CN112358397A - Equipment and method for rectifying and separating ethyl acetate and ethanol azeotrope - Google Patents
Equipment and method for rectifying and separating ethyl acetate and ethanol azeotrope Download PDFInfo
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- CN112358397A CN112358397A CN202011331299.0A CN202011331299A CN112358397A CN 112358397 A CN112358397 A CN 112358397A CN 202011331299 A CN202011331299 A CN 202011331299A CN 112358397 A CN112358397 A CN 112358397A
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- condenser
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- condensation
- ethyl acetate
- azeotrope
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- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 title claims abstract description 96
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims description 10
- 238000009833 condensation Methods 0.000 claims abstract description 56
- 230000005494 condensation Effects 0.000 claims abstract description 56
- 238000004821 distillation Methods 0.000 claims abstract description 46
- 238000011084 recovery Methods 0.000 claims abstract description 41
- 238000010992 reflux Methods 0.000 claims abstract description 11
- 238000007599 discharging Methods 0.000 claims abstract description 8
- 239000010410 layer Substances 0.000 claims description 51
- 238000003756 stirring Methods 0.000 claims description 25
- 238000010438 heat treatment Methods 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000003365 glass fiber Substances 0.000 claims description 15
- 238000000926 separation method Methods 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 13
- -1 phenolic aldehyde Chemical class 0.000 claims description 11
- 150000002148 esters Chemical class 0.000 claims description 9
- 238000009835 boiling Methods 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 7
- 238000000576 coating method Methods 0.000 claims description 7
- 239000000853 adhesive Substances 0.000 claims description 6
- 230000001070 adhesive effect Effects 0.000 claims description 6
- 239000002351 wastewater Substances 0.000 claims description 6
- 238000005260 corrosion Methods 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 4
- 229910000838 Al alloy Inorganic materials 0.000 claims description 3
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 3
- 239000012790 adhesive layer Substances 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 239000004917 carbon fiber Substances 0.000 claims description 3
- 239000011083 cement mortar Substances 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 3
- 238000005886 esterification reaction Methods 0.000 claims description 3
- 125000004494 ethyl ester group Chemical group 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- 229920002635 polyurethane Polymers 0.000 claims description 3
- 239000004814 polyurethane Substances 0.000 claims description 3
- 238000005191 phase separation Methods 0.000 claims description 2
- 238000010276 construction Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 16
- 210000003205 muscle Anatomy 0.000 description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000004321 preservation Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 239000000796 flavoring agent Substances 0.000 description 2
- 239000002304 perfume Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000020 Nitrocellulose Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 238000010533 azeotropic distillation Methods 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 238000007257 deesterification reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000000895 extractive distillation Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 235000013355 food flavoring agent Nutrition 0.000 description 1
- 239000004434 industrial solvent Substances 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Images
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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
-
- 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
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
-
- 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
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
-
- 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
Abstract
The invention discloses equipment for rectifying and separating an ethyl acetate and ethanol azeotrope, which comprises a condenser I, a distillation kettle, a reboiler I, a reboiler II, a phase separator, a pump I, a pump II, a condenser II, a recovery tower, a condenser III, a reflux tank, a pump III and a pump IV; i condenser II of condenser and condenser III all include the condenser body of taking feed pipe, discharging pipe, inlet tube, outlet pipe, condensation chamber and condenser pipe, the condenser pipe be double-deck tubular construction, including inner tube and outer support tube, outer support tube cover establish in the inner tube outside integrated into one piece has a plurality of condensation wings according to circumference evenly distributed on the lateral wall of inner tube, and outer support tube on set up the parcel portion of parcel condensation wing.
Description
Technical Field
The invention belongs to the technical field of rectification of an azeotrope of ethyl acetate and ethanol, and particularly relates to equipment and a method for rectifying and separating the azeotrope of ethyl acetate and ethanol.
