CN111099997A - Ethyl ester production device - Google Patents
Ethyl ester production device Download PDFInfo
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- CN111099997A CN111099997A CN201911364633.XA CN201911364633A CN111099997A CN 111099997 A CN111099997 A CN 111099997A CN 201911364633 A CN201911364633 A CN 201911364633A CN 111099997 A CN111099997 A CN 111099997A
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- esterification
- tower
- ethyl ester
- kettle
- air duct
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses an ethyl ester production device, which comprises an esterification tower, wherein a gas guide pipe on the esterification tower is made of Ha's B2, two ends of the gas guide pipe are formed into elbows, a flow plate on a catcher is made of Ha's B2, a rotational flow plate is of an injection type tower plate structure and is arranged at a large flange of an upper end enclosure of the catcher, materials generate rotation and centrifugal motion when passing through blades in a vapor-liquid entrainment mode, and a vapor phase enters the esterification tower through the gas guide pipe, so that gas-liquid separation is realized. The invention upgrades the material of the air duct, the rotational flow plate and the sampling tube which are easy to corrode, the material is changed from 316L to Ha's B2, and the structural form of the air duct is changed from the original dried small shrimp elbow to a forming elbow, so that the air flow can uniformly and stably pass through, the device can stably run for a long period, the energy consumption can be reduced, the environmental protection pressure is reduced, and the production is safer.
Description
Technical Field
The invention belongs to the technical field of esterification tower equipment, and particularly relates to an ethyl ester production device.
Background
In the ethyl ester production process, excessive acetic acid and ethanol are heated under the action of catalyst sulfuric acid to carry out esterification reaction, concentrated sulfuric acid is used as a catalyst in the process, the corrosion to equipment is serious, since the ethyl ester device is put into operation, the material of an air duct, a rotational flow plate and a sampling tube of an esterification tower is 316L under the condition of high-load operation, the erosion corrosion is serious, and the corrosion has great influence on the device, mainly in the following three aspects:
1. equipment corrosion leakage causes failure shutdown, and stable and continuous operation of the device is influenced;
2. after the gas-guide tube is corroded, the contact area of metal and sulfuric acid is increased, so that the concentrated sulfuric acid catalyst is inactivated, the conversion rate is reduced, the consumption of the catalyst is increased, and the operation period of the device is shortened;
3. the corrosion leakage leads to the volatilization and diffusion of ethyl ester, causes the VOC concentration to rise, and the maintenance of stopping because of corroding to bring simultaneously needs to wash the replacement to produce washing wastewater, esterification kettle draws the material number of times to increase and produces the waste residue along with increasing, brings the pressure for environmental protection and handles.
Chinese patent discloses an ethyl acetate esterification reaction tower with a heater, application number CN200410089417.6, its technical scheme mainly is: the reaction kettle is internally provided with a U-shaped heater which is a U-shaped heating tube bundle and is arranged in the kettle in a shape like a Chinese character '#'. The technical effects are as follows: the heat transfer efficiency is improved, the reaction kinetic heat distribution of the reactor is improved, and the steam unit consumption is reduced, but the U-shaped heater is made of 316L, so that the problem of corrosion also exists after long-term operation.
Disclosure of Invention
The invention aims to overcome the technical problems and provide an ethyl ester production device.
In order to achieve the purpose, the invention adopts the following technical scheme:
an ethyl ester production device comprises an esterification kettle, a catcher, a rotational flow plate, an air guide pipe, an esterification tower condenser, an esterification reflux tank and an esterification reflux pump. Excessive acetic acid and ethanol enter the esterification kettle to carry out esterification reaction under the action of catalyst sulfuric acid, ethyl acetate, water and reaction liquid in the esterification kettle generated by the reaction enter the catcher in a vapor-liquid entrainment mode to be separated, wherein a catalyst such as concentrated sulfuric acid with a high boiling point returns to the esterification kettle from the bottom of the catcher, ester, water and alcohol with a low boiling point in a product form a binary or ternary azeotrope, enter the esterification tower from the top through the gas guide tube to be rectified and purified, materials are evaporated from the top of the tower, an ester water layer is formed after passing through the esterification tower condenser to the esterification reflux tank, a bottom water phase is introduced to an ethyl ester waste water tank by using a layered interface liquid level meter, an upper ester phase enters the esterification reflux pump, after the upper ester phase comes out of the esterification reflux pump, part of the upper ester phase is used for reflux in the tower top and the tower, and the rest of the upper ester phase is introduced to an ethyl ester crude, ensuring that the water and the ester are fully separated and then enter the next working procedure.
