Cleaning and separating device for 2-ethyl anthraquinone crude product

Abstract

The utility model relates to the technical field of water washing separation, in particular to a cleaning and separating device for a 2-ethyl anthraquinone crude product, which comprises a liquid alkali elevated tank, an alkali preparation tank and an alkali washing and water washing system. The alkali washing and water washing system comprises a first-stage alkali separator, a second-stage alkali separator, a first-stage water separator, a second-stage water separator, a methylbenzene azeotropic tower, a plate-type condenser, a methylbenzene oil-water separator and a first intermediate tank which are sequentially connected, and a liquid outlet in the bottom of the methylbenzene azeotropic tower is connected with a finished product condenser through a pipeline. And a liquid outlet of the finished product condenser is connected with a middle tank II through a pipeline. The washed extraction liquid enters a toluene azeotropic tower, toluene in the extraction liquid is evaporated out and stored in a first intermediate tank after being condensed, 2-ethyl anthraquinone serving as an extraction base solution is discharged out of the toluene azeotropic tower and stored in a second intermediate tank after being condensed, and continuous alkali washing and efficient production of 2-ethyl anthraquinone are achieved.

Description

TECHNICAL FIELD

[0001] The utility model relates to the technical field of washing separation, especially to a kind of 2-ethylanthraquinone crude product's cleaning separation device. BACKGROUND

[0002] 2-ethylanthraquinone is widely used in many fields as an important organic synthesis intermediate, including manufacturing hydrogen peroxide, medicine, dye intermediate, photocuring resin catalyst, photodegradation membrane, coating and photosensitive polymerization initiator etc. Under certain conditions, 2-ethylbenzoylbenzoic acid (2-ethylbenzoylbenzoic acid aluminum complex salt is generated by reacting phthalic anhydride and ethylbenzene under the action of aluminum chloride, and 2-ethylbenzoylbenzoic acid aluminum complex salt is obtained by acid hydrolysis) and toluene undergo ring-closing reaction to generate 2-ethylanthraquinone.

[0003] Chinese invention patent with publication number CN110787484B discloses a kind of 2-ethylanthraquinone ring-closing extraction liquid's caustic wash and alkaline wastewater treatment process, comprising the following steps: (1), with caustic wash kettle, caustic wash external circulation pump, external circulation heater and mixer constitute caustic wash external circulation system, extraction oil layer is introduced into caustic wash mixer, and is fully mixed with external circulation main fluid, caustic wash liquid alkali is introduced into static mixer, in addition to effective mixing with main fluid, caustic wash liquid alkali will be further mixed under the action of subsequent external circulation pump impeller;(2), oil, water system is completed in external circulation system after caustic wash treatment, overflow to layering kettle, and separate alkaline wastewater and caustic wash oil layer;(3), alkaline wastewater is introduced into flocculation kettle, first neutralized to neutral with sulfuric acid, then general flocculant is added to carry out flocculation treatment, after pH value adjustment and filtration to remove flocculation mud, filter water is sent to biochemical treatment device, and wastewater is treated by biochemistry, or discharged according to standard, or returned to acid precipitation process as closed loop liquid dilution water closed loop circulation.

[0004] In the above device, the separation process is carried out in the same reaction kettle, which leads to low production efficiency, long caustic wash time, and cannot realize continuous caustic wash. SUMMARY

[0005] The utility model aims at providing a kind of 2-ethylanthraquinone crude product's cleaning separation device, to realize the continuous caustic wash of 2-ethylanthraquinone, improve production efficiency.

[0006] In order to solve the above technical problems, the utility model adopts the technical scheme: a kind of 2-ethyl anthraquinone crude product's cleaning separation device, it is characterized by: including liquid alkali high tank and caustic water washing system, according to caustic water washing processing flow, the caustic water washing system includes sequentially connected primary alkali separator, secondary alkali separator, primary water separator, secondary water separator, toluene azeotrope tower, plate condenser, toluene oil-water separator and intermediate tank one, the bottom discharge port of the toluene azeotrope tower is connected with finished product condenser by pipeline, the liquid outlet of the finished product condenser is connected with intermediate tank two by pipeline, the side of the primary alkali separator is connected with feed pipe, the primary alkali separator is connected secondary alkali separator by conveying pipe two, the discharge outlet of the liquid alkali high tank is respectively connected feed pipe and conveying pipe two by liquid distribution pipe.

