CN221014526U - Device for preparing ethyl acetate by reaction rectification method - Google Patents
Device for preparing ethyl acetate by reaction rectification method Download PDFInfo
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- CN221014526U CN221014526U CN202322648320.5U CN202322648320U CN221014526U CN 221014526 U CN221014526 U CN 221014526U CN 202322648320 U CN202322648320 U CN 202322648320U CN 221014526 U CN221014526 U CN 221014526U
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- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 title claims abstract description 177
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 67
- 238000000034 method Methods 0.000 title claims abstract description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 176
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 123
- 238000007670 refining Methods 0.000 claims abstract description 36
- 238000000605 extraction Methods 0.000 claims abstract description 32
- 238000010438 heat treatment Methods 0.000 claims abstract description 32
- 238000011084 recovery Methods 0.000 claims description 26
- 238000000066 reactive distillation Methods 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 238000005303 weighing Methods 0.000 claims description 7
- 230000002378 acidificating effect Effects 0.000 claims description 4
- 239000011347 resin Substances 0.000 claims description 4
- 229920005989 resin Polymers 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 238000007086 side reaction Methods 0.000 abstract description 3
- 238000004821 distillation Methods 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 239000012535 impurity Substances 0.000 description 7
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 125000004122 cyclic group Chemical group 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- WFDIJRYMOXRFFG-UHFFFAOYSA-N acetic acid anhydride Natural products CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- BJBUTJQYZDYRMJ-UHFFFAOYSA-N Kaempferol 3,7-dimethyl ether Chemical compound C=1C(OC)=CC(O)=C(C(C=2OC)=O)C=1OC=2C1=CC=C(O)C=C1 BJBUTJQYZDYRMJ-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 230000032050 esterification Effects 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000005191 phase separation Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- JPUHCPXFQIXLMW-UHFFFAOYSA-N aluminium triethoxide Chemical compound CCO[Al](OCC)OCC JPUHCPXFQIXLMW-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- CCGKOQOJPYTBIH-UHFFFAOYSA-N ethenone Chemical compound C=C=O CCGKOQOJPYTBIH-UHFFFAOYSA-N 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000011973 solid acid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model relates to a device for preparing ethyl acetate by a reaction rectifying method, which comprises a heat conducting oil heating system, a reaction rectifying tower, an extraction tower communicated with the top of the reaction rectifying tower, a refining tower communicated with the top of the extraction tower, a light component removing tower communicated with the bottom of the refining tower, and a heavy component removing tower communicated with the bottom of the light component removing tower, wherein ethyl acetate flowing out from the top of the heavy component removing tower is a target product; the reaction rectifying tower sequentially comprises a rectifying section, a reaction section, a stripping section and a tower kettle from top to bottom; the upper part of the reaction section is communicated with a preheated acetic acid tank, and the lower part of the reaction section is communicated with a preheated ethanol tank. The heat-conducting oil heating system forms a first heat-conducting oil heating cycle with the reaction section and the stripping section, and forms a second heat-conducting oil heating cycle and a third heat-conducting oil heating cycle with the acetic acid tank and the ethanol tank respectively. Compared with the prior art, the ethyl acetate prepared by the device has high purity and less side reaction.
Description
Technical Field
The utility model relates to the technical field of chemical industry, in particular to a device for preparing ethyl acetate by a reaction rectifying method.
Background
Ethyl acetate is an important organic compound, and is widely used in paints and inks as an organic solvent, as a cleaning agent in the textile industry, as a fragrance extractant for specially modified alcohols in the food industry, and as an extractant for pharmaceutical processes and organic acids. Ethyl acetate is also a raw material for the manufacture of dyes, pharmaceuticals and fragrances.
The preparation method of the ethyl acetate comprises the following steps:
1. The direct esterification method is a main process route for domestic industrial production of ethyl acetate. Acetic acid and ethanol are used as raw materials, sulfuric acid is used as a catalyst to be directly esterified to obtain ethyl acetate, and the ethyl acetate is dehydrated, fractionated and refined to obtain a finished product.
2. Acetaldehyde condensation method: and (3) taking aluminum alkyl as a catalyst, and carrying out condensation reaction on acetaldehyde to generate ethyl acetate. The technology is mostly adopted in the foreign industrial production.
