CN213790030U - 2, 3-dichloro-5-trifluoromethylpyridine continuous rectification device - Google Patents
2, 3-dichloro-5-trifluoromethylpyridine continuous rectification device Download PDFInfo
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- CN213790030U CN213790030U CN202021853120.3U CN202021853120U CN213790030U CN 213790030 U CN213790030 U CN 213790030U CN 202021853120 U CN202021853120 U CN 202021853120U CN 213790030 U CN213790030 U CN 213790030U
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Abstract
The utility model discloses a 2, 3-dichloro-5-trifluoromethylpyridine continuous rectification device, which belongs to the technical field of fine chemical engineering. The utility model provides a 2, 3-dichloro-5-trifluoromethylpyridine continuous rectification device, including the crude storage tank, the middle part at a rectifying still is connected to the crude storage tank, a rectifying still links to each other with light component receiving tank, a material transferring pump is connected with an edulcoration cauldron, a rectifying still links to each other with an edulcoration cauldron, an edulcoration cauldron is connected with secondary material transferring pump, the dropwise add jar is connected at secondary edulcoration cauldron top, secondary edulcoration cauldron is connected at the top of waste water receiving tank, secondary material transferring pump is connected at an edulcoration water knockout drum feed inlet, an edulcoration cauldron is connected at secondary edulcoration water knockout drum middle part, cubic material transferring pump is connected at secondary rectifying still middle part, secondary rectifying still connects at product receiving tank top, the utility model discloses utilize non-intermittent type serialization reaction, reduce personnel's amount of labour, provide stable and low-cost's mode of production.
Description
Technical Field
The utility model relates to a fine chemistry industry technical field especially relates to a 2, 3-dichloro-5-trifluoromethylpyridine continuous rectification device.
Background
The purification mode of the crude product neutralized by 2, 3-dichloro-5-trifluoromethylpyridine at present is to separate a light component from a crude product containing impurities through one batch rectification, chemically remove the impurities from the crude product containing the impurities through a batch impurity removal reaction, obtain the crude product without the impurities after manual layering, and obtain a finished product through secondary batch rectification.
Because the partition operation is intermittent operation, the treatment capacity of intermittent rectification feed quantity is less influenced by the volume of the kettle, heavy components are pressed by a large reflux ratio for collecting light components, and the time is long. Under the general condition, the light component pressing time of one batch rectification needs 36 hours, the product collection also needs about 36 hours, the one-kettle rectification is 10 tons of feeding amount, 7 tons of products are received, continuous sampling is needed in the process to detect the content of finished products, the labor amount of personnel is large, the production period is long, and the production cost is increased.
Disclosure of Invention
The utility model aims at solving the defects of large labor amount, long production period and high cost of personnel in the prior art and providing a 2, 3-dichloro-5-trifluoromethylpyridine continuous rectification device.
In order to achieve the above purpose, the utility model adopts the following technical scheme:
a2, 3-dichloro-5-trifluoromethylpyridine continuous rectification device comprises a crude product storage tank, a primary rectification kettle, a light component receiving tank, a primary impurity removal kettle, a secondary impurity removal kettle, a dripping tank, a secondary rectification kettle, a product receiving tank, a heavy component receiving tank and a wastewater receiving tank, wherein the crude product storage tank is connected to the middle part of the primary rectification kettle through a feed flowmeter, the top part of the primary rectification kettle is connected with the top part of the light component receiving tank, the bottom part of the primary rectification kettle is connected with a primary material transferring pump, a discharge port of the primary material transferring pump is connected with the top part of the primary impurity removal kettle through a bottom flowmeter of the primary rectification kettle, the primary kettle rectification is connected with the top part of the primary impurity removal kettle through a primary rectification condenser and a primary impurity removal condenser, the bottom part of the primary impurity removal kettle is connected with a secondary material transferring pump, the bottom part of the dripping tank is connected to the top part of the secondary impurity removal kettle, the top at the waste water receiving tank is connected through an impurity removal water knockout drum in secondary edulcoration cauldron top, the discharge gate of material pump is changeed to the secondary is connected at the top feed inlet of an impurity removal water knockout drum, the bottom of secondary impurity removal cauldron is connected with the cubic through the impurity removal water knockout drum and is changeed the material pump, the middle part at secondary impurity removal water knockout drum is connected to primary impurity removal cauldron top, the discharge gate of material pump is changeed to the cubic is connected at secondary rectifying still middle part, secondary rectifying still's top is passed through secondary rectifying tower top flow meter and is connected the top at the product receiving tank, the bottom of secondary rectifying still is changeed the top of material pump connection at heavy ends receiving tank through the quartic.
