CN216395282U - Dimethyl ester methanol recovery device - Google Patents
Dimethyl ester methanol recovery device Download PDFInfo
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- CN216395282U CN216395282U CN202122889451.3U CN202122889451U CN216395282U CN 216395282 U CN216395282 U CN 216395282U CN 202122889451 U CN202122889451 U CN 202122889451U CN 216395282 U CN216395282 U CN 216395282U
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Abstract
The utility model relates to a dimethyl ester methanol recovery device, which comprises a feed pipeline communicated with a solvent outlet of a dimethyl ester synthesis kettle and a gas-liquid separator connected with the tail end of the feed pipeline, wherein the top of the gas-liquid separator is provided with a gas outlet, the lower part of the gas-liquid separator is provided with a liquid discharge pipeline, and the dimethyl ester methanol recovery device is technically characterized in that: the gas outlet of the gas-liquid separator is communicated with the tube side inlet of the condenser by a pipeline, the tube side outlet of the condenser is communicated with the inlet of the side wall of the chromatographic column by a pipeline, the top of the chromatographic column is provided with a low-boiling-point organic matter outlet, the bottom of the chromatographic column is connected with a high-purity methanol solution conveying pipeline, the tail end of the high-purity methanol solution conveying pipeline is connected with a recovery tank, the side wall of the top of the gas-liquid separator is provided with a liquid reflux port, and a recovered methanol feeding pipeline is arranged between the liquid reflux port and the recovery tank. The device solves the problem of waste of the solvent methanol solution in the existing dimethyl ester synthesis process, remarkably reduces the use cost of the solvent, greatly reduces the environmental pollution, and is suitable for wide popularization and application.
Description
Technical Field
The utility model relates to a recovery device of solvent methanol, in particular to a dimethyl ester methanol recovery device.
Background
Dimethyl ester is an intermediate for producing imazamox, which belongs to an imidazolinone herbicide, is a side chain amino acid synthesis inhibitor and is applied before or after germination. Has excellent control effect on gramineous weeds and certain broad-leaved weeds in other leguminous plant fields such as soybean fields, such as amaranth, polygonum, chenopodium album, solanum nigrum, xanthium sibiricum, barnyard grass, green bristlegrass, crab grass, millet and the like. In China, 8 hundred million acres of soybeans exist, particularly, the planting area is large in the northeast and eastern areas of inner Mongolia, and imazethapyr is widely used for preventing and controlling grassy weeds in soybean fields.
An important step in the production process of imazamox is the synthesis of dimethyl ester, and the synthesis of dimethyl ester needs to adopt a large amount of methanol solution as a solvent, so that the recovery of a large amount of solvent is very necessary. After the reaction is finished, a large amount of methanol solution is directly discarded, which wastes resources and pollutes the environment, and in addition, the methanol wastewater treatment not only has complex process but also has high price.
Disclosure of Invention
The utility model aims to provide a dimethyl ester methanol recovery device which is reasonable in configuration and reliable in use, solves the problem of waste of a solvent methanol solution in the existing dimethyl ester synthesis process, remarkably reduces the use cost of a solvent, greatly reduces the environmental pollution, and is suitable for wide popularization and application.
The technical scheme of the utility model is as follows:
the utility model provides a dimethyl ester methanol recovery unit, includes the feed line with the solvent outlet intercommunication of dimethyl ester synthetic cauldron, with feed line end-to-end connection's vapour and liquid separator, vapour and liquid separator's top is equipped with gas outlet, and vapour and liquid separator's lower part is equipped with liquid discharge pipeline, and its technical essential is: the gas outlet of the gas-liquid separator is communicated with the tube side inlet of the condenser by a pipeline, the tube side outlet of the condenser is communicated with the inlet of the side wall of the chromatographic column by a pipeline, the top of the chromatographic column is provided with a low-boiling-point organic matter outlet, the bottom of the chromatographic column is connected with a high-purity methanol solution conveying pipeline, the tail end of the high-purity methanol solution conveying pipeline is connected with a recovery tank, the side wall of the top of the gas-liquid separator is provided with a liquid reflux port, and a recovered methanol feeding pipeline is arranged between the liquid reflux port and the recovery tank.