[0007] Preferably, the side of the liquid alkali high tank is provided with an alkali distribution tank, the secondary alkali separator is connected with the primary water separator by conveying pipe three, the bottom discharge port of the primary water separator is connected with the feed inlet of the conveying pipe three and the alkali distribution tank by pipelines respectively, and the discharge outlet of the alkali distribution tank is connected with the feed inlet of the liquid alkali high tank by a pipeline.

[0008] Preferably, the primary water separator and the secondary water separator are connected by conveying pipe four, and the bottom discharge port of the secondary water separator is connected with the toluene azeotrope tower, the conveying pipe four and the conveying pipe three by pipelines respectively.

[0009] Preferably, the bottom discharge port of the primary alkali separator is connected with the reflux inlet of the primary alkali separator by reflux pipe one, the bottom discharge port of the secondary alkali separator is connected with the reflux inlet of the secondary alkali separator by reflux pipe two, and the reflux pipe two is connected with the feed pipe by reflux pipe three.

[0010] Preferably, the reflux pipe one is connected with the pickling water washing system by conveying pipe one.

[0011] Preferably, according to the pickling water washing processing flow, the pickling water washing system includes acid extraction still, oil-water separation tower and oil-water separator connected in sequence, one end of the conveying pipe one is connected to the acid extraction still, and the bottom discharge port of the acid extraction still is connected with intermediate tank three by conveying pipe eight.

[0012] Preferably, the bottom discharge port of the oil-water separation tower is connected with the reflux inlet of the oil-water separation tower by reflux pipe four, the bottom discharge port of the oil-water separator is connected with the reflux inlet of the oil-water separator by reflux pipe six, and the discharge outlet of the oil-water separator is connected to the acid extraction still by reflux pipe five.

[0013] Preferably, the side of the intermediate tank three is provided with a recovery tank, the reflux pipe four is connected with the recovery tank by conveying pipe six, the reflux pipe six is connected with the conveying pipe six by conveying pipe five, and the conveying pipe eight is connected with the recovery tank by conveying pipe seven.

[0014] The beneficial effects of the present application are as follows:

[0015] The 2-ethylanthraquinone crude product is treated by twice alkaline washing, effectively removing impurities in the solution, improving the purity of 2-ethylanthraquinone; twice water washing ensures the cleanliness of the solution, avoiding pollution problems in subsequent treatment; the washed extraction liquid enters the toluene azeotrope tower, toluene in the extraction liquid is evaporated and stored in intermediate tank one after condensation, 2-ethylanthraquinone is discharged from the toluene azeotrope tower as extraction bottom liquid and stored in intermediate tank two after condensation, realizing continuous alkaline washing and efficient production of 2-ethylanthraquinone crude product. BRIEF DESCRIPTION OF DRAWINGS

[0016] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the drawings needed in the following embodiment or prior art description will be briefly introduced. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creative labor.

[0017] Figure 1 It is a structural schematic diagram of the alkaline washing and water washing system;

[0018] Figure 2 It is a structural schematic diagram of the acid washing and water washing system.

[0019] The drawings are as follows: 1, feed pipe, 2, conveying pipe one, 3, reflux pipe one, 4, primary alkali separator, 5, secondary alkali separator, 6, liquid alkali high tank, 7, alkali preparation tank, 8, primary water separator, 9, secondary water separator, 10, plate condenser, 11, toluene oil-water separator, 12, toluene azeotrope tower, 13, intermediate tank one, 14, product condenser, 15, intermediate tank two, 16, conveying pipe four, 17, conveying pipe three, 18, reflux pipe two, 19, conveying pipe two, 20, liquid preparation pipe, 21, reflux pipe three, 22, acid precipitation extraction kettle, 23, reflux pipe four, 24, reflux pipe five, 25, reflux pipe six, 26, oil-water separator, 27, conveying pipe five, 28, oil-water separation tower, 29, conveying pipe six, 30, recovery tank, 31, intermediate tank three, 32, conveying pipe seven, 33, conveying pipe eight. DETAILED DESCRIPTION

[0020] The features and exemplary embodiments of each aspect of the present application will be described in detail below, in order to make the purpose, technical scheme and advantages of the present application more clear and apparent, the present application will be further described in detail below with reference to the drawings and specific embodiments. It should be understood that the specific embodiments described herein are configured only to explain the present application and are not configured to limit the present application. For those skilled in the art, the present application can be implemented without some of these specific details. The following description of the embodiments is merely to provide a better understanding of the present application by showing examples of the present application.

[0021] The orientation words appearing in the following description are the directions shown in the drawings, and are not limited to the specific structure of the present application. In the description of the present application, it should be noted that, unless otherwise explicitly specified and limited, the terms "mounting", "connection" should be understood broadly, for example, it can be fixedly connected, or it can be detachably connected or integrally connected; it can be directly connected or indirectly connected. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances.