Furthermore, the material of the air duct adopts Ha's B2.
Furthermore, both ends of the air duct are formed elbows.
Furthermore, the rotational flow plate is of a jet type tower plate structure and is arranged at a large flange of the upper end enclosure of the catcher, materials generate rotation and centrifugal motion when passing through the blades in a vapor-liquid entrainment mode, absorption liquid is uniformly distributed to each blade through the middle blind plate to form a thin liquid layer, the thin liquid layer and the rotating upward air flow form rotation and centrifugal effects, concentrated sulfuric acid with high boiling point and high density is sprayed into fine liquid drops, the fine liquid drops are thrown to the wall of the device and then return to the esterification kettle for reuse through the potential difference, and a vapor phase enters the esterification tower through the air guide pipe.
Furthermore, the material of the rotational flow plate adopts Ha's B2.
Furthermore, an inserted sampling tube is installed at the top of the esterification kettle and used for sampling and analyzing reaction kettle liquid.
Further, the sampling tube is inserted into the bottom of the esterification kettle from the top of the esterification kettle to 40cm in the form of an inner insertion tube through welding.
Furthermore, the sampling tube is made of Ha's B2.
The invention upgrades the material of the air duct, the rotational flow plate and the sampling tube which are easy to corrode, the material is changed from 316L to Ha's B2, and the structure of the air duct is changed from the original dried shrimp elbow to the forming elbow, so that the air flow can uniformly and stably pass through, the device can stably run for a long period, the energy consumption can be reduced, the environmental protection pressure can be reduced, and the production is safer.
Drawings
FIG. 1: the invention discloses a production process flow schematic diagram of an ethyl ester production device.
FIG. 2: the structure of the rotational flow plate is shown schematically.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and examples.
The first embodiment is as follows:
as shown in figure 1, the ethyl ester production device comprises an esterification kettle, a catcher, a rotational flow plate, an air duct, an esterification tower condenser, an esterification reflux tank and an esterification reflux pump. Excessive acetic acid and ethanol enter the esterification kettle to carry out esterification reaction under the action of catalyst sulfuric acid, ethyl acetate, water and reaction liquid in the esterification kettle generated by the reaction enter the catcher in a vapor-liquid entrainment mode to be separated, wherein a catalyst such as concentrated sulfuric acid with a high boiling point returns to the esterification kettle from the bottom of the catcher, low boiling point (ester, water) and alcohol in a product form a binary or ternary azeotrope, the binary or ternary azeotrope enters the esterification tower from the top through the gas-guide tube to be rectified and purified, the material is evaporated from the top of the tower, the material passes through the condenser of the esterification tower to form an ester water layer in the esterification reflux tank, a bottom water phase is introduced to an ethyl ester waste water tank by using a layered interface level meter, an upper ester phase enters the esterification reflux pump, after the material exits from the esterification reflux pump, part of the upper ester phase is used for reflux in the top of the tower and in the tower, and the rest of the upper ester phase is, ensuring that the water and the ester are fully separated and then enter the next working procedure.
Preferably, the air duct is made of Ha's B2, and two ends of the air duct are formed into bends.
As shown in fig. 2, the rotational flow plate is of a jet-type tower plate structure and is installed at a large flange of the upper head of the catcher, the material generates rotation and centrifugal motion when passing through the blades 1 in a vapor-liquid entrainment mode, the absorption liquid is uniformly distributed to each blade 1 through the middle blind plate to form a thin liquid layer, the thin liquid layer and the rotating upward air flow form rotation and centrifugal effects, the concentrated sulfuric acid with high boiling point and high density is sprayed into fine liquid drops, the liquid drops are thrown to the wall of the device and then return to the esterification kettle through a potential difference for reuse, and the vapor phase enters the esterification tower through the gas guide tube.
Preferably, the material of the cyclone plate is Ha's B2.
Example two:
the difference from the first embodiment is only that the top of the esterification kettle is provided with a plug-in sampling pipe for sampling and analyzing the reaction kettle liquid.
Preferably, the sampling tube is inserted into the esterification kettle from the top to the bottom of the esterification kettle by welding in the form of an inner insertion tube.
