CN112358397B - 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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- CN112358397B CN112358397B CN202011331299.0A CN202011331299A CN112358397B CN 112358397 B CN112358397 B CN 112358397B CN 202011331299 A CN202011331299 A CN 202011331299A CN 112358397 B CN112358397 B CN 112358397B
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- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 title claims abstract description 72
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims description 5
- 238000004821 distillation Methods 0.000 claims abstract description 44
- 238000011084 recovery Methods 0.000 claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000010992 reflux Methods 0.000 claims abstract description 12
- 238000007599 discharging Methods 0.000 claims abstract description 8
- 239000010410 layer Substances 0.000 claims description 49
- 238000009833 condensation Methods 0.000 claims description 28
- 230000005494 condensation Effects 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 25
- 238000010438 heat treatment Methods 0.000 claims description 22
- 238000004321 preservation Methods 0.000 claims description 16
- 239000003365 glass fiber Substances 0.000 claims description 15
- 238000009413 insulation Methods 0.000 claims description 11
- -1 phenolic aldehyde Chemical class 0.000 claims description 11
- 150000002148 esters Chemical class 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 238000009835 boiling Methods 0.000 claims description 8
- 239000000853 adhesive Substances 0.000 claims description 6
- 230000001070 adhesive effect Effects 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 239000002351 wastewater Substances 0.000 claims description 6
- 238000005260 corrosion Methods 0.000 claims description 5
- 230000032050 esterification Effects 0.000 claims description 4
- 238000005886 esterification reaction 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
- 125000004494 ethyl ester group Chemical group 0.000 claims description 3
- 238000005191 phase separation Methods 0.000 claims description 3
- 229920002635 polyurethane Polymers 0.000 claims description 3
- 239000004814 polyurethane Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 description 16
- 238000004519 manufacturing process Methods 0.000 description 7
- 210000003205 muscle Anatomy 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000002304 perfume Substances 0.000 description 3
- 238000002156 mixing Methods 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
- 150000001242 acetic acid derivatives Chemical class 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
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 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
- 238000000895 extractive distillation Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 239000004434 industrial solvent 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
- 239000012450 pharmaceutical intermediate Substances 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
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 still, 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 a condenser body with a feeding pipe, a discharging pipe, a water inlet pipe, a water outlet pipe, a condensing cavity and a condensing pipe, wherein 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.
Description
Technical Field
The invention belongs to the technical field of rectification of ethyl acetate and ethanol azeotrope, and in particular relates to equipment and a method for rectifying and separating ethyl acetate and ethanol azeotrope.
Background
Ethyl Acetate (EA), also known as Ethyl Acetate, is a branch of the downstream derivative of acetic acid. It belongs to the category of chemical solvents, is an important green organic solvent, has excellent dissolution performance, and is a quick-drying industrial solvent. Ethyl acetate is widely used in the production of polymers such as fibers, rubbers, resins, and pharmaceutical intermediates; can also be used for producing liquid nitrocellulose ink for a copying machine; as fresheners in the textile industry; flavor extractants for use in the food industry as specially modified alcohols; the perfume industry is the most important perfume additive as a component of a perfume accord. In addition, ethyl acetate can also be used as a solvent for adhesives, a diluent for paints, and a raw material for manufacturing medicines and dyes.
The existing ethyl acetate production method mainly adopts an esterification method of acetic acid and ethanol, the ethanol is excessive in the reaction process, the ethanol and water in the obtained ethyl acetate crude product can not meet the requirement of 99.7% of the purity of the superior product of GB/T3728-2007 industrial ethyl acetate, the ethyl acetate and the ethanol are required to be separated and purified again, but the boiling point of the ethyl acetate and the boiling point of the ethanol are only 1 ℃ worse and have azeotropy, so that the production of the high-purity ethyl acetate can not be realized through common rectification. At present, the separation method is carried out by azeotropic distillation and extractive distillation in industry, but the existing condenser and distillation still have unsatisfactory effects, so that the effect of rectification separation is unsatisfactory.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a device rectification separation method for rectifying and separating an azeotrope of ethyl acetate and ethanol.
