° around sector fixed plate 234, sector fixed plate 2351 and sector fixed plate 234 form a flow channel, until friction plate 2353 breaks away from first arc plate 222, first arc plate 222 is rapidly reset under the elastic force of bending spring 2358, the flow channel between sector fixed plate 234 and sector fixed plate 234 is closed, at this time, the water phase in split-phase funnel 233 is totally flowed out, and ethyl acetate remains in split-phase funnel 233. Similarly, the separating funnel 233 containing only ethyl acetate is rotated to the side of the second arc plate 223, and since the ethyl acetate content in the separating funnel 233 is about 83%, by increasing the effective length of the second arc plate 223, the ethyl acetate in the separating funnel 233 is entirely flowed into the ester phase housing 13, and when the friction plate 2353 is separated from the first arc plate 222, the flow passage between the sector moving plate 2351 and the sector fixed plate 234 is closed again, and the next cycle is entered.
Referring to fig. 1-8, acetic acid and ethanol are mixed according to a certain proportion and enter an esterification kettle, then concentrated sulfuric acid catalyst is added into the esterification kettle for esterification reaction, the reacted product enters an esterification tower, and vapor phase ethyl acetate and water enter a phase separator for phase separation after being cooled by a tower top condenser to obtain crude ester. However, when the phase separator is used for sedimentation and layering, a problem exists that the ester layer contains more water, and the preparation of ethyl acetate is a continuous process, so that the sedimentation time of ethyl acetate and water in the phase separator cannot be long enough, the obtained ester phase is not thoroughly separated from the water phase, and more water is carried in the refluxed ester phase to enter the esterification tower. According to the invention, the traditional phase separator is replaced by combining the phase separation main body 1 and the phase separation component 2, so that the separation of an ester phase and a water phase is accelerated, and meanwhile, more water carried in the refluxing ester phase is prevented from entering the esterification tower, and the integral purification rate and purity of ethyl acetate are improved.
When in use, the driver 24 (servo motor group) in the phase separation assembly 2 is started to drive the shaft lever 231 in the phase separation assembly 23 to rotate slowly and uniformly clockwise around the inside of the annular plate 221, and drive the triangular plate 232 and the phase separation funnel 233 to rotate slowly and uniformly synchronously. The phase separation funnels 233 are designed to be three groups in total, the included angle between the phase separation funnels 233 is 120 degrees, when one of the phase separation funnels 233 is transported below the sensor 16, the sensor 16 regulates and controls the valve on the feed valve pipe 12 to be opened through an external PLC, ethyl acetate and water cooled in the feed valve pipe 12 flow into the corresponding phase separation funnel 233 through the feed valve pipe 12 (the pipe orifice diameter of the feed valve pipe 12 is larger, the diameter of the phase separation funnel 233 is far larger than the pipe orifice diameter of the feed valve pipe 12), the feed valve pipe 12 can fill the phase separation funnel 233 before the phase separation funnels 233 are separated from the pipe orifice of the feed valve pipe 12, the valve of the feed valve pipe 12 is synchronously closed, the phase separation funnels 233 filled with ethyl acetate and water continue to slowly rotate at a uniform speed, and the subsequent phase separation funnels 233 are continuously filled with ethyl acetate and water in batches. After the phase separation funnel 233 filled with ethyl acetate and water is slowly rotated 120 ° (the time taken during rotation is long, ethyl acetate and water are not compatible with each other, and there is a large difference in density between them, so that ethyl acetate and water form upper and lower stages of layering in the phase separation funnel 233), at the same time, the regulator 235 starts to contact the first arc plate 222 on the adhesion plate 22, a passage may be formed between the regulator 235 and the sector plate 234, moisture at the lower end of the phase separation funnel 233 flows into the water phase casing 14, the passage between the regulator 235 and the sector plate 234 is rapidly closed when the regulator 235 is separated from the first arc plate 222, ethyl acetate remains in the phase separation funnel 233, then the regulator 235 contacts the second arc plate 223, a passage is formed again between the regulator 235 and the sector plate 234, ethyl acetate flows into the ester phase casing 13, and when the regulator 235 is separated from the second arc plate 223, the passage between the regulator 235 and the sector plate 234 is closed, and then the phase separation funnel 233 is again rotated to the lower side of the feed valve pipe 12 to enter the next cycle. The three-component phase funnel 233 corresponds to three conditions of ethyl acetate and water mixed liquid, ethyl acetate and water layering liquid and ethyl acetate respectively, and the phase funnel 233 is matched with the feed valve pipe 12, the sensor 16 and the phase separation component 2, so that water phase, ester phase and ethyl acetate and water layering are synchronously carried out, compared with the traditional phase separator, settling layering (time consuming is long) firstly, then water phase separation and finally ester phase separation are carried out, the separation time of ethyl acetate and water is greatly shortened, and meanwhile, when the regulator 235 is matched with the phase separation piece 23, the phase funnel 233 continuously rotates slowly at a constant speed, wherein the two-component phase funnel 233 carries out water phase and ester phase separation, ethyl acetate and water in the other component phase funnel 233 are sufficiently time to precipitate, mutual interference is avoided, and the conditions that the settling time of ethyl acetate and water in the phase separator is not long enough and the separation of the obtained ester phase and the water phase is not thorough are avoided.