3. Ethylene and acetic acid are directly esterified to generate ethyl acetate. Ethyl acetate may also be prepared by reacting acetic acid, acetic anhydride or ketene with ethanol; can also be produced by the reaction of two molecules of acetaldehyde under the catalysis of aluminum ethoxide. In addition, ethyl acetate is also a byproduct in the industrial production of acetic acid by butane oxidation.
The ethyl acetate prepared by the reaction rectification method is a novel separation process with wide application prospect. The chemical reaction and the rectification separation process are completed simultaneously in the catalytic rectification tower. The method overcomes the defect that when a sulfuric acid catalyst is used, ethanol and acetic acid can only be added into a tower kettle, and the content of alcohol in crude ester obtained from the tower top is high. There is a reported process for preparing ethyl acetate by catalytic distillation, as disclosed in patent CN102134191a, in which acetic acid and ethanol are used to perform catalytic reaction in a catalytic distillation tower, crude ester with low alcohol content (ethanol content is 0.02 wt%) is obtained at the top of the tower, so that energy consumption for refining the subsequent crude ester is reduced, however, because the ethanol is placed in the tower kettle to be heated in this technology, there is a great heat loss in heat transfer, and the purity of the finally obtained ethyl acetate product is not higher (purity is not less than 99.95%).
Disclosure of utility model
The utility model aims to overcome the defects of the prior art and provide a device for preparing ethyl acetate by a reactive distillation method.
The aim of the utility model can be achieved by the following technical scheme:
The technical scheme of the utility model is to provide a device for preparing ethyl acetate by a reaction rectification method, which comprises a reaction rectification tower, an extraction tower communicated with the top of the reaction rectification tower, a refining tower communicated with the top of the extraction tower, a light component removing tower communicated with the bottom of the refining tower, and a heavy component removing tower communicated with the bottom of the light component removing tower, wherein ethyl acetate flowing out of the top of the heavy component removing tower is a target product;
wherein the reaction rectifying tower sequentially comprises a rectifying section, a reaction section, a stripping section and a tower kettle from top to bottom;
the upper part of the reaction section is communicated with a preheated acetic acid tank, and the lower part of the reaction section is communicated with a preheated ethanol tank.
In some embodiments, the device for preparing ethyl acetate by the reactive distillation method further comprises a heat conduction oil heating system, wherein the heat conduction oil heating system forms a first heat conduction oil heating cycle with the reaction section and the stripping section, the heat conduction oil heating system forms a second heat conduction oil heating cycle with the acetic acid tank, and the heat conduction oil heating system forms a third heat conduction oil heating cycle with the ethanol tank.
The refining tower, the light component removing tower and the heavy component removing tower are heated in a steam tracing mode.
In some specific embodiments, the device for preparing ethyl acetate by the reactive distillation method further comprises a refined phase-splitting tank communicated with the top of the refining tower, wherein the refined phase-splitting tank comprises an oil phase outlet and a water phase outlet, two branches are also led out from the oil phase outlet, and the two branches are respectively communicated with a rectifying section of the reactive distillation tower and the extraction tower to realize cyclic utilization.
In some embodiments, the device for preparing ethyl acetate by the reactive distillation method further comprises an ethanol recovery tower, wherein the tower bottom of the reactive distillation tower, the tower bottom of the extraction tower and the water phase outlet of the refined phase-splitting tank are all communicated with the ethanol recovery tower, and the ethanol recovery tower is communicated with the ethanol tank to realize cyclic utilization.
The ethanol recovery tower is heated in a steam tracing mode.
In some embodiments, an acetic acid weighing assembly is disposed in the acetic acid tank and an ethanol weighing assembly is disposed in the ethanol tank.
In some embodiments, the reaction section is internally filled with a solid acidic ionic resin.
In some specific embodiments, the stripping section and the reaction section are respectively provided with valves for controlling the temperature in the upper, middle and lower sections.
