Ketoxime extractive distillation system

Abstract

The utility model provides an extractive distillation system for ketoxime, which comprises a reaction kettle, an extractant intermediate tank, an extraction tank, a partition rectifying tower, a condenser and an acetoxime storage tank, a rectifying tower feed pipe is arranged between the extraction tank and the partition rectifying tower, and a feed pipe heat preservation jacket is sleeved on the outer layer of the rectifying tower feed pipe. One end of the feed pipe heat preservation jacket is connected with the condensation water outlet pipe, the other end of the feed pipe heat preservation jacket is connected with the return pipe, and the end, away from the partition plate rectifying tower, of the condenser is connected to the top of the extracting agent intermediate tank. According to the ketoxime extractive distillation system provided by the utility model, heat in the condenser can be recycled to the front end of the partition plate distillation tower while water in ketoxime is separated, so that the energy consumption is reduced, and the economic benefit of a product is improved.

Description

TECHNICAL FIELD

[0001] The utility model relates to the technical field of fractionation, more particularly, relates to a kind of ketoxime's extraction rectification system. BACKGROUND

[0002] Ketoxime compound is a kind of very important organic compound, is widely used in pesticide, medicine and other related fields, and ketoxime, butanone oxime as organic silicon crosslinking agent intermediate and polyurethane blocking agent, demand also substantially increases.Ketoxime can be effectively synthesized by hydroxylamine sulfate method, but many deficiencies are exposed when purifying product, ketoxime product is easy to carry more moisture when extracting, thereby reducing the purity of product, and when extracting agent is recycled, it will produce greater energy consumption, increase the economic cost of ketoxime product.

[0003] The above problems are urgent to be solved, so the utility model provides a kind of ketoxime's extraction rectification system. UTILITY MODEL CONTENT

[0004] The utility model solves the technical problems to provide a kind of ketoxime's extraction rectification system, improve the energy consumption recovery when extracting agent is recycled, increase the economic cost of ketoxime product.

[0005] The technical scheme that the utility model solves its technical problems is as follows: a kind of ketoxime's extraction rectification system, including reaction kettle, extraction agent intermediate tank, extraction tank, baffle rectification tower, condenser, ketoxime storage tank, the top of the reaction kettle is connected to the middle part of the extraction agent intermediate tank, the top of the extraction agent intermediate tank is connected to the middle part of the extraction tank, the top of the extraction tank is connected to the middle part of the baffle rectification tower, the extraction tank and the baffle rectification tower are equipped with rectification tower feed pipe between, the outer layer of the rectification tower feed pipe is equipped with feed pipe heat preservation jacket, the top of the baffle rectification tower is connected to the condenser, the right middle part of the baffle rectification tower is connected to the ketoxime storage tank, the middle part of the condenser is equipped with condensing water pipe, the condenser is equipped with reflux pipe close to the baffle rectification tower one end, the one end of the feed pipe heat preservation jacket is connected with the condensing water pipe, the other end of the feed pipe heat preservation jacket is connected with the reflux pipe, the one end of the condenser away from the baffle rectification tower is connected to the top of the extraction agent intermediate tank.

[0006] Preferably, the reaction kettle is equipped with stirrer, filter, the filter is located in the inside top end of the reaction kettle, and ketoxime product is discharged from the top of the reaction kettle after filtering through the filter.

[0007] Preferably, the reaction kettle is transported by the lifting pump ketoxime water mixed solution in the bottom to the extraction agent intermediate tank and is mixed with toluene, and the toluene steam at the top of the baffle rectification tower is liquefied by the condenser and then returns to the extraction agent intermediate tank for reuse.

[0008] Preferably, the extraction tank bottom is connected with an extraction water phase tank, the toluene in the extraction tank extracts the acetone oxime out and is discharged from the extraction tank top to the baffle rectifying column, and the water phase at the extraction tank bottom flows into the extraction water phase tank.

[0009] Preferably, the middle part of the baffle rectifying column is ketone oxime, and the top part is toluene vapor, and the ketone oxime is discharged from the middle part of the baffle rectifying column to the acetone oxime storage tank for storage.

[0010] Preferably, the baffle rectifying column is provided with baffles, the baffles include first, second and third vertical baffles arranged vertically and first and second horizontal baffles arranged horizontally, and the first, second and third vertical baffles are uniformly spaced between the first and second horizontal baffles.