Background
Ethyl Acetate (EA), also known as Ethyl Acetate, is a branch of downstream acetic acid derived products. It belongs to the category of chemical solvents, is an important green organic solvent, has excellent solubility and is a quick-drying industrial solvent. Ethyl acetate is widely used for the production of polymers such as fibers, rubbers, resins and the like and medical intermediates; can also be used for producing liquid nitrocellulose ink for duplicators; as a freshener in the textile industry; flavor extractants for use as specially modified alcohols in the food industry; the perfume industry is the most important perfume additive, which can be used as a component of a flavoring agent. In addition, ethyl acetate is also used as a solvent for adhesives, a diluent for paints, and a raw material for manufacturing drugs and dyes.
At present, an acetic acid and ethanol esterification method is mainly adopted in an ethyl acetate production method, ethanol is excessive in the reaction process, ethanol and water in an obtained ethyl acetate crude product cannot meet the requirement of 99.7% of the purity of a superior product of GB/T3728-2007 ethyl acetate for industrial use, separation and purification are needed again, but the boiling points of the ethyl acetate and the ethanol are only different by 1 ℃ and azeotropic exists, so that the production of high-purity ethyl acetate cannot be realized through ordinary rectification. At present, azeotropic distillation and extractive distillation are industrially used for the separation method, but the effect of the existing condenser and distillation still is not ideal, so that the rectification separation effect is not ideal.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for rectifying and separating ethyl acetate and ethanol azeotrope by using equipment.
In order to achieve the purpose, the invention provides the following technical scheme: an apparatus for rectifying and separating an ethyl acetate and ethanol azeotrope comprises a condenser I, a distillation kettle, a reboiler I, a reboiler II, a phase separator, a pump I, a pump II, a condenser II, a recovery tower, a condenser III, a reflux tank, a pump III and a pump IV; the condenser I, the condenser II and the condenser III respectively comprise condenser bodies with a feeding pipe, a discharging pipe, a water inlet pipe, a water outlet pipe, a condensing cavity and a condensing pipe, the condensing pipe is of a double-layer pipe structure and comprises an inner pipe and an outer supporting pipe, the outer supporting pipe is sleeved outside the inner pipe, a plurality of condensing wings which are uniformly distributed according to the circumference are integrally formed on the outer side wall of the inner pipe, and a wrapping part for wrapping the condensing wings is arranged on the outer supporting pipe; the distillation kettle comprises a kettle body, wherein a stirring shaft is arranged in the kettle body, a stirring motor is arranged at the top of the kettle body and drives the stirring shaft to rotate, a cavity is formed in the side wall of the kettle body, and a heating inlet pipe and a heating outlet pipe which are communicated with the cavity are arranged outside the kettle body; the reaction kettle is characterized in that a heat insulation layer is coated outside the kettle body, the cavity is in an annular column shape, a plurality of rotating shafts which are uniformly distributed according to the column shape and extend into the cavity are arranged at the top of the kettle body, stirring blades are arranged at the positions, located in the cavity, of the rotating shafts, and each rotating shaft is driven by a rotating motor.
By adopting the technical scheme, the plurality of condensation wings which are uniformly distributed according to the circumference are integrally formed on the outer side wall of the inner pipe of the condensation pipe, and the wrapping part wrapping the condensation wings is arranged on the outer supporting pipe, so that the integral contact area of the condensation pipe can be increased, and the condensation effect is ensured; the distillation still drives the stirring leaf rotation through setting up the rotation axis for heating medium in the air carries out good stirring and mixes, thereby ensures the stability of heating medium temperature, in order to ensure the effect of distillation.
The invention is further configured to: the stirring blades are spiral, and the rotating directions of two adjacent rotating shafts are opposite.
Through adopting foretell technical scheme, stirring leaf is the heliciform, and the rotation direction of two adjacent rotation axes is opposite to can further ensure the effect of mixing.
The invention is further configured to: the heat-insulating layer is coated outside the kettle body through an adhesive.
By adopting the technical scheme, the heat-insulating layer is coated outside the kettle body through the adhesive, so that the manufacturing of the distillation kettle can be facilitated.
The invention is further configured to: the heat-insulating layer comprises a phenolic aldehyde heat-insulating plate layer and inorganic glass fiber layers arranged on two sides of the phenolic aldehyde heat-insulating plate layer, the inorganic glass fiber layers are of a structure of a polymer modified cement mortar composite glass fiber felt layer, and the phenolic aldehyde heat-insulating plate layer is connected with the inorganic glass fiber layers through siloxane modified polyurethane adhesive layers.