Preferably, the sampling tube is made of Ha's B2.
The following further shows a corrosion comparison experiment for fixing four materials on the outer side (corrosion prone area) of the elbow of the gas guide tube, and the results of the experiment are shown in the following table 1:
table 1: comparative experimental data
| Material of | Weight before experiment (g) | Post-test weight (g) | Amount of Corrosion (g) | Corrosion ratio (%) | Days of experiment |
| 6XN | 88.4125 | 84.7186 | 3.6939 | 4.18 | 180 |
| 6XN welding | 85.0645 | 81.822 | 3.2425 | 3.81 | 180 |
| 316L | 95.83 | 89.8874 | 5.9426 | 6.2 | 180 |
| 316L welding | 89.7435 | 84.7627 | 4.9808 | 5.55 | 180 |
| Hastelloy B2 | 25.1557 | 25.1556 | 0.0001 | 0 | 180 |
| Hardgrove B2 welding | 26.2345 | 26.2343 | 0.0002 | 0 | 180 |
The experimental data in table 1 show that the original equipment body is made of 316L, the half-year corrosion rate is 6.2%, the corrosion rate of the Hashima B2 material is almost 0 and can be ignored, the corrosion resistance of the air guide tube in a severe environment of mixed acid can be better met, the original 316L material with the thickness of 10mm can be completely replaced by the B2 material with the thickness of 5mm, and meanwhile, for saving the cost, the two flanges can be combined by adopting a B2 flanging carbon-added steel loop flange.
After the embodiment is applied, the problem of corrosion and leakage of equipment is solved, and the device can stably and continuously operate; the sulfuric acid is not easy to inactivate, and the operation period is prolonged; waste residues, waste water and waste gas are obviously reduced, and the environmental protection benefit is obvious; the maintenance frequency is obviously reduced.
The inspection result after the applicant runs the present embodiment internally is given below, specifically as follows:
and 5, 14 to 18 in 2019, modifying the airway of the 6# esterification tower. The operation is carried out in 19 days in 5 months, the periodic stop inspection is carried out in 17 days in 7 months, the operation is continuously carried out for 58 days, and the inspection results are as follows: 1. the welding seam and the base metal are observed by naked eyes without corrosion, and the wall thickness measured by a thickness gauge is 4.9-5mm (without corrosion); 2. all welds were colour tested for defects. The air duct of the 6# esterification tower is checked and confirmed again in 9 months, 12 days and 10 months and 10 days respectively, the corrosion condition is good, and the expected effect of the 6# esterification tower is achieved after the material upgrading and tracking.
Finally, it should be noted that: the above embodiments are only used to illustrate the present invention and do not limit the technical solutions described in the present invention; thus, while the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted; all such modifications and variations are intended to be included herein within the scope of this disclosure and the present invention and protected by the following claims.
Claims (8)
1. An ethyl ester production device comprises an esterification kettle, a catcher, a rotational flow plate, an air duct, an esterification tower condenser, an esterification reflux groove and an esterification reflux pump, and is characterized in that excessive acetic acid and ethanol enter the esterification kettle under the action of catalyst sulfuric acid to perform esterification reaction, the ethyl acetate, water and reaction liquid in the esterification kettle generated by the reaction enter the catcher in a vapor-liquid entrainment mode for separation, wherein catalysts such as concentrated sulfuric acid with high boiling point return the esterification kettle from the bottom of the catcher, ester, water and alcohol with low boiling point in the product form binary or ternary azeotrope, enter the esterification tower from the top through the air duct to perform rectification and purification, the material is evaporated from the top of the tower, an ester water layer is formed after passing through the esterification tower condenser to the esterification reflux groove, and a bottom water phase is introduced to an ethyl ester waste water groove by utilizing a layered interface level meter, and the upper ester phase enters the esterification reflux pump, after the upper ester phase comes out of the esterification reflux pump, the rest of the upper ester phase is introduced into an ethyl ester crude ester phase separator for continuous dehydration except that a part of the upper ester phase is used for reflux at the top of the tower and in the tower, and the water and the ester are fully separated and then enter the next procedure.
2. The ethyl ester production apparatus according to claim 1, characterized in that: the material of the air duct adopts Ha's B2.
3. The ethyl ester production apparatus according to claim 1, characterized in that: the two ends of the air duct are formed elbows.