In the dimethyl ester methanol recovery device, the filler of the chromatographic column is activated carbon or molecular sieve or silica gel or zeolite.
Foretell dimethyl ester methanol recovery unit, the condenser adopts the heat preservation condenser, the heat preservation condenser includes vertical casing, locates the helix formula heat exchange tube in the vertical casing, the central line and the horizontal plane of helix formula heat exchange tube are perpendicular, and the gas outlet intercommunication with vapour and liquid separator behind the vertical casing is drawn forth to the upper end of helix formula heat exchange tube, and the lower extreme of helix formula heat exchange tube is drawn forth behind the vertical casing and is linked together with the entry of chromatography column lateral wall, is fixed with a plurality of heat preservation fins between the lateral wall of helix formula heat exchange tube periphery and vertical casing, and every heat preservation fin extends along vertical casing's direction of height, vertical casing's top side is equipped with condensate shell side entry pipeline, and vertical casing's bottom is equipped with the export of condensate shell side.
According to the dimethyl ester methanol recovery device, the recovery tank is internally provided with the dumping baffle which divides the recovery tank into the left recovery chamber and the right recovery chamber, the upper part of the left recovery chamber is communicated with the upper part of the right recovery chamber, the right recovery chamber is wide at the upper part and narrow at the lower part, the tail end of the high-purity methanol solution conveying pipeline is positioned above the right recovery chamber, the side of the right recovery chamber is provided with the cleaning port, and the bottom of the left recovery chamber is communicated with the recovered methanol feeding pipeline.
According to the dimethyl ester methanol recovery device, the conveying pump is arranged on the high-purity methanol solution conveying pipeline, the control valve I is arranged on the front side of the inlet of the conveying pump, the control valve II is arranged on the outlet side of the conveying pump, a bypass pipeline is arranged between the front side of the control valve I and the rear side of the control valve II, and the control valve III is arranged on the bypass pipeline.
The utility model has the beneficial effects that:
the utility model solves the problem of waste of solvent methanol solution in the existing dimethyl ester synthesis process, when the reflux of dimethyl ester reaction liquid is finished, and sampling and tracking the dimethyl ester to reach the standard, the utility model introduces organic matters such as solvent and the like into a gas-liquid separator through a feeding pipeline, separates out the low-boiling point methanol solvent when the boiling point of the methanol is reached, cools the low-boiling point methanol solvent through a condenser, allows cooling liquid to enter a chromatographic column filled with fillers, obtains methanol with higher purity after filtration and separation, is recycled by a recycling tank and then sent to the gas-liquid separator again, and finally sends the high-purity methanol solution to a dimethyl ester production line for recycling. The utility model obviously reduces the use cost of the solvent, greatly reduces the environmental pollution and is suitable for wide popularization and application.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic structural view of a condenser of the present invention;
FIG. 3 is a schematic view of the recovery tank of the present invention.
In the figure: 1. the device comprises a feeding pipeline, a gas-liquid separator, a condenser, a 301 upper end, a 302 heat preservation fin plate, a 303 spiral heat exchange pipe, a 304 condensate shell pass outlet, a 305 lower end, a 306 condensate shell pass inlet pipeline, a 4 chromatographic column, a 5 filler, a 6 control valve I, a 7 delivery pump, a 8 control valve II, a 9 bypass pipeline, a 10 control valve III, a 11 recovery tank, a 1101 right recovery chamber, a 1102 left recovery chamber, a 12 recovered methanol feeding pipeline, a 13 liquid discharge pipeline, a 14 gas outlet, a 15 low boiling point organic matter outlet and a 16 high purity methanol solution delivery pipeline.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings.