After ethyl acetate and water in the separating funnel 233 are layered, at the same time the separating funnel 233 rotates to one side of the first arc plate 222 of the attaching plate 22, the side sides of the first arc plate 222 and the second arc plate 223 are designed to be arc sides, the friction plate 2353 on the regulator 235 starts to contact the first arc plate 222, the first arc plate 222 generates friction force on the friction plate 2353 to drive the friction plate 2353 to rotate clockwise, because the lengths of the first arc plate 222 and the second arc plate 223 are far longer than the length of the friction plate 2353, the friction plate 2353 moves along the outer side of the first arc plate 222 for a very short time, the friction plate 2353 drives the clamping plate 2352 to be attached to the outer side of the limiting block 2355 rapidly (the maximum rotation angle of the friction plate 2353 is 90 degrees, the rotation time of the friction plate 2353 is negligible), the clamping plate 2352 slides along the outer side of the hard arc rod 2357, and presses the bending spring 2358 to drive the fan-shaped moving plate 2351 to rotate clockwise around the fan-shaped fixed plate 234 by 90 degrees, and a flow channel is formed between the fan-shaped moving plate 2351 and the fan-shaped fixed plate 234; due to the limiting effect of the limiting block 2355, during the subsequent friction sliding of the friction plate 2353 along the outer side of the first arc plate 222, water in the phase separation funnel 233 flows into the water phase shell 14 through the flow channel until the friction plate 2353 is separated from the first arc plate 222, the friction force of the friction plate 2353 received by the first arc plate 222 disappears, the first arc plate 222 is quickly reset under the elastic force of the bending spring 2358, the fan-shaped movable plate 2351 is driven to rotate 90 degrees anticlockwise, the flow channel between the fan-shaped movable plate 2351 and the fan-shaped fixed plate 234 is closed, at this time, all water phase in the phase separation funnel 233 flows out, ethyl acetate remains in the phase separation funnel 233 (because the valve on the feed valve tube 12 is regulated by the PLC, the volume of each time flowing into the phase separation funnel 233 is constant, the ethyl acetate and water generated by the reaction of acetic acid and ethanol, the water content is about 17%, and then the water volume of the phase separation funnel 233 is determined, and the water volume of just can be completely separated from the phase separation funnel 233 when the friction plate 2353 is separated from the first arc plate 222 by combining the effective length of the first arc plate 222 and the rotation speed of the phase separation funnel 233 bottom diameter.
Similarly, the separating funnel 233 containing only ethyl acetate is rotated to the side of the second arc plate 223, and since the ethyl acetate content in the separating funnel 233 is about 83%, by increasing the effective length of the second arc plate 223, the ethyl acetate in the separating funnel 233 is entirely flowed into the ester phase housing 13, and when the friction plate 2353 is separated from the first arc plate 222, the flow passage between the sector moving plate 2351 and the sector fixed plate 234 is closed again, and the next cycle is entered.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; these modifications or substitutions do not depart from the essence of the corresponding technical solutions from the protection scope of the technical solutions of the embodiments of the present invention.
Claims (9)
1. A purification device for ethyl acetate production, comprising:
the device comprises a phase separation main body (1), wherein the phase separation main body (1) comprises a phase separation tank (11), a feed valve pipe (12) which can be communicated with an external condenser is fixedly communicated with the top of the phase separation tank (11), an ester phase shell (13) and a water phase shell (14) are respectively arranged at the bottom of the inner wall of the phase separation tank (11), and the interiors of the ester phase shell (13) and the water phase shell (14) are communicated with external equipment through discharge pipes;
the phase separation assembly (2), the phase separation assembly (2) comprises a base rod (21), the bottom end of the base rod (21) is fixedly connected with the bottom of the inner wall of the phase separation tank (11), the top of the base rod (21) is fixedly connected with a bonding plate (22), the top of the bonding plate (22) is rotationally connected with a phase separation piece (23), and the top of the phase separation tank (11) is provided with a driver (24) which can be in transmission connection with the outer side of the phase separation piece (23);
the split-phase piece (23) comprises a shaft lever (231), the bottom end of the shaft lever (231) is connected with the inside of the attaching plate (22) in a rotating mode, the top end of the shaft lever (231) penetrates through the split-phase tank (11) and extends to the inside of the driver (24), a triangular plate (232) is sleeved outside the shaft lever (231), a split-phase funnel (233) is arranged inside the triangular plate (232), a fan-shaped fixed plate (234) is fixedly connected to the inner wall of the split-phase funnel (233), and a regulator (235) which can be matched with the outer side of the attaching plate (22) is rotationally connected to the bottom of the fan-shaped fixed plate (234) and used for opening and closing the bottom end of the split-phase funnel (233).