[0011] Preferably, the baffle rectifying column is further provided with a wire, and the wire is arranged at the top right side of the third vertical baffle.

[0012] Preferably, the baffle rectifying column bottom is provided with a reboiler.

[0013] Preferably, the condenser is provided with two sets of condensing pipes, one set of high-temperature condensing pipes is arranged near one end of the baffle rectifying column, one set of low-temperature condensing pipes is arranged away from the other end of the baffle rectifying column, and the high-temperature condensing pipes and the low-temperature condensing pipes are not communicated.

[0014] Preferably, the high-temperature condensing pipes are connected with the condensate water pipe at the lower side away from the other end of the baffle rectifying column, the high-temperature condensing pipes are connected with the reflux pipe at the lower side near the baffle rectifying column, the high-temperature condensing pipes are connected with the first water inlet pipe at the upper side near the baffle rectifying column, the low-temperature condensing pipes are connected with the water outlet pipe at the lower side away from the other end of the baffle rectifying column, and the low-temperature condensing pipes are connected with the second water inlet pipe at the upper side near the baffle rectifying column.

[0015] The toluene vapor at the top of the baffle rectifying column is liquefied by the condenser and then returns to the toluene intermediate tank for reuse, the toluene in the extraction tank extracts the ketone oxime out and is discharged from the extraction tank top to the baffle rectifying column through the rectifying column feed pipe, the high-temperature liquid at the end of the condenser away from the baffle rectifying column is transported to the feed pipe jacket through the condensate water pipe to warm the ketone oxime, and the energy consumption is reduced. BRIEF DESCRIPTION OF DRAWINGS

[0016] The utility model will be further described below in combination with the drawings and examples.

[0017] In the picture: Figure 1 This is a schematic diagram of the extraction and distillation system for ketoxime of this invention;

[0018] Figure 2 for Figure 1 Schematic diagram of the structure of the intermediate reaction vessel;

[0019] Figure 3 for Figure 1 Schematic diagram of the structure of the intermediate condenser and the insulation jacket of the feed pipe;

[0020] Figure 4 for Figure 1 A schematic diagram of the structure of a distillation column with a central partition.

[0021] 1. Extractive distillation system; 10. Reactor; 11. Agitator; 12. Filter; 20. Intermediate tank for extractant; 30. Extraction tank; 31. Feed pipe of distillation column; 32. Insulated jacket for feed pipe; 33. Aqueous phase tank for extraction; 40. Baffled distillation column; 41. Baffle; 411. First vertical baffle; 412. Second vertical baffle; 413. Third vertical baffle; 414. First horizontal baffle; 415. Second horizontal baffle; 42. Wire; 43. Reboiler; 50. Condenser; 501. High-temperature condenser tube; 502. Low-temperature condenser tube; 51. Condensate outlet pipe; 52. Reflux pipe; 53. First inlet pipe; 54. Outlet pipe; 55. Second inlet pipe; 60. Ketone oxime storage tank. Detailed Implementation

[0022] To make the technical problem to be solved, the technical solution, and the beneficial effects of this utility model clearer, the present utility model will now be described in detail with reference to the accompanying drawings. This drawing is a simplified schematic diagram, illustrating only the basic aspects of the present utility model, and therefore only shows the components relevant to the present utility model. Obviously, the described embodiments are only some, not all, of the embodiments of this utility model. All other embodiments obtained by those skilled in the art based on the embodiments of this utility model without creative effort are within the scope of protection of this utility model.

[0023] like Figure 1 As shown, this utility model provides an extraction and distillation system 1 for ketoximes, including a reaction vessel 10, an intermediate extractant tank 20, an extraction tank 30, a partition distillation column 40, a condenser 50, and a ketoxime storage tank 60.

[0024] like Figure 2 As shown, the reactor 10 is equipped with a stirrer 11 and a filter 12. The filter 12 is located at the top inside the reactor 10. The ketoxime product is filtered through the filter 12 and discharged from the top of the reactor 10. The filter 12 has holes corresponding to the stirrer 11 for the stirrer 11 to pass through.

[0025] The top of the reactor 10 is connected to the middle of the extractant intermediate tank 20 by a pipeline, and the reactor 10 transports the ketoxime water mixed solution at the top to the extractant intermediate tank 20 through the lifting pump, and the ketoxime water mixed solution is mixed with the toluene in the extractant intermediate tank 20, and the condenser 50 is connected to the top of the extractant intermediate tank 20 by a pipeline, and the toluene vapor at the top of the partition rectification tower 40 is liquefied by the condenser 50 and then flows back to the extractant intermediate tank 20 for reuse.