Through adopting foretell technical scheme, the heat preservation includes phenolic aldehyde heat preservation sheet layer, inorganic glass fiber layer to make the heat preservation can play good heat preservation effect, and then ensure stills's heat utilization ratio.
The invention is further configured to: an anti-corrosion coating is sprayed outside the heat-insulating layer.
By adopting the technical scheme, the anti-corrosion coating is sprayed outside the heat-insulating layer, so that the practical service life of the heat-insulating layer can be ensured.
The invention is further configured to: the outside of parcel portion is provided with a plurality of along the straight line evenly distributed and fan-shaped flaky condensation muscle, condensation muscle and inner tube coaxial setting.
Through adopting foretell technical scheme, the outside of parcel portion is provided with a plurality of along the straight line evenly distributed and fan-shaped flaky condensation muscle, and the condensation muscle sets up with the inner tube is coaxial to ensure the holistic condensation effect of condenser pipe greatly.
The invention is further configured to: a plurality of uniformly distributed support ribs are respectively arranged outside the wrapping part and on two sides of the condensation rib, and the support ribs and the condensation wings are distributed in a staggered manner.
Through adopting foretell technical scheme, outside the parcel portion, and be located the bracing piece that is provided with a plurality of evenly distributed respectively on the condensation muscle both sides, the bracing piece has also further improved the surface area of condenser pipe when improving parcel portion intensity to the effect and the efficiency of condensation have further been ensured.
The invention is further configured to: the inner pipe is made of copper or copper alloy, and the outer supporting pipe is made of aluminum or aluminum alloy.
Through adopting foretell technical scheme, through the setting of two kinds of materials, do the thickness of inner tube as far as possible thin, the support of rethread outer stay tube has ensured the bulk strength of condenser pipe to when guaranteeing the condensation effect reduced the cost that inner tube raw and other materials dropped into.
The invention is further configured to: the condensing wing is provided with a plurality of condensing holes which are uniformly distributed and penetrate through the wrapping part, heat conducting rods are inserted in the condensing holes, and the heat conducting rods contain heat conducting carbon fibers.
Through adopting foretell technical scheme, be provided with a plurality of evenly distributed on the condensation wing and run through the condensation hole of parcel portion, insert on the condensation hole and be equipped with the heat conduction stick to can further improve the condensation efficiency of condenser pipe.
The invention is further configured to: the rectification separation method of the device comprises the following steps:
the method comprises the following steps that firstly, crude ester continuously enters a distillation kettle through a condenser I, the boiling of materials in the distillation kettle is realized under the heating action of a reboiler I by the materials in the distillation kettle, the ternary azeotrope formed by the ester, alcohol and water and the binary azeotrope formed by the ethyl ester and water are low in boiling point, the top of the distillation kettle is evaporated after the distillation kettle is rectified, the evaporated product enters a reboiler II connected with a recovery tower and is condensed in the reboiler II, the condensed liquid enters a phase separator for phase separation, the ester phase is sent to the distillation kettle through a pump I, the water phase enters a recovery working section, the distillation kettle continuously discharges materials through the pump II to obtain ethyl acetate, the whole system is closed and emptied after air is exhausted, and the system is kept to operate under a pressurized state;
step two, continuously feeding the wastewater into a recovery tower through a condenser II, carrying out reduced pressure distillation in the recovery tower under the heating action of a reboiler II, feeding evaporated materials into a condenser III for condensation, feeding the condensate into a reflux tank of the recovery tower, connecting the recovery tank with a vacuum system to maintain the vacuum state of the whole system, dividing the condensate in the reflux tank into two streams, feeding one stream into the recovery tower through a pump III to maintain the rectification state of the recovery tower, extracting one stream out of a de-esterification system, and continuously discharging the wastewater from a kettle of the recovery tower through a pump IV;
wherein: in the first step, the steam of the distillate which is distilled from the top of the distillation still and enters a reboiler of the recovery tower is used as a heat source of the recovery tower in the second step; in the first step, the heating temperature of the distillation kettle is 100-; in the second step, the heating temperature of the recovery tower is 68-78 ℃, the temperature of the top of the tower is 35-45 ℃, and the relative vacuum pressure of the system is 65-75 KPa.