[0022] The embodiment of the present application provides a kind of 2-ethylanthraquinone crude product's cleaning separation device, including liquid alkali high tank 6, alkali tank 7 and caustic washing water washing system, according to caustic washing water washing process flow, this caustic washing water washing system includes sequentially connected first alkali separator 4, second alkali separator 5, first water separator 8, second water separator 9, toluene azeotrope tower 12, plate condenser 10, toluene oil-water separator 11 and intermediate tank one 13.The bottom discharge port of toluene azeotrope tower 12 is connected with finished product condenser 14 by pipeline, and the liquid outlet of finished product condenser 14 is connected with intermediate tank two 15 by pipeline.

[0023] The bottom discharge port of first alkali separator 4 is connected with the backflow port thereon by backflow pipe one 3, to form circulating backflow, to ensure that liquid alkali and 2-ethylanthraquinone crude product have longer contact time and more sufficient reaction, so that impurities are removed more effectively.The bottom discharge port of second alkali separator 5 is connected with the backflow port thereon by backflow pipe two 18, to form circulating backflow.Meanwhile, part of the solution is sent into feed pipe 1 again through backflow pipe three 21, and enters first alkali separator 4 again with new 2-ethylanthraquinone crude product for processing.This circulating backflow design not only improves the utilization rate of liquid alkali, but also ensures the sufficiency and effectiveness of the caustic washing process.It helps to reduce the residual amount of impurities and improve the purity and quality of the product.As liquid alkali continuously reacts with 2-ethylanthraquinone crude product in the circulation process, the consumption of new liquid alkali can also be reduced, thereby reducing production cost.

[0024] After the 2-ethylanthraquinone crude product in the primary alkali separator 4 is washed with alkali, the upper liquid is fed into the secondary alkali separator 5 through the delivery pipe two 19 for secondary washing with alkali, and the lower liquid in the primary alkali separator 4 is fed into the primary alkali separator 4 again through the reflux pipe one 3 after being washed with alkali, mixed with the new 2-ethylanthraquinone crude product, and washed with alkali again. The discharge port of the liquid alkali high tank 6 is connected to the feed pipe 1 and the delivery pipe two 19 through the liquid distribution pipe 20, so as to realize the supplement of alkali liquid. After the 2-ethylanthraquinone crude product in the secondary alkali separator 5 is washed with alkali for the second time, the upper liquid is fed into the primary water separator 8 through the delivery pipe three 17 for water washing, and the lower liquid is fed into the secondary alkali separator 5 again through the reflux pipe two 18 or is fed into the feed pipe 1 through the reflux pipe three 21, and is fed into the primary alkali separator 4 again with the new 2-ethylanthraquinone crude product for treatment.

[0025] After the upper extraction liquid (mainly composed of 2-ethylanthraquinone and toluene) in the primary water separator 8 is washed with water, the extraction liquid is fed into the secondary water separator 9 through the delivery pipe four 16 for secondary water washing, and the upper extraction liquid after water washing is fed into the toluene azeotrope tower 12 for further separation and purification, and the required components are separated out by using the boiling point difference of the components. The toluene with a lower boiling point is evaporated to form gaseous toluene, the gaseous toluene is condensed through the plate condenser 10, is extracted through the toluene oil-water separator 11, and is stored in the intermediate tank one 13 to obtain a toluene solution. The remaining solution in the toluene azeotrope tower 12 is cooled through the product condenser 14 and is stored in the intermediate tank two 15 to obtain a 2-ethylanthraquinone solution.

[0026] The lower extraction liquid (mainly composed of unreacted liquid alkali and water) in the primary water separator 8 after water washing is fed into the alkali distribution tank 7 to participate in the liquid alkali distribution or is fed into the delivery pipe three 17 for secondary water washing. The lower extraction liquid after water washing in the secondary water separator 9 is fed into the delivery pipe three 17 (when the lower extraction liquid contains high-concentration liquid alkali), or is fed into the delivery pipe four 16 (when the lower extraction liquid contains high-concentration liquid alkali), or is fed into the toluene azeotrope tower 12 (when the lower extraction liquid contains low-concentration liquid alkali).

[0027] The reflux pipe one 3 is connected to the acid washing and water washing system through the delivery pipe one 2. According to the acid washing and water washing process, the acid washing and water washing system comprises the acid extraction still 22, the oil-water separation tower 28 and the oil-water separator 26 which are connected in sequence. One end of the delivery pipe one 2 is connected to the acid extraction still 22, and the bottom discharge port of the acid extraction still 22 is connected to the intermediate tank three 31 through the delivery pipe eight 33.