[0026] The top of the extractant intermediate tank 20 is connected to the middle of the extraction tank 30 by a pipeline, and the high-water ketoxime solution in the mixed reactor 10 of the extractant intermediate tank 20, the toluene solution refluxed by the condenser 50, and the original toluene in the extractant intermediate tank 20 are extracted from the ketoxime solution discharged from the reactor 10, and are transported to the extraction tank 30 for layered extraction treatment.

[0027] As shown in Figure 3 The extraction tank 30 is provided with a rectification tower feed pipe 31 between the extraction tank 30 and the partition rectification tower 40, and the outer layer of the rectification tower feed pipe 31 is sleeved with a feed pipe heat preservation jacket 32, the water phase in the extraction tank 30 flows from the bottom to the extraction water phase tank 33, and the toluene in the extraction tank 30 extracts the ketoxime and then is discharged from the top of the extraction tank 30 to the partition rectification tower 40.

[0028] The middle of the partition rectification tower 40 is connected to the ketoxime storage tank 60 by a pipeline, and the top of the partition rectification tower 40 is connected to the condenser 50 by a pipeline, and the middle of the partition rectification tower 40 is ketoxime, and the top is toluene vapor, and the ketoxime is discharged from the middle of the partition rectification tower 40 to the ketoxime storage tank 60 for storage.

[0029] As shown in Figure 4 The partition rectification tower 40 is provided with a partition 41, and the partition 41 includes a first vertical partition 411, a second vertical partition 412, and a third vertical partition 413 arranged vertically, and a first horizontal partition 414 and a second horizontal partition 415 arranged horizontally, and the first vertical partition 411, the second vertical partition 412, and the third vertical partition 413 are uniformly and spacedly arranged between the first horizontal partition 414 and the second horizontal partition 415.

[0030] The ketoxime enters from the left middle of the partition rectification tower 40, flows downward through the passage between the left side wall of the partition rectification tower 40 and the first vertical partition 411, then enters upward through the passage between the first vertical partition 411 and the second vertical partition 412, then enters downward through the passage between the second vertical partition 412 and the third vertical partition 413, and finally flows upward through the right passage, and the multiple partitions arranged in the middle of the partition rectification tower 40 enhance the mass transfer effect.

[0031] The partition rectification tower 40 is also provided with a wire 42 arranged at the top right side of the third vertical partition 413.

[0032] The bottom of the partition rectification tower 40 is connected with a reboiler 43, and the reboiler 43 is used for warming the partition rectification tower 40 to toluene 120 DEG C under 1KPa, and toluene is evaporated to be gaseous, and ketoxime is liquid.

[0033] As shown in the figure, two sets of condensing pipes are arranged in the condenser 50, one set of high-temperature condensing pipe 501 is arranged near one end of the partition rectification tower (40), and one set of low-temperature condensing pipe 502 is arranged away from the other end of the partition rectification tower 40, and the high-temperature condensing pipe 501 is not communicated with the low-temperature condensing pipe 502. Figure 3 The lower side of the end of the high-temperature condensing pipe 501 away from the partition rectification tower 40 is connected with a condensing water outlet pipe 51, the lower side of the high-temperature condensing pipe 501 near the partition rectification tower 40 is connected with a reflux pipe 52, and the upper side of the high-temperature condensing pipe 501 near the partition rectification tower 40 is connected with a first water inlet pipe 53.

[0034] The end of the high-temperature condensing pipe 501 is connected to one end of the feed pipe insulation jacket 32 through the condensing water outlet pipe 51, and the other end of the feed pipe insulation jacket 32 is connected to the starting end of the high-temperature condenser through the reflux pipe 52.

[0035] The lower side of the end of the low-temperature condensing pipe 502 away from the partition rectification tower 40 is connected with a water outlet pipe 54, and the upper side of the low-temperature condensing pipe 502 near the partition rectification tower 40 is connected with a second water inlet pipe 55.

[0036] The upper side of the low-temperature condensing pipe 502 near the partition rectification tower 40 is connected with the second water inlet pipe 55, and the lower side of the low-temperature condensing pipe 502 away from the partition rectification tower 40 is connected with the water outlet pipe 54.