Drawings
FIG. 1 is a flow diagram of the process for separating an azeotrope of ethyl acetate and ethanol by differential pressure distillation of the invention;
FIG. 2 is a schematic diagram of the structure of the distillation still in the invention;
FIG. 3 is an enlarged view of a portion of FIG. 2 at I;
FIG. 4 is a schematic view of the condenser of the present invention;
FIG. 5 is a schematic view of the condenser tube of the present invention;
FIG. 6 is a schematic cross-sectional view of a condenser tube according to the present invention;
reference numbers in the drawings and corresponding part names: 1-condenser I, 2-distillation still, 3-reboiler I, 4-reboiler II, 5-phase separator, 6-pump I, 7-pump II, 8-condenser II, 9-recovery tower, 10-condenser III, 11-reflux tank, 12-pump III, 13-pump IV, 101-feeding pipe, 102-discharging pipe, 103-water inlet pipe, 104-water outlet pipe, 105-condenser body, 106-inner pipe, 107-outer supporting pipe, 108-condensing wing, 109-wrapping part, 110-condensing rib, 111-supporting rib, 112-condensing hole and 113-heat conducting rod; 201-kettle body, 202-stirring shaft, 203-stirring motor, 204-cavity, 205-insulating layer, 205 a-phenolic aldehyde insulating plate layer, 205 b-inorganic glass fiber layer, 206-rotating shaft, 207-stirring blade, 208-rotating motor and 209-anticorrosive coating.
Detailed Description
One embodiment of the present invention is further explained with reference to fig. 1 to 6.
An apparatus for rectifying and separating ethyl acetate and ethanol azeotrope comprises a condenser I1, a distillation still 2, a reboiler I3, a reboiler II 4, a phase separator 5, a pump I6, a pump II 7, a condenser II 8, a recovery tower 9, a condenser III 10, a reflux tank 11, a pump III 12 and a pump IV 13; the condenser I1, the condenser II 8 and the condenser III 10 respectively comprise a condenser body 105 with a feeding pipe 101, a discharging pipe 102, a water inlet pipe 103, a water outlet pipe 104, a condensation cavity and a condensation pipe, the condensation pipe is of a double-layer pipe structure and comprises an inner pipe 106 and an outer supporting pipe 107, the outer supporting pipe 107 is sleeved outside the inner pipe 106, a plurality of condensation wings 108 which are uniformly distributed according to the circumference are integrally formed on the outer side wall of the inner pipe 106, and a wrapping part 109 for wrapping the condensation wings 108 is arranged on the outer supporting pipe 107; the distillation kettle 2 comprises a kettle body 201, a stirring shaft 202 is arranged in the kettle body 201, a stirring motor 203 is arranged at the top of the kettle body 201, the stirring shaft 202 is driven by the stirring motor 203 to rotate, a cavity 204 is formed in the side wall of the kettle body 201, and a heating inlet pipe and a heating outlet pipe which are communicated with the cavity 204 are arranged outside the kettle body 201; the reaction kettle is characterized in that a heat insulation layer 205 is coated outside the kettle body 201, the cavity 204 is in an annular column shape, a plurality of rotating shafts 206 which are uniformly distributed according to the column shape and extend into the cavity 204 are arranged at the top of the kettle body 201, stirring blades 207 are arranged at the positions, located in the cavity 204, of the rotating shafts 206, and each rotating shaft 206 is driven by a rotating motor 208.
A plurality of condensation wings 108 which are uniformly distributed according to the circumference are integrally formed on the outer side wall of the inner pipe 106 of the condensation pipe, and a wrapping part 109 which wraps the condensation wings 108 is arranged on the outer supporting pipe 107, so that the whole contact area of the condensation pipe can be increased, and the condensation effect is ensured; still 2 drives stirring leaf 207 through setting up rotation axis 206 and rotates for the heating medium in the air carries out good stirring and mixes, thereby ensures the stability of heating medium temperature, with the effect of ensureing to distill.