In some specific embodiments, an extraction feeding tank is further arranged between the rectifying section tower top and the extraction tower, a refining feeding tank is further arranged between the extraction tower top and the refining tower, a distillation tank is arranged between the oil phase outlet end of the refining phase-splitting tank and the rectifying section tower top and between the oil phase outlet end of the refining phase-splitting tank and the extraction feeding tank, a tower kettle buffer tank is arranged between the refining tower kettle and the light component removing tower, a heavy component removing feeding tank is arranged between the light component removing tower kettle and the heavy component removing tower, a product tank is arranged at the top of the heavy component removing tower, and an ethanol recovery tank is arranged between the ethanol recovery tower and the ethanol tank.
In some specific embodiments, the acetic acid tank, the ethanol tank, the extraction feed tank, the refining feed tank, the distillation tank, the tower kettle buffer tank, the weight removal feed tank and the ethanol recovery tank are all provided with feed pumps.
Compared with the prior art, the utility model has the following beneficial effects:
(1) The esterification catalyst generally adopts sulfuric acid, has the defects of strong acid corrosiveness, more side reactions, difficult byproduct treatment, environmental pollution and the like, and the solid acidic ion resin is filled in the reaction section of the reaction rectifying tower, so that the corrosion is low, and the environmental pollution phenomenon is not obvious.
(2) The utility model uses the reactive rectifying tower to carry out the reaction, the solid acid catalyst is filled in the reaction section, the two raw materials are in countercurrent reaction in the reactor, namely, acetic acid flows downwards from top to bottom in a liquid form, ethanol evaporates from bottom to top in a gas form, the chemical reaction balance in the kettle type reaction can be broken, the reaction is carried out more thoroughly, the acetic acid is almost completely converted, and the utilization efficiency of the subsequent rectifying tower is improved.
(3) The ethanol adopts a mode of preheating the lower section of the reaction section by heat conducting oil, so that the heat loss is reduced compared with the mode of heating the ethanol at the tower kettle, the heat conducting oil is used for preheating, meanwhile, the heat source is utilized to the greatest extent, and the ethanol enters the reaction section upwards in a gaseous mode, so that the smooth reaction is ensured; the acetic acid is provided with a heat conduction oil heating system, so that the acetic acid is prevented from crystallizing at low temperature, and a heat source is utilized to the greatest extent.
(4) Raw materials such as acetic acid and ethanol adopt the charge pump feeding, and raw materials acetic acid jar and ethanol jar all adopt weighing module, real time monitoring raw materials gets into the weight of reaction rectifying column, guarantee feeding proportion and stability.
(5) The catalytic reaction rectifying tower adopts a sectional heating mode of a reaction section and a stripping section, is relatively lower than the required temperature of a heating mode of a tower kettle, greatly reduces heat loss and reduces energy consumption.
(6) The redundant ethanol is recycled through the ethanol recycling tower, so that the cost is saved.
Drawings
Fig. 1 is a schematic view of the structure of the device of the present utility model.
The figures are identified as follows:
1 is a reactive distillation column, 1-1 is a distillation section, 1-2 is a reaction section, 1-3 is a stripping section, 1-4 is a column kettle, 2 is an extraction column, 2-1 is an extraction feed tank, 3 is a refining column, 3-1 is a refining feed tank, 3-2 is a column kettle buffer tank, 4 is a light component removal column, 5 is a heavy component removal column, 5-1 is a heavy component removal feed tank, 5-2 is a product tank, 6 is a refined phase separation tank, 6-1 is a distillation tank, 7 is an ethanol recovery column, 7-1 is an ethanol recovery tank, 8 is a heat conducting oil heating system, 8-1 is an acetic acid tank, and 8-2 is an ethanol tank.
Detailed Description
The utility model will now be described in detail with reference to the drawings and specific examples. The present embodiment is implemented on the premise of the technical scheme of the present utility model, and a detailed implementation manner and a specific operation process are given, but the protection scope of the present utility model is not limited to the following examples.
In the following embodiments, unless otherwise specified, functional components or structures are indicated as conventional components or structures adopted in the art to achieve the corresponding functions.