Preferably, the top of rectifying still links to each other with a rectifying condenser import, the top lateral wall of rectifying still links to each other with light component receiving tank through a rectifying tower top flowmeter, a rectifying condenser connects between the connecting pipe of two sets of rectifying tower top flowmeters, the top of rectifying condenser passes through pipe connection once and receives the top of jar at light component.
Preferably, the primary impurity removal kettle and the primary impurity removal condenser are connected in a gas phase mode.
Preferably, the side wall of the bottom of the primary rectifying still is connected with a primary rectifying reboiler, the primary rectifying reboiler is connected with the feed inlet of the primary material transferring pump, and the bottom of the primary rectifying still is connected with the feed inlet of the primary material transferring pump through a conduit.
Preferably, the top of the secondary impurity removal kettle is connected to a discharge port at the bottom of the primary impurity removal water separator, and the wastewater receiving tank is connected to a discharge port at the side wall of the primary impurity removal water separator.
Preferably, the top of secondary rectifying still is connected with the secondary rectification condenser, the top links to each other with product receiving tank top, the top lateral wall of secondary rectifying still passes through secondary rectifying tower top flowmeter and links to each other with product receiving tank top, secondary rectifying tower top flowmeter bottom passes through pipe connection between two sets of secondary rectifying tower top flowmeters.
Preferably, the outlet on the side of the bottom of the secondary rectifying still is connected with a secondary rectifying reboiler, the top of the secondary rectifying reboiler is connected with the feed inlet of the quartic material transferring pump, and the bottom of the secondary rectifying still is connected with the feed inlet of the quartic material transferring pump through a conduit.
Preferably, a primary rectifying tower bottom flowmeter is arranged between the discharge port of the primary material transfer pump and the primary impurity removal kettle, and a secondary tower bottom flowmeter is arranged between the discharge port of the quartic material transfer pump and the heavy component receiving tank.
Compared with the prior art, the utility model provides a 2, 3-dichloro-5-trifluoromethylpyridine continuous rectification device, possesses following beneficial effect:
1. according to the continuous rectifying device for the 2, 3-dichloro-5-trifluoromethylpyridine, the primary impurity removal kettle and the primary impurity removal condenser are connected in a gas phase mode, the primary impurity removal condenser is enabled to flow back to the primary impurity removal kettle, and in order to keep the pressure consistent with the pressure of the two rectifying kettles, the vacuum is connected behind the primary impurity removal condenser.
2. The continuous rectification device for the 2, 3-dichloro-5-trifluoromethylpyridine is connected with an upper inlet of a primary impurity removal kettle through a side port of a secondary impurity removal water separator, is used for supplying sodium hydroxide which is not completely reacted in the secondary impurity removal kettle, and realizes cyclic utilization.
Drawings
Fig. 1 is a schematic structural diagram of a 2, 3-dichloro-5-trifluoromethylpyridine continuous rectification device provided by the utility model.
In the figure: 1. a crude product storage tank; 2. a primary rectifying still; 3. a light component receiving tank; 4. a primary impurity removal kettle; 5. a secondary impurity removal kettle; 6. a dropping tank; 7. a secondary rectifying kettle; 8. a product receiving tank; 9. a heavies receiving tank; 10. a wastewater receiving tank; e1, a primary rectification reboiler; e2, a primary rectification condenser; e3, a primary impurity removal condenser; e4, a secondary impurity removal condenser; e5, a secondary rectification condenser; e6, a secondary rectification reboiler; q1, feed flowmeter; q2, a primary rectification tower top flow meter; q3, a secondary rectification tower bottom flow meter; q4, primary rectification tower bottom flow meter; q5, a secondary rectification tower top flow meter; p1, a primary transfer pump; p2, a secondary transfer pump; p3, a third material transfer pump; p4, a four-time material transferring pump; f1, primary impurity removal water separator; f2, and a secondary impurity removal water separator.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore, should not be construed as limiting the present invention.