In order to achieve the above purpose, the present invention provides the following technical solutions: an apparatus for rectifying and separating an azeotrope of ethyl acetate and ethanol comprises a condenser I, a distillation still, 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 both comprise a condenser body with a feeding pipe, a discharging pipe, a water inlet pipe, a water outlet pipe, a condensing cavity and a condensing pipe, wherein 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, the stirring motor 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 kettle is characterized in that the heat preservation layer is coated outside the kettle body, the cavity is in a ring column shape, a plurality of rotating shafts which are uniformly distributed according to columns and extend into the cavity are arranged at the top of the kettle body, stirring blades are arranged at positions of the rotating shafts in the cavity, and each rotating shaft is driven by a rotating motor.
By adopting the technical scheme, the outer side wall of the inner pipe of the condensing pipe is integrally provided with the plurality of condensing wings which are uniformly distributed according to the circumference, and the outer supporting pipe is provided with the wrapping part for wrapping the condensing wings, so that the whole contact area of the condensing pipe can be increased, and the condensing effect is ensured; the distilling still drives the stirring blade to rotate through the rotating shaft, so that heating medium in air is well stirred and mixed, and the stability of the temperature of the heating medium is ensured, so that the distilling effect is ensured.
The invention is further provided with: the stirring blades are spiral, and the rotation directions of two adjacent rotating shafts are opposite.
By adopting the technical scheme, the stirring blade is spiral, and the rotation directions of the two adjacent rotating shafts are opposite, so that the mixing effect can be further ensured.
The invention is further provided with: the heat preservation layer is coated outside the kettle body through an adhesive.
By adopting the technical scheme, the heat preservation 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 provided with: 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, wherein the inorganic glass fiber layers are of a structure of polymer modified cement mortar composite glass fiber silk felt layers, 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 the heat utilization ratio of stills.
The invention is further provided with: and 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 provided with: the outside of parcel portion is provided with a plurality of along straight evenly distributed and fan-shaped flaky condensation muscle, condensation muscle and the coaxial setting of inner tube.
Through adopting foretell technical scheme, the outside of parcel portion is provided with a plurality of along straight evenly distributed and fan-shaped flaky condensation muscle, and condensation muscle and the coaxial setting of inner tube to ensure the holistic condensation effect of condenser pipe greatly.
The invention is further provided with: a plurality of evenly distributed supporting ribs are respectively arranged outside the wrapping part and on two sides of the condensing ribs, and the supporting ribs and the condensing wings are distributed in a staggered mode.
Through adopting foretell technical scheme, be provided with a plurality of evenly distributed's supporting rib respectively on the parcel portion is outside, and lie in the condensation muscle both sides, the supporting rib has also further improved the surface area of condenser pipe when improving parcel portion intensity to condensation effect and efficiency have further been ensured.
The invention is further provided with: the inner tube is made of copper or copper alloy, and the outer support tube is made of aluminum or aluminum alloy.
Through adopting foretell technical scheme, through the setting of two kinds of materials, make 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 the cost that inner tube raw and other materials input has been reduced when guaranteeing the condensation effect.
The invention is further provided with: the condensing wing is provided with a plurality of condensing holes which are uniformly distributed and penetrate through the wrapping part, the condensing holes are inserted with heat conducting rods, and the heat conducting rods contain heat conducting carbon fibers.