Example 1:
as shown in fig. 1, the device for preparing ethyl acetate by a reaction rectifying method comprises a heat conducting oil heating system 8, a reaction rectifying tower 1 connected with the heat conducting oil heating system 8, an extraction tower 2 communicated with the top of the reaction rectifying tower 1, a refining tower 3 communicated with the top of the extraction tower 2, a light component removing tower 4 communicated with the tower kettle of the refining tower 3, and a heavy component removing tower 5 communicated with the tower kettle of the light component removing tower 4, wherein ethyl acetate flowing out from the top of the heavy component removing tower 5 is ethyl acetate with purity higher than 99%;
Wherein the reactive rectifying tower 1 sequentially comprises a rectifying section 1-1, a reaction section 1-2, a stripping section 1-3 and a tower kettle 1-4 from top to bottom;
The upper part of the reaction section 1-2 is communicated with a preheated acetic acid tank 8-1, and the lower part is communicated with a preheated ethanol tank 8-2.
The heat conduction oil heating system 8 forms a first heat conduction oil heating cycle with the reaction section 1-2 and the stripping section 1-3, the heat conduction oil heating system 8 forms a second heat conduction oil heating cycle with the acetic acid tank 8-1, and forms a third heat conduction oil heating cycle with the ethanol tank 8-2.
In this embodiment, the device for preparing ethyl acetate by reactive distillation further includes a refining phase-splitting tank 6 connected to the top of the refining tower 3, where the refining phase-splitting tank 6 includes an oil phase outlet and a water phase outlet, and two branches are further led out from the oil phase outlet, and are respectively connected to the rectifying section 1-1 of the reactive distillation tower 1 and the extraction tower 2 to realize cyclic utilization.
In this embodiment, the apparatus for preparing ethyl acetate by reactive distillation further includes an ethanol recovery tower 7, where the bottoms 1-4 of the reactive distillation tower 1, the bottoms of the extraction tower 2, and the water phase outlet of the refined phase separation tank 6 are all connected to the ethanol recovery tower 7, and the ethanol recovery tower 7 is connected to the ethanol tank 8-2 to realize cyclic utilization.
In this embodiment, an acetic acid weighing component is disposed in the acetic acid tank 8-1, and an ethanol weighing component is disposed in the ethanol tank 8-2.
In this embodiment, the reaction section 1-2 is internally filled with a solid acidic ion resin.
In this embodiment, the stripping section 1-3 and the reaction section 1-2 are respectively provided with valves for controlling temperatures in upper, middle and lower sections.
In the embodiment, an extraction feeding tank 2-1 is further arranged between the top of the rectifying section 1-1 and the extraction tower 2, a refining feeding tank 3-1 is further arranged between the top of the extraction tower 2 and the refining tower 3, a distillation tank 6-1 is arranged between the oil phase outlet end of the refining phase-splitting tank 6 and the top of the rectifying section 1-1 and between the oil phase outlet end of the refining phase-splitting tank 2-1, a tower kettle buffer tank 3-2 is arranged between the tower kettle of the refining tower 3 and the light component removing tower 4, a heavy component removing feeding tank 5-1 is arranged between the tower kettle of the light component removing tower 4 and the heavy component removing tower 5, a product tank 5-2 is arranged on the top of the heavy component removing tower 5, and an ethanol recovery tank 7-1 is arranged between the ethanol recovery tank 7 and the ethanol tank 8-2.
In this embodiment, the acetic acid tank 8-1, the ethanol tank 8-2, the extraction feed tank 2-1, the purification feed tank 3-1, the distillation tank 6-1, the column bottom buffer tank 3-2, the heavy removal feed tank 5-1, and the ethanol recovery tank 7-1 are all provided with feed pumps.
Example 2:
as shown in fig. 1, a process for preparing ethyl acetate by reactive distillation is provided, which is based on the apparatus of the above example 1, and includes the following steps:
(1) Acetic acid tank 8-1 to 35 ℃ is preheated by conduction oil heating system 8 to prevent acetic acid crystallization, meanwhile conduction oil is utilized to the greatest extent, acetic acid is introduced from the upper part of reaction section 1-2 of reaction rectifying tower 1 to the greatest extent, ethanol is introduced from the lower part, the mol ratio of ethanol to acetic acid is 1.2:1, the reflux ratio of the top of the tower is 0.5:1, the temperature of stripping section 1-3 is controlled to 90 ℃, the upper section temperature of reaction section 1-2 is controlled to 92 ℃, the middle section temperature of reaction section 1-2 is controlled to 91 ℃, the lower section temperature of reaction section 1-2 is controlled to 90 ℃, the tower pressure is 0.08MPa, crude ethyl acetate a, water, trace acetic acid and trace ethanol are obtained, enter extraction feeding tank 2-1 from the top of rectifying section 1-1, unreacted water, acetic acid and ethanol enter ethanol recovery tower 7 from tower kettle 1-4 to carry out rectification, normal pressure and temperature are 92 ℃, ethanol obtained by rectification flows into ethanol recovery tank 7-1 from the top of ethanol recovery tower 7, and the ethanol is periodically recovered to be fed into preheated ethanol tank 8-2 for recycling.