Further: the stirring blade 207 is helical, and the rotation directions of two adjacent rotating shafts 206 are opposite.
The mixing blade 207 has a spiral shape, and the rotation directions of the two adjacent rotating shafts 206 are opposite to each other, whereby the mixing effect can be further ensured.
Further setting: the heat-insulating layer 205 is coated outside the kettle body 201 by an adhesive.
The distillation still 2 can be easily manufactured by coating the outside of the still body 201 with an adhesive through the heat insulating layer 205.
Further: the heat-insulating layer 205 comprises a phenolic aldehyde heat-insulating plate layer 205a and inorganic glass fiber layers 205b arranged on two sides of the phenolic aldehyde heat-insulating plate layer 205a, the inorganic glass fiber layers 205b are in a structure of a polymer modified cement mortar composite glass fiber felt layer, and the phenolic aldehyde heat-insulating plate layer 205a is connected with the inorganic glass fiber layers 205b through a siloxane modified polyurethane adhesive layer.
The heat-insulating layer 205 comprises a phenolic aldehyde heat-insulating plate layer 205a and an inorganic glass fiber layer 205b, so that the heat-insulating layer 205 can have a good heat-insulating effect, and the heat utilization rate of the distillation kettle 2 is further ensured.
Further: an anti-corrosion coating 209 is sprayed on the outside of the heat-insulating layer 205.
The heat-insulating layer 205 is coated with an anticorrosive coating 209, so that the practical life of the heat-insulating layer 205 can be ensured.
Further: a plurality of fan-shaped condensing ribs 110 which are uniformly distributed along a straight line are arranged on the outer side of the wrapping part 109, and the condensing ribs 110 and the inner pipe 106 are coaxially arranged.
The outside through parcel portion 109 is provided with a plurality of along the straight evenly distributed and fan-shaped flaky condensation muscle 110, and condensation muscle 110 and the coaxial setting of inner tube 106 to ensure the holistic condensation effect of condenser pipe greatly.
Further: a plurality of uniformly distributed support ribs 111 are respectively arranged outside the wrapping part 109 and on two sides of the condensing rib 110, and the support ribs 111 and the condensing wings 108 are distributed in a staggered manner.
Through outside parcel portion 109, and be located and be provided with a plurality of evenly distributed's brace rod 111 respectively on the condensation muscle 110 both sides, the surface area of condenser pipe has also further been improved when brace rod 111 improves parcel portion 109 intensity to the effect and the efficiency of condensation have further been ensured.
Further: the inner tube 106 is made of copper or copper alloy, and the outer support tube 107 is made of aluminum or aluminum alloy.
The thickness of the inner pipe 106 is made as thin as possible by the arrangement of two materials, and the integral strength of the condensation pipe is ensured by the support of the outer support pipe 107, and the cost of the raw material input of the inner pipe 106 is reduced while the condensation effect is ensured.
Further: the condensation wing 108 is provided with a plurality of condensation holes 112 which are uniformly distributed and penetrate through the wrapping part 109, heat conduction rods 113 are inserted into the condensation holes 112, and the heat conduction rods 113 contain heat conduction carbon fibers.
The condensing wing 108 is provided with a plurality of condensing holes 112 which are uniformly distributed and penetrate through the wrapping part 109, and the heat conducting rod 113 is inserted into the condensing holes 112, so that the condensing efficiency of the condensing pipe can be further improved.