As shown in figures 1-3, the dimethyl ester methanol recovery device comprises a feed pipeline 1 communicated with a solvent outlet of a dimethyl ester synthesis kettle, a gas-liquid separator 2 connected with the tail end of the feed pipeline 1, the top of the gas-liquid separator 2 is provided with a gas outlet 14, the lower part of the gas-liquid separator 2 is provided with a liquid discharge pipeline 13, the gas outlet 14 of the gas-liquid separator 2 is communicated with the tube-side inlet of the condenser 3 by a pipeline, the tube pass outlet of the condenser 3 is communicated with the inlet on the side wall of the chromatographic column 4 by a pipeline, the top of the chromatographic column 4 is provided with a low boiling point organic matter outlet 15, the bottom of the chromatographic column 4 is connected with a high-purity methanol solution conveying pipeline 16, the tail end of the high-purity methanol solution conveying pipeline 16 is connected with the recovery tank 11, the side wall of the top of the gas-liquid separator 2 is provided with a liquid return port, and a recovered methanol feeding pipeline 12 is arranged between the liquid return port and the recovery tank 11.
In this embodiment, the filler 5 of the chromatographic column 4 is activated carbon, molecular sieve, silica gel or zeolite.
The condenser 3 adopts a heat-preservation condenser, and has good heat-preservation performance. The heat preservation condenser includes vertical shell, locates the helix type heat exchange tube 303 in the vertical shell, the central line and the horizontal plane of helix type heat exchange tube 303 are perpendicular, and the upper end 301 of helix type heat exchange tube 303 draws forth behind the vertical shell with the gas outlet 14 intercommunication of vapour and liquid separator 2, the lower extreme 305 of helix type heat exchange tube 303 draw forth behind the vertical shell with the entry intercommunication of chromatography column 4 lateral wall, be fixed with a plurality of heat preservation fins 302 between the lateral wall of helix type heat exchange tube 303 periphery and vertical shell, every heat preservation fin 302 extends along vertical shell's direction of height, vertical shell's top side is equipped with condensate shell side entry pipeline 306, and vertical shell's bottom is equipped with condensate shell side export 304. The high-purity methanol solution conveying device is characterized in that a conveying pump 7 is arranged on the high-purity methanol solution conveying pipeline 16, a control valve I6 is arranged on the front side of an inlet of the conveying pump 7, a control valve II 8 is arranged on the outlet side of the conveying pump 7, a bypass pipeline 9 is arranged between the front side of the control valve I6 and the rear side of the control valve II 8, and a control valve III 10 is arranged on the bypass pipeline 9. When the delivery pump 7 breaks down, the control valve III 10 is opened, the bypass pipeline 9 is communicated, the control valve I6 and the control valve II 8 are closed, and the delivery pump 7 is overhauled.
The recovery tank 11 is internally provided with a baffle arranged in a dumping manner, the baffle divides the recovery tank 11 into a left recovery chamber 1102 and a right recovery chamber 1101 with upper parts communicated with each other, the right recovery chamber 1101 is wide at the top and narrow at the bottom, the tail end of the high-purity methanol solution conveying pipeline 16 is positioned above the right recovery chamber 1101, a cleaning port is arranged on the side of the right recovery chamber 1101, and the bottom of the left recovery chamber 1102 is communicated with a recovered methanol feeding pipeline 12. The right recovery chamber 1101 is provided so that the packing 5 of the chromatography column 4 is deposited therein and does not participate in the recovery again.
When the device is used, when the reflux of the dimethyl ester reaction liquid is finished, sampling and tracking the dimethyl ester to reach the standard, organic matters such as a solvent and the like are introduced into a gas-liquid separator 2 through a feeding pipeline 1, the temperature is raised to the boiling point of the methanol, the low-boiling-point methanol solvent is separated, the methanol solvent is cooled through a condenser 3, the collected methanol solvent is filtered and separated through a chromatographic column 4 filled with a filler 5 to obtain the methanol with higher purity, the methanol is recovered through a recovery tank 11 and then sent to the gas-liquid separator 2 again, and the methanol solution with high purity is finally sent to a dimethyl ester production line for recovery and reuse.