(2) Ethyl acetate a and water in the extraction feed tank 2-1 enter from the middle lower part of the extraction tower 2 through a feed pump, meanwhile, water continuously enters the extraction tower 2, ethyl acetate a is washed by countercurrent water, an oil phase extracted from the tower top enters the refining feed tank 3-1, a water phase extracted from the tower bottom enters the ethanol recovery tower 7 for rectification, the temperature of normal pressure is 92 ℃, ethanol liquid extracted from the tower top enters the ethanol recovery tank 7-1, and the recovered ethanol is periodically pumped into the preheated ethanol tank 8-2 through the feed pump, so that the recycling of redundant ethanol is realized.
(3) The oil phase in the refining feeding tank 3-1 is pumped into a refining tower 3 through a feeding pump to refine ethyl acetate, the temperature is 90 ℃ under normal pressure, the ethyl acetate c, the trace ethanol and the trace water are extracted from the tower top and enter a refining phase-splitting tank 6 through ternary azeotropy of ethyl acetate, ethanol and water, and the refined ethyl acetate b at the tower bottom enters a tower bottom buffer tank 3-2 to wait for further purification.
(4) Separating oil from water in the refined phase-splitting tank 6-1, feeding the oil phase at the top of the tower into a rectifying tank 6-1 through a feed pump, feeding a part of the oil phase into a rectifying section 1-1 as reflux liquid for reactive rectification, feeding a part of the oil phase into an extraction tower feed tank 2-1, and performing secondary extraction;
the water phase at the tower bottom is pumped into an ethanol recovery tower 7 through a feed pump for rectification, the temperature is 92 ℃ under normal pressure, ethanol liquid extracted from the tower top enters an ethanol recovery tank 7-1, and the recovered ethanol is pumped into a preheated ethanol tank 8-2 through the feed pump at regular intervals, so that the recycling of the redundant ethanol is realized.
(5) Ethyl acetate b in the tower kettle buffer tank 3-2 enters the light component removing tower 4 through a feed pump to remove light component and purify, the temperature is 75 ℃ under normal pressure, light component impurities (impurities with low boiling point) are extracted from the tower top, and the tower kettle is mainly higher-purity ethyl acetate d which enters the heavy component removing feed tank 5-1.
(6) Ethyl acetate d in the heavy-removal feeding tank 5-1 enters the heavy-removal tower 5 through a feeding pump to carry out rectification and purification, the temperature is 95 ℃ under normal pressure, ethyl acetate e products with high purity extracted from the tower top enter the product tank 5-2, and impurities with heavy components (impurities with high boiling point) are extracted from the tower bottom.
The purity of the ethyl acetate e obtained was 99.99%, the acetic acid content was 0.00015%, the ethanol content was 0.004%, and the water was 0.004%.
Example 3:
Most of the same as in example 2, except that in step (1), the molar ratio of ethanol to acetic acid was 1.05:1, the reflux ratio at the top of the column was 1:1, and the column pressure was 0.1MPa.
Ethyl acetate e with purity of 99.99%, acetic acid content of 0.00018%, ethanol content of 0.003% and water of 0.004% was obtained.
Example 4:
Compared with the embodiment 2, the method is the same in most parts, and the difference is that in the step (1), the molar ratio of ethanol to acetic acid is 1.1:1, the reflux ratio of the tower top is 1.5:1, the temperature of a stripping section 1-3 is controlled to 91 ℃, the temperature of the upper section of a reaction section 1-2 is controlled to 93 ℃, the temperature of the middle section of the reaction section 1-2 is controlled to 93 ℃, the temperature of the lower section of the reaction section 1-2 is controlled to 92 ℃, and the tower pressure is 0.09MPa;
in the step (1), the step (2) and the step (4), the temperature in the ethanol recovery tower 7 is 93 ℃;
In the step (3), the temperature in the refining tower 3 is 91 ℃;
in the step (5), the temperature in the light component removal tower 4 is 76 ℃;
in the step (6), the temperature in the weight loss column 5 was 97 ℃.