Example (b):
referring to fig. 1, a 2, 3-dichloro-5-trifluoromethylpyridine continuous rectification device comprises a crude product storage tank 1, a primary rectification kettle 2, a light component receiving tank 3, a primary impurity removal kettle 4, a secondary impurity removal kettle 5, a dripping tank 6, a secondary rectification kettle 7, a product receiving tank 8, a heavy component receiving tank 9 and a wastewater receiving tank 10, wherein the crude product storage tank 1 is connected with the middle part of the primary rectification kettle 2 through a feed flowmeter Q1, the top part of the primary rectification kettle 2 is connected with the top part of the light component receiving tank 3, the bottom part of the primary rectification kettle 2 is connected with a primary material transfer pump P1, a discharge port of the primary material transfer pump P1 is connected with the top part of the primary impurity removal kettle 4 through a primary rectification tower flowmeter Q4, the primary rectification kettle 2 is connected with the top part of the primary impurity removal kettle 4 through a primary rectification condenser E2 and a primary impurity removal condenser E3, 4 bottoms in the primary impurity removal kettle are connected with secondary material transferring pump P2, 6 bottoms in the dropwise adding tank are connected at the top of secondary impurity removal kettle 5, the top of secondary impurity removal kettle 5 is connected at the top of waste water receiving tank 10 through primary impurity removal water knockout drum F1, the discharge gate of secondary material transferring pump P2 is connected at the top feed inlet of primary impurity removal water knockout drum F1, the bottom of secondary impurity removal kettle 5 is connected with tertiary material transferring pump P3 through secondary impurity removal water knockout drum F2, the middle part of secondary impurity removal water knockout drum F2 is connected at 4 tops in primary impurity removal kettle, the discharge gate of tertiary material transferring pump P3 is connected at 7 middle parts in secondary rectification kettle, secondary rectification 7's top is connected at 8 tops in product rectification receiving tank through secondary tower top flowmeter Q5, secondary rectification kettle 7's bottom is connected at the top of heavy weight component receiving tank 9 through quartic material transferring pump P4.
The top of the primary rectifying still 2 is connected with the inlet of a primary rectifying condenser E2, the side wall of the top of the primary rectifying still 2 is connected with the light component receiving tank 3 through a primary rectifying tower top flowmeter Q2, the primary rectifying condenser E2 is connected between connecting pipes of two groups of primary rectifying tower top flowmeters Q2, and the top of the primary rectifying condenser E2 is connected with the top of the light component receiving tank 3 through a conduit.
The primary impurity removal kettle 4 and the primary impurity removal condenser E3 adopt a gas phase connection mode.
The side wall of the bottom of the primary rectifying still 2 is connected with a primary rectifying reboiler E1, the primary rectifying reboiler E1 is connected with the feed inlet of a primary material transfer pump P1, and the bottom of the primary rectifying still 2 is connected with the feed inlet of a primary material transfer pump P1 through a guide pipe.
The top of the secondary impurity removal kettle 5 is connected with a discharge port at the bottom of the primary impurity removal water separator F1, and the wastewater receiving tank 10 is connected with a discharge port at the side wall of the primary impurity removal water separator F1.
The top of the secondary rectifying still 7 is connected with a secondary rectifying condenser E5, the top is connected with the top of the product receiving tank 8, the top side wall of the secondary rectifying still 7 is connected with the top of the product receiving tank 8 through a secondary rectifying tower top flowmeter Q5, and the bottom of the secondary rectifying tower top flowmeter Q5 is connected between two sets of secondary rectifying tower top flowmeters Q5 through a guide pipe.
The outlet at the bottom side of the secondary rectifying still 7 is connected with a secondary rectifying reboiler E6, the top of the secondary rectifying reboiler E6 is connected with the feed inlet of a quartic material transfer pump P4, and the bottom of the secondary rectifying still 7 is connected with the feed inlet of a quartic material transfer pump P4 through a guide pipe.
A primary rectifying tower bottom flowmeter is arranged between the discharge port of the primary material transfer pump P1 and the primary impurity removing kettle 4, and a secondary tower bottom flowmeter Q3 is arranged between the discharge port of the four-time material transfer pump P4 and the heavy component receiving tank 9.