Through adopting foretell technical scheme, be provided with a plurality of evenly distributed and run through the condensation hole of parcel portion on the condensation wing, 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 provided with: the rectification separation method of the equipment comprises the following steps:
continuously feeding crude ester into a distillation kettle through a condenser I, boiling the material in the distillation kettle under the heating action of a reboiler I, and because the boiling point of a ternary azeotrope formed by ester, alcohol and water and a binary azeotrope formed by ethyl ester and water is low, distilling the crude ester out of the top of the distillation kettle after rectification by the distillation kettle, feeding the distilled product into a reboiler II connected with a recovery tower, condensing the distilled product in the reboiler II, feeding the condensed product into a phase separator for phase separation, feeding the ester phase into the distillation kettle through a pump I, feeding the water phase into a recovery section, continuously discharging the distillation kettle through the pump II to obtain ethyl acetate, closing the whole system after air is discharged, and keeping the system to run under a pressurized state;
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, condensing the distilled material in a condenser III, 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 parts, feeding one part of condensate into the recovery tower through a pump III to maintain the rectification state of the recovery tower, collecting the other part of condensate out of an esterification system, and continuously discharging the wastewater from the bottom of the recovery tower through a pump IV;
wherein: in the first step, steam of a steam product entering a recovery tower reboiler is distilled out from the top of the distillation kettle and is used as a heat source of the recovery tower in the second step; the heating temperature of the distillation still in the first step is 100-110 ℃, the temperature of the top of the distillation still is 85-95 ℃, and the system pressure is 85-95KPa; 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 65-75KPa.
Drawings
FIG. 1 is a flow chart of the production process of the invention for separating ethyl acetate and ethanol azeotrope by differential pressure distillation;
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 structure of the condenser of the present invention;
FIG. 5 is a schematic view of the condenser tube structure of the condenser of the present invention;
FIG. 6 is a schematic cross-sectional view of a condenser tube of the present invention;
reference numerals and corresponding part names in the drawings: 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 column, 10-condenser III, 11-reflux tank, 12-pump III, 13-pump IV, 101-feed pipe, 102-discharge pipe, 103-feed pipe, 104-outlet pipe, 105-condenser body, 106-inner pipe, 107-outer support pipe, 108-condensing wing, 109-wrapping part, 110-condensing rib, 111-support rib, 112-condensing hole, 113-heat conducting bar; 201-kettle body, 202-stirring shaft, 203-stirring motor, 204-cavity, 205-heat insulation layer, 205 a-phenolic aldehyde heat insulation board layer, 205 b-inorganic glass fiber layer, 206-rotation shaft, 207-stirring blade, 208-rotation motor and 209-anticorrosive coating.
Detailed Description
An embodiment of the present invention will be further described with reference to fig. 1 to 6.
An apparatus for rectifying and separating an 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 feed pipe 101, a discharge pipe 102, a water inlet pipe 103, a water outlet pipe 104, a condensation cavity and a condensation pipe, wherein the condensation pipe is of a double-layer pipe structure and comprises an inner pipe 106 and an outer support pipe 107, the outer support pipe 107 is sleeved outside the inner pipe 106, a plurality of condensation wings 108 uniformly distributed along 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 support pipe 107; the distillation kettle 2 comprises a kettle body 201, wherein 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 kettle is characterized in that an insulating layer 205 is coated outside the kettle body 201, the cavity 204 is in a ring column shape, a plurality of rotating shafts 206 which are uniformly distributed according to columns and extend into the cavity 204 are arranged at the top of the kettle body 201, stirring blades 207 are arranged at positions of the rotating shafts 206 in the cavity 204, and each rotating shaft 206 is driven by a rotating motor 208.
The outer side wall of the inner pipe 106 of the condensing pipe is integrally provided with a plurality of condensing wings 108 which are uniformly distributed along the circumference, and the outer supporting pipe 107 is provided with a wrapping part 109 which wraps the condensing wings 108, so that the whole contact area of the condensing pipe can be increased, and the condensing effect is ensured; the distillation still 2 drives the stirring blade 207 to rotate by arranging the rotating shaft 206, so that heating medium in air is well stirred and mixed, thereby ensuring the stability of the temperature of the heating medium and ensuring the distillation effect.
Further: the stirring blades 207 are spiral, and the rotation directions of the two adjacent rotation shafts 206 are opposite.
The stirring blade 207 is spiral, and the rotation directions of the two adjacent rotation shafts 206 are opposite to each other, whereby the mixing effect can be further ensured.
Further set up: the heat insulation layer 205 is coated on the outer part of the kettle body 201 through an adhesive.
The insulating layer 205 is coated on the outside of the kettle body 201 by an adhesive, so that the manufacturing of the distillation kettle 2 can be facilitated.