Ethyl acetate e with 99.99% purity, acetic acid content 0.0002%, ethanol content 0.004% and water 0.004% was obtained.
Examples 2-4 were subjected to synthesis, multiple extractions (removal of water and ethanol), purification (removal of small amounts of ethanol and water in the form of ternary azeotropes), light removal (removal of light component impurities), and heavy removal (removal of heavy component impurities) to prepare ethyl acetate of high purity (purity greater than 99.99%). The produced side reaction impurities are very few, the reaction effect is good, the acetic acid content at the top of the tower is controlled within 0.002%, the ethanol content is 0.003% -0.004%, the water content is 0.004%, and the purity of the ethyl acetate is more than 99.99%.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present utility model. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present utility model is not limited to the above-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present utility model.
Claims (10)
1. The device for preparing the ethyl acetate by the reaction rectification method is characterized by comprising a reaction rectification tower (1), an extraction tower (2) communicated with the top of the reaction rectification tower (1), a refining tower (3) communicated with the top of the extraction tower (2), a light component removing tower (4) communicated with the tower kettle of the refining tower (3), and a heavy component removing tower (5) communicated with the tower kettle of the light component removing tower (4), wherein the ethyl acetate flowing out of the top of the heavy component removing tower (5) is a target product;
Wherein the reaction rectifying tower (1) comprises a rectifying section (1-1), a reaction section (1-2), a stripping section (1-3) and a tower kettle (1-4) from top to bottom in sequence;
the upper part of the reaction section (1-2) is communicated with a preheated acetic acid tank (8-1), and the lower part of the reaction section is communicated with a preheated ethanol tank (8-2).
2. The device for preparing ethyl acetate by using the reactive distillation method according to claim 1, further comprising a conduction oil heating system (8), wherein the conduction oil heating system (8) forms a first conduction oil heating cycle with the reaction section (1-2) and the stripping section (1-3), the conduction oil heating system (8) forms a second conduction oil heating cycle with the acetic acid tank (8-1), and the conduction oil heating system (8) forms a third conduction oil heating cycle with the ethanol tank (8-2).
3. The device for preparing ethyl acetate by using the reactive distillation method according to claim 2, further comprising a refining phase-splitting tank (6) communicated with the top of the refining column (3), wherein the refining phase-splitting tank (6) comprises an oil phase outlet and a water phase outlet, and two branches are also led out from the oil phase outlet and are respectively communicated with a rectifying section (1-1) of the reactive distillation column (1) and the extraction column (2).
4. A device for preparing ethyl acetate by a reactive distillation method according to claim 3, wherein the device for preparing ethyl acetate by a reactive distillation method further comprises an ethanol recovery tower (7), and the ethanol recovery tower (7) is communicated with the ethanol tank (8-2).
5. The device for preparing ethyl acetate by using the reaction and rectification method according to claim 4, wherein the tower kettles (1-4) of the reaction and rectification tower (1), the tower kettles of the extraction tower (2) and the water phase outlet of the refining phase-splitting tank (6) are all communicated with the ethanol recovery tower (7).
6. The apparatus for preparing ethyl acetate by using the reactive distillation method according to claim 1, wherein an acetic acid weighing assembly is provided in the acetic acid tank (8-1).
7. The apparatus for preparing ethyl acetate by using the reactive distillation method according to claim 1, wherein an ethanol weighing assembly is arranged in the ethanol tank (8-2).
8. The apparatus for preparing ethyl acetate by using a reactive distillation process according to claim 1, wherein the inside of the reaction section (1-2) is filled with a solid acidic ion resin.
9. The apparatus for preparing ethyl acetate by a reactive distillation process according to claim 1, wherein the stripping section (1-3) is provided with valves for controlling temperatures in upper, middle and lower three sections.
10. The apparatus for preparing ethyl acetate by using a reactive distillation process according to claim 1, wherein the reaction sections (1-2) are respectively provided with valves for controlling temperatures in upper, middle and lower sections.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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