Further: the rectification separation method of the device comprises the following steps:
the method comprises the following steps that firstly, crude ester continuously enters a distillation kettle 2 through a condenser I1, the boiling of materials in the distillation kettle 2 is realized under the heating action of a reboiler I3, the boiling point of a ternary azeotrope formed by the ester, alcohol and water and a binary azeotrope formed by the ethyl ester and water is low, after the materials are rectified by the distillation kettle, the top of the distillation kettle is evaporated, the evaporated product enters a reboiler II 4 connected with a recovery tower 9 and is condensed in the reboiler II 4, the condensed liquid enters a phase splitter 5 for phase splitting, the ester phase is sent to the distillation kettle 2 through a pump I6, the water phase enters a recovery working section, the distillation kettle 2 is continuously discharged through a pump II 7 to obtain ethyl acetate, the whole system is closed and emptied after air is exhausted, and the system is kept to operate under a pressurization state;
step two, continuously feeding the wastewater into a recovery tower 9 through a condenser II 8, carrying out reduced pressure distillation in the recovery tower 9 under the heating action of a reboiler II 4, feeding the evaporated material into a condenser III 10 for condensation, feeding the condensate into a reflux tank 11 of the recovery tower 9, connecting the recovery tank with a vacuum system to maintain the vacuum state of the whole system, simultaneously dividing the condensate in the reflux tank 11 into two streams, feeding one stream into the recovery tower 9 through a pump III 12 to maintain the rectification state of the recovery tower 9, extracting the deesterification system, and continuously discharging the wastewater from the kettle of the recovery tower 9 through a pump IV 13;
wherein: in the first step, the steam of the distillate evaporated from the top of the distillation still 2 and entering a reboiler of the recovery tower 9 is used as a heat source of the recovery tower 9 in the second step; in the first step, the heating temperature of the distillation kettle 2 is 100-110 ℃, the tower top temperature is 85-95 ℃, and the system pressure is 85-95 KPa; in the second step, the heating temperature of the recovery tower 9 is 68-78 ℃, the tower top temperature is 35-45 ℃, and the relative vacuum pressure of the system is 65-75 KPa.
The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, so: all equivalent changes made according to the structure, shape and principle of the invention are covered by the protection scope of the invention.
Claims (10)
1. An apparatus for rectifying and separating ethyl acetate and ethanol azeotrope comprises a condenser I (1), a distillation still (2), a reboiler I (3), a reboiler II (4), a phase separator (5), a pump I (6), a pump II (7), a condenser II (8), a recovery tower (9), a condenser III (10), a reflux tank (11), a pump III (12) and a pump IV (13);
the method is characterized in that: the condenser I (1), the condenser II (8) and the condenser III (10) respectively comprise a condenser body (105) with a feeding pipe (101), a discharging pipe (102), a water inlet pipe (103), a water outlet pipe (104), a condensation cavity and a condensation pipe, the condensation pipe is of a double-layer pipe structure and comprises an inner pipe (106) and an outer supporting pipe (107), the outer supporting pipe (107) is sleeved outside the inner pipe (106), a plurality of condensation wings (108) which are uniformly distributed according to the circumference are integrally formed on the outer side wall of the inner pipe (106), and a wrapping part (109) wrapping the condensation wings (108) is arranged on the outer supporting pipe (107);
the distillation kettle (2) comprises a kettle body (201), a stirring shaft (202) is arranged in the kettle body (201), a stirring motor (203) is arranged at the top of the kettle body (201), the stirring motor (203) drives the stirring shaft (202) to rotate, a cavity (204) is formed in the side wall of the kettle body (201), and a heating inlet pipe and a heating outlet pipe which are communicated with the cavity (204) are arranged outside the kettle body (201); the device is characterized in that a heat insulation layer (205) is coated outside the kettle body (201), the cavity (204) is in an annular column shape, a plurality of rotating shafts (206) which are uniformly distributed according to a cylinder and extend into the cavity (204) are arranged at the top of the kettle body (201), stirring blades (207) are arranged at the positions, located in the cavity (204), of the rotating shafts (206), and each rotating shaft (206) is driven by a rotating motor (208).
2. The apparatus for rectification separation of azeotrope of ethyl acetate and ethanol as claimed in claim 1, wherein: the stirring blades (207) are spiral, and the rotating directions of two adjacent rotating shafts (206) are opposite.
3. The apparatus for rectification separation of azeotrope of ethyl acetate and ethanol as claimed in claim 2, wherein: the heat-insulating layer (205) is coated outside the kettle body (201) through an adhesive.