Further: the heat insulation layer 205 comprises a phenolic aldehyde heat insulation plate layer 205a and inorganic glass fiber layers 205b arranged on two sides of the phenolic aldehyde heat insulation plate layer 205a, wherein the inorganic glass fiber layers 205b are of a structure of polymer modified cement mortar composite glass fiber silk felt layers, and the phenolic aldehyde heat insulation plate layer 205a and the inorganic glass fiber layers 205b are connected through siloxane modified polyurethane adhesive layers.
Through heat preservation 205 including phenolic aldehyde heat preservation layer 205a, inorganic glass fiber layer 205b to make heat preservation 205 play good heat preservation effect, and then ensure the heat utilization ratio of stills 2.
Further: an anti-corrosion coating 209 is sprayed outside the heat preservation layer 205.
The anti-corrosion coating 209 is sprayed outside the heat preservation layer 205, so that the service life of the heat preservation layer 205 can be ensured.
Further: a plurality of fan-shaped sheet-shaped condensation ribs 110 which are uniformly distributed along the straight line are arranged on the outer side of the wrapping part 109, and the condensation ribs 110 and the inner tube 106 are coaxially arranged.
The outside through parcel portion 109 is provided with a plurality of along 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 supporting ribs 111 are respectively arranged outside the wrapping part 109 and on two sides of the condensing ribs 110, and the supporting ribs 111 and the condensing wings 108 are distributed in a staggered manner.
Through being provided with a plurality of evenly distributed's supporting rib 111 respectively on the outside of parcel portion 109 and being located condensation rib 110 both sides, supporting rib 111 has also further improved the surface area of condenser pipe when improving parcel portion 109 intensity to further ensured effect and the efficiency of condensation.
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.
Through the arrangement of the two materials, the thickness of the inner tube 106 is made as thin as possible, the overall strength of the condensing tube is ensured through the support of the outer supporting tube 107, and the cost of raw material investment of the inner tube 106 is reduced while the condensing effect is ensured.
Further: a plurality of condensing holes 112 which are uniformly distributed and penetrate through the wrapping part 109 are formed in the condensing wing 108, heat conducting rods 113 are inserted into the condensing holes 112, and the heat conducting rods 113 contain heat conducting 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 condensing holes 112 are inserted with heat conducting rods 113, so that the condensing efficiency of the condensing tube can be further improved.
Further: the rectification separation method of the equipment comprises the following steps:
firstly, continuously feeding crude ester into a distillation kettle 2 through a condenser I1, boiling the material in the distillation kettle 2 under the heating action of a reboiler I3, and closing and emptying the whole system after air is discharged because the boiling point of a ternary azeotrope formed by the ester, alcohol and water and a binary azeotrope formed by ethyl ester and water is low, and keeping the system in a pressurized state after the distillation kettle top is distilled, feeding the distilled product into a reboiler II 4 connected with a recovery tower 9, condensing in the reboiler II 4, feeding the condensate into a phase separator 5 for phase separation, feeding the ester phase into the distillation kettle 2 through a pump I6, feeding the water phase into a recovery section, continuously discharging the distillation kettle 2 through a pump II 7;
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, condensing the distilled material into a condenser III 10, 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, dividing the condensate in the reflux tank 11 into two parts, feeding one part of the condensate into the recovery tower 9 through a pump III 12 to maintain the rectification state of the recovery tower 9, collecting the other part of the condensate out of the 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, steam of a steam product entering a reboiler of the recovery tower 9 is distilled out from the top of the distillation kettle 2 and is used as a heat source of the recovery tower 9 in the second step; the heating temperature of the distillation kettle 2 in the first step is 100-110 ℃, the temperature of the top of the tower is 85-95 ℃, and the system pressure is 85-95KPa; 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 65-75KPa.
The above embodiments are only preferred embodiments of the present invention, and are not intended to limit the scope of the present invention in this way, therefore: all equivalent changes in structure, shape and principle of the invention should be covered in the scope of protection of the invention.