[0037] One end of the feed pipe insulation jacket 32 is connected with the condensing water outlet pipe 51, and the other end of the feed pipe insulation jacket 32 is connected with the reflux pipe 52, and the high-temperature liquid away from the partition rectification tower 40 of the condenser 50 is transported into the feed pipe insulation jacket 32 through the condensing water outlet pipe 51 to warm the ketoxime, and the liquid after being warmed is refluxed into the condenser 50 through the reflux pipe 52.

[0038] The working process of the ketoxime extraction rectification system 1 is as follows:

[0039] The reaction kettle 10 transports the ketoxime water mixed solution at the top into the extraction agent intermediate tank 20 through the lifting pump, and then is mixed with toluene, the toluene steam at the top of the partition rectification tower 40 is liquefied by the condenser 50 and then is refluxed into the extraction agent intermediate tank 20 for reuse, the toluene in the extraction tank 30 extracts the ketoxime and then is discharged from the top of the extraction tank 30 into the partition rectification tower 40, the water phase at the bottom of the extraction tank 30 flows into the extraction water phase tank 33, and the ketoxime is discharged from the middle of the partition rectification tower 40 and is stored in the ketoxime storage tank 60.

[0040]

[0041] ​The high-temperature liquid generated in the condenser 50 is transported to the feed pipe heat insulation jacket 32 through the condensate outlet pipe 51 to warm the ketoxime, and the warmed liquid is returned to the condenser 50 through the reflux pipe 52.

[0042] The ketoxime extraction distillation system 1 has the following beneficial effects:

[0043] 1. The high-temperature liquid generated in the condenser 50 is transported to the feed pipe heat insulation jacket 32 through the condensate outlet pipe 51 to warm the ketoxime, and the warmed liquid is returned to the condenser 50 through the reflux pipe 52.

[0044] 2. The condenser 50 is connected to the top of the partition rectification tower 40, which can separate the toluene carried by the extraction tank 30 and return it to the extraction agent intermediate tank 20, thereby improving the product purity of the ketoxime and the utilization rate of toluene.

[0045] 3. The multiple partitions 41 and iron wires 42 in the middle of the partition rectification tower 40 enhance the mass transfer effect.

[0046] It should be noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments in accordance with the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It will be further understood that the terms "comprises" and / or "comprising," when used in this specification, specify the presence of stated features, steps, operations, elements, and / or components, but do not preclude the presence or addition of one or more other features, steps, operations, elements, components, and / or groups thereof.

[0047] It should be noted that the terms "first", "second", and the like in the description and in the claims of the present application are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the use of these terms in the description and in the claims of the present application is merely to distinguish one element from another and not necessarily to describe a particular sequential or chronological order.

[0048] Based on the above ideal embodiments according to the present application, the relevant personnel can make various changes and modifications without deviating from the scope of the present application based on the above description. The technical scope of the present application is not limited to the contents described in the specification, and must be determined based on the scope of the claims.

Claims

1. A system for the extractive rectification of a ketoxime, characterized by: The extractive distillation system (1) comprises a reaction kettle (10), an extractant intermediate tank (20), an extraction tank (30), a partition distillation column (40), a condenser (50), and an acetone oxime storage tank (60), the top of the reaction kettle (10) is connected to the middle of the extractant intermediate tank (20), the top of the extractant intermediate tank (20) is connected to the middle of the extraction tank (30), the top of the extraction tank (30) is connected to the middle of the partition distillation column (40), a distillation column feed pipe (31) is arranged between the extraction tank (30) and the partition distillation column (40), an outer layer of the distillation column feed pipe (31) is sleeved with a feed pipe heat preservation jacket (32), the top of the partition distillation column (40) is connected to the condenser (50), the right middle of the partition distillation column (40) is connected to the acetone oxime storage tank (60), the middle of the condenser (50) is provided with a condensate water pipe (51), the condenser (50) is provided with a reflux pipe (52) close to one end of the partition distillation column (40), one end of the feed pipe heat preservation jacket (32) is connected to the condensate water pipe (51), the other end of the feed pipe heat preservation jacket (32) is connected to the reflux pipe (52), and the end of the condenser (50) away from the partition distillation column (40) is connected to the top of the extractant intermediate tank (20).