The working principle is as follows: in the utility model, when in use, the sufficient 2, 3-dichloro-5-trifluoromethylpyridine crude product accumulated in the crude product storage tank 1 before operation is analyzed to form components, the sufficient 10% sodium hydroxide solution is stored in the dropwise adding tank 6, the primary rectification condenser E2 and the secondary rectification condenser E5 are opened to generate condensation circulating water, the full reflux is completely opened at the bottom of the top kettle of the primary rectification kettle 2, the vacuum degree of all equipment is-0.065 MPa, the material is fed into the primary rectification kettle 2 by the mobile flow, the primary rectification reboiler E1 and the secondary rectification reboiler E2 are opened to heat steam, the material feeding is stopped when the reflux amount at the top of the kettle is 1.5 times of the material feeding amount, the sampling from the top of the primary rectification kettle 2 is started, when the content of the top 2 of the primary rectification kettle 2 and the 3-dichloro-5-trifluoromethylpyridine is not more than 2%, simultaneously, extracting the top and the bottom of a primary rectifying kettle 2, wherein the extraction flow at the bottom of the primary rectifying kettle 2 is 95 percent of the sincerity of the content of 2, 3-dichloro-5-trifluoromethylpyridine in a crude product and the feeding flow, the extraction flow at the top of the primary rectifying kettle 2 is the difference of the feeding flow of the crude product minus the extraction flow at the bottom of the primary rectifying kettle 2, the crude product extracted at the bottom of the primary rectifying kettle 2 is accumulated in a primary impurity removing kettle 4 to be stirred and then fed into a secondary impurity removing kettle 5 through a secondary material transfer pump P2, simultaneously a jacket in the secondary impurity removing kettle 5 is opened for heating and stirring, when the temperature reaches 60 ℃, 10 percent of liquid alkali is dripped, when the material in the secondary impurity removing kettle 5 reaches 80 percent of volume, a kettle bottom valve of the secondary impurity removing kettle 5 is opened, a tertiary material transfer pump P3 is opened to feed an oil layer to a secondary rectifying kettle 7 at a certain speed, the water layer can be divided into a primary impurity removal kettle 4 through a secondary impurity removal water separator F2, the oil layer in a secondary impurity removal water separator F2 can not be completely emptied in the feeding process, the liquid alkali is excessive, the unreacted liquid alkali can carry out eagle pre-impurity removal in a secondary impurity removal kettle 5, the alkaline water is finally divided into a wastewater receiving tank 101 through a primary impurity removal water separator F1, the product after secondary impurity removal only contains recombination and products, when the secondary rectification tower top flow meter Q5 at the top of the secondary rectification kettle 7 kettle is 1.5 times of the flow of the primary rectification tower bottom flow meter Q4, the feeding of the alkaline water to the secondary rectification kettle 7 is stopped, the product is collected to the product receiving tank 8 when the content of the sample in the secondary rectification kettle 7 is more than 99.5 percent, the secondary rectification tower top flow meter Q6 is a primary rectification tower bottom flow meter Q4 and a feed flow meter Q1 during collection 90% of the 2, 3-dichloro-5-trifluoromethylpyridine content, and the secondary rectification tower bottom flowmeter Q3 is the flow obtained by subtracting the secondary rectification tower top flowmeter Q5 from 95% of the primary rectification tower bottom flowmeter Q4.
The above, only be the concrete implementation of the preferred embodiment of the present invention, but the protection scope of the present invention is not limited thereto, and any person skilled in the art is in the technical scope of the present invention, according to the technical solution of the present invention and the utility model, the concept of which is equivalent to replace or change, should be covered within the protection scope of the present invention.
Claims (8)
1. A2, 3-dichloro-5-trifluoromethylpyridine continuous rectification device comprises a crude product storage tank (1), a primary rectification kettle (2), a light component receiving tank (3), a primary impurity removal kettle (4), a secondary impurity removal kettle (5), a dripping tank (6), a secondary rectification kettle (7), a product receiving tank (8), a heavy component receiving tank (9) and a wastewater receiving tank (10), and is characterized in that the crude product storage tank (1) is connected to the middle part of the primary rectification kettle (2) through a feeding flowmeter (Q1), the top of the primary rectification kettle (2) is connected with the top of the light component receiving tank (3), the bottom of the primary rectification kettle (2) is connected with a primary material transfer pump (P1), the discharge hole of the primary material transfer pump (P1) is connected with the top of the primary impurity removal kettle (4) through a primary rectification tower bottom flowmeter (Q4), the primary rectifying still (2) is connected with the top of the primary impurity removing still (4) through a primary rectifying condenser (E2) and a primary impurity removing condenser (E3), the bottom of the primary impurity removing still (4) is connected with a secondary material transferring pump (P2), the bottom of the dripping tank (6) is connected with the top of the secondary impurity removing still (5), the top of the secondary impurity removing still (5) is connected with the top of the waste water receiving tank (10) through a primary impurity removing water separator (F1), the discharge port of the secondary material transferring pump (P2) is connected with the top feed port of the primary impurity removing water separator (F1), the bottom of the secondary impurity removing still (5) is connected with a tertiary material transferring pump (P3) through a secondary impurity removing water separator (F2), the top of the primary impurity removing still (4) is connected with the middle of the secondary impurity removing water separator (F2), the discharge port of the tertiary material transferring pump (P3) is connected with the middle of the secondary rectifying still (7), the top of the secondary rectifying still (7) is connected with the top of the product receiving tank (8) through a secondary rectifying tower top flow meter (Q5), and the bottom of the secondary rectifying still (7) is connected with the top of the heavy component receiving tank (9) through a four-time material transfer pump (P4).