2. A purification device for ethyl acetate production according to claim 1 wherein: the inside of the phase separation tank (11) is a closed space, and the saturated sodium carbonate solution is filled in the phase separation tank (11), and the outside of the phase separation tank (11) is fixedly communicated with a collecting valve pipe (15).
3. A purification device for ethyl acetate production according to claim 1 wherein: the bottom end of the feeding valve pipe (12) is located above the phase separation funnel (233), a sensor (16) is arranged on the outer side of the feeding valve pipe (12), and the bottom end of the sensor (16) penetrates through the phase separation tank (11) and extends to the position above the phase separation funnel (233).
4. A purification device for ethyl acetate production according to claim 1 wherein: laminating board (22) are including annular plate (221), first arc board (222) and second arc board (223) outside all with annular plate (221) outside fixed connection, annular plate (221) top fixedly connected with draw-in groove (224), set-square (232) are through setting up slide and draw-in groove (224) inner wall sliding connection in its bottom, first arc board (222) are located water phase shell (14) directly over, second arc board (223) are located ester looks shell (13) directly over.
5. The purification device for ethyl acetate production according to claim 4, wherein: the regulator (235) comprises a sector moving plate (2351), the top of the sector moving plate (2351) is rotationally connected with the bottom of the sector fixed plate (234) through a rotating rod, and the sector moving plate (2351) is fixedly connected with a friction plate (2353) through a clamping plate (2352) arranged on the outer side of the sector moving plate.
6. The purification device for ethyl acetate production according to claim 5, wherein: the split-phase funnel (233) is provided with a sealing ring (236) through a groove (2331) arranged in the split-phase funnel, the outer side of the sealing ring (236) is tightly attached to the outer side of a sector-shaped movable plate (2351), the outer side of a friction plate (2353) is separated from the outer side of a ring plate (221), and the outer sides of the friction plate (2353) are attached to the outer sides of a first arc plate (222) and a second arc plate (223) respectively.
7. The purification device for ethyl acetate production according to claim 6, wherein: the split-phase funnel is characterized in that a track (2354) which can be in sliding connection with the outer side of the clamping plate (2352) is fixedly connected to the outer side of the split-phase funnel (233), and a limiting block (2355) and a shielding plate (2356) are respectively arranged in the track (2354).
8. The purification device for ethyl acetate production according to claim 7, wherein: stopper (2355) and shielding plate (2356) all are provided with two, just equidistant crisscross setting between stopper (2355) and shielding plate (2356), shielding plate (2356) outside fixedly connected with can with inside sliding connection's of joint board (2352) stereoplasm arc pole (2357).
9. The purification device for ethyl acetate production according to claim 8, wherein: the shielding plate (2356) is fixedly connected with a bending spring (2358) outside, the bending spring (2358) is sleeved outside the hard arc rod (2357), and one end, away from the shielding plate (2356), of the bending spring (2358) is fixedly connected with the outer side of the clamping plate (2352).
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310463254.6A CN116459752B (en) | 2023-04-26 | 2023-04-26 | A purification device for ethyl acetate production |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310463254.6A CN116459752B (en) | 2023-04-26 | 2023-04-26 | A purification device for ethyl acetate production |
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| CN116459752B CN116459752B (en) | 2023-10-20 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN208943487U (en) * | 2018-10-11 | 2019-06-07 | 九江齐鑫化工有限公司 | Grease separator in a kind of sec-butyl acetate azeotropic distillation |
| CN212818288U (en) * | 2020-04-08 | 2021-03-30 | 上海抚佳精细化工有限公司 | Oil-water separation device and esterification reaction system using same |
| CN217449045U (en) * | 2022-06-13 | 2022-09-20 | 河南全宇制药股份有限公司 | Ethyl acetate extraction device |
| CN218131609U (en) * | 2022-06-25 | 2022-12-27 | 辽宁新邦新材料有限公司 | Closed high-speed dispersion equipment for production of phenyl silicone rubber in aerospace field |
| EP4148060A1 (en) * | 2021-01-25 | 2023-03-15 | Anhui Jinhe Industrial Co., Ltd. | Production equipment and production method for sucrose-6-ester |
-
2023
- 2023-04-26 CN CN202310463254.6A patent/CN116459752B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN208943487U (en) * | 2018-10-11 | 2019-06-07 | 九江齐鑫化工有限公司 | Grease separator in a kind of sec-butyl acetate azeotropic distillation |
| CN212818288U (en) * | 2020-04-08 | 2021-03-30 | 上海抚佳精细化工有限公司 | Oil-water separation device and esterification reaction system using same |
| EP4148060A1 (en) * | 2021-01-25 | 2023-03-15 | Anhui Jinhe Industrial Co., Ltd. | Production equipment and production method for sucrose-6-ester |
| CN217449045U (en) * | 2022-06-13 | 2022-09-20 | 河南全宇制药股份有限公司 | Ethyl acetate extraction device |
| CN218131609U (en) * | 2022-06-25 | 2022-12-27 | 辽宁新邦新材料有限公司 | Closed high-speed dispersion equipment for production of phenyl silicone rubber in aerospace field |
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| CN116459752B (en) | 2023-10-20 |
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