4. The apparatus for rectification separation of azeotrope of ethyl acetate and ethanol as claimed in claim 3, wherein: the heat-insulating layer (205) comprises a phenolic aldehyde heat-insulating plate layer (205a) and inorganic glass fiber layers (205b) arranged on two sides of the phenolic aldehyde heat-insulating plate layer (205a), the inorganic glass fiber layers (205b) are of a structure of a polymer modified cement mortar composite glass fiber felt layer, and the phenolic aldehyde heat-insulating plate layer (205a) is connected with the inorganic glass fiber layers (205b) through a siloxane modified polyurethane adhesive layer.
5. The apparatus for rectification separation of azeotrope of ethyl acetate and ethanol as claimed in claim 4, wherein: an anti-corrosion coating (209) is sprayed on the outside of the heat-insulating layer (205).
6. The apparatus for rectification separation of azeotrope of ethyl acetate and ethanol as claimed in claim 5, wherein: the fan-shaped condensing ribs (110) are uniformly distributed in a straight line mode and are in a fan-shaped sheet shape, and the condensing ribs (110) and the inner pipe (106) are arranged coaxially.
7. The apparatus for rectification separation of azeotrope of ethyl acetate and ethanol as claimed in claim 6, wherein: a plurality of uniformly distributed support ribs (111) are respectively arranged outside the wrapping part (109) and on two sides of the condensation rib (110), and the support ribs (111) and the condensation wings (108) are distributed in a staggered manner.
8. The apparatus for rectification separation of azeotrope of ethyl acetate and ethanol as claimed in claim 7, wherein: the inner pipe (106) is made of copper or copper alloy, and the outer supporting pipe (107) is made of aluminum or aluminum alloy.
9. The apparatus for rectification separation of azeotrope of ethyl acetate and ethanol as claimed in claim 8, wherein: the condensation wing (108) is provided with a plurality of condensation holes (112) which are uniformly distributed and penetrate through the wrapping part (109), heat conducting rods (113) are inserted into the condensation holes (112), and the heat conducting rods (113) contain heat conducting carbon fibers.
10. The apparatus for rectification separation of azeotrope of ethyl acetate and ethanol as claimed in claim 1, wherein: the rectification separation method of the device comprises the following steps:
the method comprises the following steps that firstly, crude ester continuously enters a distillation kettle (2) through a condenser I (1), the boiling of materials in the distillation kettle (2) is realized under the heating action of a reboiler I (3) by the materials in the distillation kettle (2), the ternary azeotrope formed by the ester, alcohol and water and the binary azeotrope formed by the ethyl ester and the water are low in boiling point, the distillation kettle is rectified and then the top of the distillation kettle is evaporated, the evaporated product enters a reboiler II (4) connected with a recovery tower (9), the condensation is obtained in the reboiler II (4), the condensate enters a phase separator (5) for phase separation, the ester phase is sent to the distillation kettle (2) through a pump I (6), the water phase enters a recovery working section, the distillation kettle (2) is continuously discharged through a pump II (7) to obtain ethyl acetate, the whole system is closed and emptied after air is removed, and the system is kept to operate under a pressurization state;
step two, continuously feeding the wastewater into a recovery tower (9) through a condenser II (8), carrying out reduced pressure distillation in the recovery tower (9) under the heating action of a reboiler II (4), feeding evaporated materials into a condenser III (10) for condensation, feeding condensate into a reflux tank (11) of the recovery tower (9), connecting the recovery tank with a vacuum system to maintain the vacuum state of the whole system, simultaneously dividing the condensate in the reflux tank (11) into two streams, feeding one stream into the recovery tower (9) through a pump III (12) to maintain the rectification state of the recovery tower (9), feeding the other stream into a de-esterification system, and continuously discharging the wastewater from the kettle of the recovery tower (9) through a pump IV (13);
wherein: in the first step, the steam of the distillate which is distilled out from the top of the distillation kettle (2) and enters a reboiler of the recovery tower (9) is used as a heat source of the recovery tower (9) in the second step; in the first step, the heating temperature of the distillation kettle (2) is 100-110 ℃, the temperature at the top of the distillation kettle is 85-95 ℃, and the system pressure is 85-95 KPa; in the second step, the heating temperature of the recovery tower (9) is 68-78 ℃, the tower top temperature is 35-45 ℃, and the relative vacuum pressure of the system is 65-75 KPa.
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