2. The system for the extractive rectification of ketoximes according to claim 1, characterized in that: The reaction kettle (10) is provided with a stirrer (11) and a filter (12), the filter (12) is arranged at the top end inside the reaction kettle (10), and the ketone oxime product is discharged from the top of the reaction kettle (10) after being filtered by the filter (12).

3. The system for extractive rectification of ketoximes according to claim 1, characterized in that: The reaction kettle (10) delivers the acetone oxime water mixed solution at the bottom to the extractant intermediate tank (20) through a lifting pump, and the toluene vapor at the top of the partition distillation column (40) is liquefied by the condenser (50) and then returns to the extractant intermediate tank (20) for reuse.

4. The system for extractive rectification of ketoximes according to claim 1, characterized in that: The extraction tank (30) is connected with an extraction water phase tank (33), the toluene in the extraction tank (30) extracts the acetone oxime and then discharges the acetone oxime from the top of the extraction tank (30) to the partition distillation column (40), and the water phase at the bottom of the extraction tank (30) flows into the extraction water phase tank (33).

5. The system for extractive rectification of ketoximes according to claim 1, characterized in that: The middle of the partition distillation column (40) is filled with ketone oxime, and the top is filled with toluene vapor, and the ketone oxime is discharged from the middle of the partition distillation column (40) to the acetone oxime storage tank (60) for storage.

6. The system for the extractive rectification of ketoximes according to claim 1, characterized in that: The partition distillation column (40) is provided with a partition (41), the partition (41) comprises first, second and third vertical partitions (411, 412, 413) arranged vertically and first and second horizontal partitions (414, 415) arranged horizontally, and the first, second and third vertical partitions (411, 412, 413) are evenly and spacedly arranged between the first and second horizontal partitions (414, 415).

7. The system for the extractive rectification of a ketoxime according to claim 6, characterized in that: The baffle rectifying tower (40) is further provided with a wire (42) arranged at the top right side of the third vertical baffle (413).

8. The system for the extractive rectification of ketoximes according to claim 1, characterized in that: The baffle rectifying tower (40) is further provided with a reboiler (43) at the bottom.

9. The system for the extractive rectification of ketoximes according to claim 1, characterized in that: The condenser (50) is provided with two sets of condensing pipes, one set of high-temperature condensing pipes (501) is arranged near one end of the baffle rectifying tower (40), and one set of low-temperature condensing pipes (502) is arranged away from the other end of the baffle rectifying tower (40), and the high-temperature condensing pipes (501) and the low-temperature condensing pipes (502) are not communicated.

10. The system for the extractive rectification of a ketoxime according to claim 9, characterized in that: The high-temperature condensing pipes (501) are connected with the condensing water outlet pipe (51) at the lower side away from the baffle rectifying tower (40), the high-temperature condensing pipes (501) are connected with the reflux pipe (52) at the lower side near the baffle rectifying tower (40), the high-temperature condensing pipes (501) are connected with the first water inlet pipe (53) at the upper side near the baffle rectifying tower (40), the low-temperature condensing pipes (502) are connected with the water outlet pipe (54) at the lower side away from the baffle rectifying tower (40), and the low-temperature condensing pipes (502) are connected with the second water inlet pipe (55) at the upper side near the baffle rectifying tower (40). The baffle rectifying tower (40) is further provided with a wire (42) arranged at the top right side of the third vertical baffle (413). The baffle rectifying tower (40) is further provided with a reboiler (43) at the bottom. The condenser (50) is provided with two sets of condensing pipes, one set of high-temperature condensing pipes (501) is arranged near one end of the baffle rectifying tower (40), and one set of low-temperature condensing pipes (502) is arranged away from the other end of the baffle rectifying tower (40), and the high-temperature condensing pipes (501) and the low-temperature condensing pipes (502) are not communicated. The high-temperature condensing pipes (501) are connected with the condensing water outlet pipe (51) at the lower side away from the baffle rectifying tower (40), the high-temperature condensing pipes (501) are connected with the reflux pipe (52) at the lower side near the baffle rectifying tower (40), the high-temperature condensing pipes (501) are connected with the first water inlet pipe (53) at the upper side near the baffle rectifying tower (40), the low-temperature condensing pipes (502) are connected with the water outlet pipe (54) at the lower side away from the baffle rectifying tower (40), and the low-temperature condensing pipes (502) are connected with the second water inlet pipe (55) at the upper side near the baffle rectifying tower (40).

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