2. The continuous rectification device of 2, 3-dichloro-5-trifluoromethylpyridine according to claim 1, wherein the top of the primary rectification kettle (2) is connected with the inlet of a primary rectification condenser (E2), the top side wall of the primary rectification kettle (2) is connected with the light component receiving tank (3) through a primary rectification tower top flowmeter (Q2), the primary rectification condenser (E2) is connected between the connecting pipes of the two sets of primary rectification tower top flowmeters (Q2), and the top of the primary rectification condenser (E2) is connected with the top of the light component receiving tank (3) through a conduit.
3. The continuous rectification device of 2, 3-dichloro-5-trifluoromethylpyridine according to claim 2, wherein the primary impurity removal kettle (4) and the primary impurity removal condenser (E3) are connected in a gas phase.
4. A continuous rectification plant of 2, 3-dichloro-5-trifluoromethylpyridine according to claim 3, wherein the bottom side wall of the primary rectification kettle (2) is connected with a primary rectification reboiler (E1), the primary rectification reboiler (E1) is connected with the feed inlet of the primary material transfer pump (P1), and the bottom of the primary rectification kettle (2) is connected with the feed inlet of the primary material transfer pump (P1) through a conduit.
5. The continuous rectification device for 2, 3-dichloro-5-trifluoromethylpyridine according to claim 4, characterized in that the top of the secondary impurity removal kettle (5) is connected to the bottom discharge port of the primary impurity removal water separator (F1), and the wastewater receiving tank (10) is connected to the side wall discharge port of the primary impurity removal water separator (F1).
6. A2, 3-dichloro-5-trifluoromethylpyridine continuous rectification device according to claim 5, characterized in that a secondary rectification condenser (E5) is connected to the top of the secondary rectification kettle (7), the top is connected to the top of the product receiving tank (8), the top side wall of the secondary rectification kettle (7) is connected to the top of the product receiving tank (8) through a secondary rectification tower top flowmeter (Q5), and the bottom of the secondary rectification tower top flowmeter (Q5) is connected between the two sets of secondary rectification tower top flowmeters (Q5) through a conduit.
7. The continuous rectification device of 2, 3-dichloro-5-trifluoromethylpyridine according to claim 6, wherein the outlet on the bottom side of the secondary rectification kettle (7) is connected with a secondary rectification reboiler (E6), the top of the secondary rectification reboiler (E6) is connected with the feed inlet of the quaternary material transfer pump (P4), and the bottom of the secondary rectification kettle (7) is connected with the feed inlet of the quaternary material transfer pump (P4) through a conduit.
8. The continuous rectification device of 2, 3-dichloro-5-trifluoromethylpyridine according to claim 7, characterized in that a primary rectification column bottom flowmeter is arranged between the discharge port of the primary transfer pump (P1) and the primary impurity removal kettle (4), and a secondary column bottom flowmeter (Q3) is arranged between the discharge port of the quaternary transfer pump (P4) and the heavy component receiving tank (9).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021853120.3U CN213790030U (en) | 2020-08-31 | 2020-08-31 | 2, 3-dichloro-5-trifluoromethylpyridine continuous rectification device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021853120.3U CN213790030U (en) | 2020-08-31 | 2020-08-31 | 2, 3-dichloro-5-trifluoromethylpyridine continuous rectification device |
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| CN213790030U true CN213790030U (en) | 2021-07-27 |
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| CN202021853120.3U Active CN213790030U (en) | 2020-08-31 | 2020-08-31 | 2, 3-dichloro-5-trifluoromethylpyridine continuous rectification device |
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| CN (1) | CN213790030U (en) |
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