The embodiments of the present invention have been described in detail, but the description is only for the preferred embodiments of the present invention and should not be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the scope of the utility model are also within the scope of the present patent.
Claims (5)
1. The utility model provides a dimethyl ester methanol recovery unit, includes the feed line with the solvent outlet intercommunication of dimethyl ester synthetic cauldron, with feed line end connection's vapour and liquid separator, vapour and liquid separator's top is equipped with gas outlet, and vapour and liquid separator's lower part is equipped with liquid discharge pipeline, its characterized in that: the gas outlet of the gas-liquid separator is communicated with the tube side inlet of the condenser by a pipeline, the tube side outlet of the condenser is communicated with the inlet of the side wall of the chromatographic column by a pipeline, the top of the chromatographic column is provided with a low-boiling-point organic matter outlet, the bottom of the chromatographic column is connected with a high-purity methanol solution conveying pipeline, the tail end of the high-purity methanol solution conveying pipeline is connected with a recovery tank, the side wall of the top of the gas-liquid separator is provided with a liquid reflux port, and a recovered methanol feeding pipeline is arranged between the liquid reflux port and the recovery tank.
2. The dimethyl ester methanol recovery device of claim 1, wherein: the filler of the chromatographic column is active carbon or molecular sieve or silica gel or zeolite.
3. The dimethyl ester methanol recovery device of claim 1, wherein: the condenser adopts the heat preservation condenser, the heat preservation condenser includes vertical casing, locates the helix type heat exchange tube in the vertical casing, the central line and the horizontal plane of helix type heat exchange tube are perpendicular, draw forth vertical casing back with vapour and liquid separator's gas outlet intercommunication in the upper end of helix type heat exchange tube, draw forth vertical casing back with the entry intercommunication of chromatography column lateral wall the lower extreme of helix type heat exchange tube, be fixed with a plurality of heat preservation finned plates between the lateral wall of helix type heat exchange tube periphery and vertical casing, every heat preservation finned plate extends along vertical casing's direction of height, vertical casing's top side is equipped with condensate shell side entry pipeline, and vertical casing's bottom is equipped with the export of condensate shell side.
4. The dimethyl ester methanol recovery device of claim 1, wherein: the recovery tank is internally provided with a left recovery chamber and a right recovery chamber which are arranged in a dumping manner, the left recovery chamber and the right recovery chamber are communicated with the upper part of the recovery tank through the baffles, the right recovery chamber is wide at the top and narrow at the bottom, the tail end of the high-purity methanol solution conveying pipeline is positioned above the right recovery chamber, a cleaning port is arranged on the side of the right recovery chamber, and the bottom of the left recovery chamber is communicated with a recovered methanol feeding pipeline.
5. The dimethyl ester methanol recovery device of claim 1, wherein: the high-purity methanol solution conveying pipeline is provided with a conveying pump, a control valve I is arranged on the front side of an inlet of the conveying pump, a control valve II is arranged on the side of an outlet of the conveying pump, a bypass pipeline is arranged between the front side of the control valve I and the rear side of the control valve II, and a control valve III is arranged on the bypass pipeline.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122889451.3U CN216395282U (en) | 2021-11-24 | 2021-11-24 | Dimethyl ester methanol recovery device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122889451.3U CN216395282U (en) | 2021-11-24 | 2021-11-24 | Dimethyl ester methanol recovery device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN216395282U true CN216395282U (en) | 2022-04-29 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202122889451.3U Active CN216395282U (en) | 2021-11-24 | 2021-11-24 | Dimethyl ester methanol recovery device |
Country Status (1)
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|---|---|
| CN (1) | CN216395282U (en) |
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2021
- 2021-11-24 CN CN202122889451.3U patent/CN216395282U/en active Active
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