Claims (2)
1. An apparatus for rectifying and separating an 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) condenser II (8) and the condenser III (10) 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 condensing cavity and a condensing pipe, wherein the condensing 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 condensing wings (108) 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 condensing wings (108) is arranged on the outer supporting pipe (107);
the distillation kettle (2) comprises a kettle body (201), wherein 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 kettle is characterized in that an insulating layer (205) is coated outside the kettle body (201), the cavity (204) is in a ring column shape, a plurality of rotating shafts (206) which are uniformly distributed according to columns and extend into the cavity (204) are arranged at the top of the kettle body (201), stirring blades (207) are arranged at positions of the rotating shafts (206) in the cavity (204), and each rotating shaft (206) is driven by one rotating motor (208);
a plurality of fan-shaped sheet-shaped condensation ribs (110) which are uniformly distributed along the straight line are arranged on the outer side of the wrapping part (109), and the condensation ribs (110) and the inner tube (106) are coaxially arranged;
a plurality of uniformly distributed supporting ribs (111) are respectively arranged outside the wrapping part (109) and on two sides of the condensing ribs (110), and the supporting ribs (111) and the condensing wings (108) are distributed in a staggered manner;
the inner tube (106) is made of copper or copper alloy, and the outer support tube (107) is made of aluminum or aluminum alloy;
a plurality of condensing holes (112) which are uniformly distributed and penetrate through the wrapping part (109) are formed in the condensing wing (108), heat conducting rods (113) are inserted into the condensing holes (112), and the heat conducting rods (113) contain heat conducting carbon fibers;
the stirring blades (207) are spiral, and the rotation directions of two adjacent rotation shafts (206) are opposite;
the heat preservation layer (205) is coated outside the kettle body (201) through an adhesive;
the heat insulation layer (205) comprises a phenolic aldehyde heat insulation board layer (205 a) and inorganic glass fiber layers (205 b) arranged on two sides of the phenolic aldehyde heat insulation board layer (205 a), wherein the inorganic glass fiber layers (205 b) are of a structure of polymer modified cement mortar composite glass fiber silk felt layers, and the phenolic aldehyde heat insulation board layer (205 a) is connected with the inorganic glass fiber layers (205 b) through a siloxane modified polyurethane adhesive layer;
an anti-corrosion coating (209) is sprayed outside the heat preservation layer (205).
2. The apparatus for separating an ethyl acetate and ethanol azeotrope by rectification as claimed in claim 1, wherein: the rectification separation method of the equipment comprises the following steps:
firstly, continuously feeding crude ester into a distillation kettle (2) through a condenser I (1), boiling the material in the distillation kettle (2) under the heating action of a reboiler I (3), and continuously discharging the material in the distillation kettle (2) through a pump I (6), so as to obtain ethyl acetate, wherein the boiling point of a ternary azeotrope formed by the ester, the alcohol and the water and a binary azeotrope formed by the ethyl ester and the water are low, the top of the distillation kettle is distilled out after the distillation of the distillation kettle, the distilled product enters a reboiler II (4) connected with a recovery tower (9), condensation is obtained in the reboiler II (4), the condensed liquid enters a phase separator (5) for phase separation, the ester phase enters the distillation kettle (2) through a pump I (6), the water phase enters a recovery section, the distillation kettle (2) is continuously discharged through a pump II (7), and the whole system is closed and is emptied after air is discharged, and the system is kept to run under a pressurized state;
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 distilled material into a condenser III (10) for condensation, feeding the condensate into a reflux tank (11) of the recovery tower (9), connecting the reflux tank with a vacuum system to maintain the vacuum state of the whole system, 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), collecting the esterification system, and continuously feeding the wastewater from the kettle of the recovery tower (9) through a pump IV (13);
wherein: in the first step, steam of a distilled product entering a reboiler of a recovery tower (9) is distilled out from the top of a distillation kettle (2) and is used as a heat source of the recovery tower (9) in the second step; the heating temperature of the distillation still (2) in the first step is 100-110 ℃, the tower top temperature is 85-95 ℃, and the system pressure is 85-95KPa; 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 65-75KPa.
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