4. The ethyl ester production apparatus according to claim 1, characterized in that: the cyclone plate is of an injection type tower plate structure and is arranged at a large flange of an upper head of the catcher, materials generate rotation and centrifugal motion when passing through the blades in a vapor-liquid entrainment mode, absorption liquid is uniformly distributed to each blade through the middle blind plate to form a thin liquid layer, the thin liquid layer and the rotating upward air flow form rotation and centrifugal effects, concentrated sulfuric acid with high boiling point and high density is sprayed into fine liquid drops, the fine liquid drops are thrown to a wall of the device and then return to the esterification kettle for reuse through a potential difference, and a vapor phase enters the esterification tower through the air duct.
5. The ethyl ester production apparatus according to claim 1, characterized in that: the material of the rotational flow plate adopts Ha's B2.
6. The ethyl ester production apparatus according to claim 1, characterized in that: and an inserted sampling tube is arranged at the top of the esterification kettle and is used for sampling and analyzing reaction kettle liquid.
7. The ethyl ester production apparatus according to claim 6, wherein: the sampling tube is inserted into the bottom of the esterification kettle from the top of the esterification kettle to 40cm in the form of an inner insertion tube by welding.
8. The ethyl ester production apparatus according to claim 7, wherein: the sampling tube is made of Ha's B2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911364633.XA CN111099997A (en) | 2019-12-26 | 2019-12-26 | Ethyl ester production device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911364633.XA CN111099997A (en) | 2019-12-26 | 2019-12-26 | Ethyl ester production device |
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| CN111099997A true CN111099997A (en) | 2020-05-05 |
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| CN201911364633.XA Pending CN111099997A (en) | 2019-12-26 | 2019-12-26 | Ethyl ester production device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116747802A (en) * | 2023-08-22 | 2023-09-15 | 东营市和瑞化学科技有限公司 | Propylene carbonate catalyst separation device and application method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101486642A (en) * | 2009-02-16 | 2009-07-22 | 江门天诚溶剂制品有限公司 | Heat pump production method of ethyl acetate and production apparatus thereof |
| CN202143807U (en) * | 2011-07-16 | 2012-02-15 | 江门天诚溶剂制品有限公司 | Foam destroyer used for producing acetate |
| CN203971583U (en) * | 2014-06-25 | 2014-12-03 | 泰兴金江化学工业有限公司 | A kind of Despumation device of acetate production use |
| CN106220500A (en) * | 2016-08-17 | 2016-12-14 | 泰兴金江化学工业有限公司 | A kind of ethyl acetate production energy-saving equipment |
| CN106478415A (en) * | 2016-08-17 | 2017-03-08 | 泰兴金江化学工业有限公司 | A kind of ethyl acetate energy-saving processing technique |
| CN206858473U (en) * | 2016-08-17 | 2018-01-09 | 泰兴金江化学工业有限公司 | A kind of ethyl acetate production energy-saving equipment |
-
2019
- 2019-12-26 CN CN201911364633.XA patent/CN111099997A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101486642A (en) * | 2009-02-16 | 2009-07-22 | 江门天诚溶剂制品有限公司 | Heat pump production method of ethyl acetate and production apparatus thereof |
| CN202143807U (en) * | 2011-07-16 | 2012-02-15 | 江门天诚溶剂制品有限公司 | Foam destroyer used for producing acetate |
| CN203971583U (en) * | 2014-06-25 | 2014-12-03 | 泰兴金江化学工业有限公司 | A kind of Despumation device of acetate production use |
| CN106220500A (en) * | 2016-08-17 | 2016-12-14 | 泰兴金江化学工业有限公司 | A kind of ethyl acetate production energy-saving equipment |
| CN106478415A (en) * | 2016-08-17 | 2017-03-08 | 泰兴金江化学工业有限公司 | A kind of ethyl acetate energy-saving processing technique |
| CN206858473U (en) * | 2016-08-17 | 2018-01-09 | 泰兴金江化学工业有限公司 | A kind of ethyl acetate production energy-saving equipment |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116747802A (en) * | 2023-08-22 | 2023-09-15 | 东营市和瑞化学科技有限公司 | Propylene carbonate catalyst separation device and application method thereof |
| CN116747802B (en) * | 2023-08-22 | 2023-10-10 | 东营市和瑞化学科技有限公司 | Propylene carbonate catalyst separation device and application method thereof |
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Application publication date: 20200505 |