[0028] The bottom discharge port of the oil-water separation tower 28 is connected to the reflux port of the oil-water separation tower 28 through the reflux pipe four 23, the bottom discharge port of the oil-water separator 26 is connected to the reflux port of the oil-water separator 26 through the reflux pipe six 25, and the discharge port of the oil-water separator 26 is connected to the acid extraction still 22 through the reflux pipe five 24.

[0029] The side of the intermediate tank three 31 is provided with a recovery tank 30, the return pipe four 23 is connected with the recovery tank 30 through the conveying pipe six 29, the return pipe six 29 is connected with the conveying pipe six 29 through the conveying pipe five 27, and the conveying pipe eight 33 is connected with the recovery tank 30 through the conveying pipe seven 32.

[0030] The 2-ethylanthraquinone crude product treated by the device comes from the post-product of the closed loop reaction (2-ethylbenzoylbenzoic acid is closed loop under the action of a catalyst), and thus contains a certain concentration of 2-ethylbenzoylbenzoic acid (BE acid). The solution (containing 2-ethylbenzoylbenzoic acid sodium, sodium hydroxide and part of 2-ethylbenzoylbenzoic acid) after one alkali washing or two alkali washings enters the acid precipitation extraction kettle 22 along the conveying pipe one 2, and 98% sulfuric acid is added to the acid precipitation extraction kettle 22 to acidify the solution, and the sulfuric acid reacts with the 2-ethylbenzoylbenzoic acid sodium to generate BE acid and sodium sulfate. After the acidification of the acid precipitation extraction kettle 22 is completed, the upper liquid enters the intermediate tank three 31 along the conveying pipe eight 33, and the BE acid is stored. The lower liquid enters the recovery tank 30 through the conveying pipe seven 32, and the sodium sulfate is stored. Since there is still part of the BE acid in the lower liquid, in order to recover, after extraction through the oil-water separation tower 28 and the oil-water separator 26 in turn, the upper liquid finally enters the acid precipitation extraction kettle 22 along the conveying pipe five 24 to be re-acidified with a new solution, and the lower liquid in the process enters the recovery tank 30 along the conveying pipe six 29 (corresponding to the oil-water separation tower 28) or the conveying pipe five 27 (corresponding to the oil-water separator 26).

[0031] According to the above embodiments of the utility model, these embodiments do not describe all the details, and do not limit the utility model to the specific embodiments. Obviously, according to the above description, many modifications and changes can be made. The description selects and specifically describes these embodiments in order to better explain the principles and practical applications of the utility model, so that the person skilled in the art can well utilize the utility model and make modifications and uses on the basis of the utility model. Any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the utility model shall be included in the protection scope of the utility model.

Claims

1. A cleaning separation apparatus for 2-ethylanthraquinone crude, characterized by: The alkali liquor high tank (6) and the caustic washing water washing system are connected, and the caustic washing water washing system comprises a first alkali separator (4), a second alkali separator (5), a first water separator (8), a second water separator (9), a toluene azeotrope tower (12), a plate condenser (10), a toluene oil-water separator (11) and an intermediate tank (13) connected in sequence, the bottom liquid outlet of the toluene azeotrope tower (12) is connected with a finished product condenser (14) through a pipeline, the liquid outlet of the finished product condenser (14) is connected with an intermediate tank (15) through a pipeline, one side of the first alkali separator (4) is connected with a feed pipe (1), the first alkali separator (4) is connected with the second alkali separator (5) through a conveying pipe (19), and the discharge outlet of the alkali liquor high tank (6) is connected with the feed pipe (1) and the conveying pipe (19) through a liquid distribution pipe (20).

2. A washing separation apparatus of 2-ethylanthraquinone crude according to claim 1, characterized by: One side of the alkali liquor high tank (6) is provided with an alkali distribution tank (7), the second alkali separator (5) is connected with the first water separator (8) through a conveying pipe (17), the bottom liquid outlet of the first water separator (8) is connected with the feed inlet of the conveying pipe (17) and the alkali distribution tank (7) through a pipeline respectively, and the discharge outlet of the alkali distribution tank (7) is connected with the feed inlet of the alkali liquor high tank (6) through a pipeline.

3. The washing separation apparatus of crude 2-ethylanthraquinone according to claim 2, characterized by: The first water separator (8) and the second water separator (9) are connected through a conveying pipe (16), and the bottom liquid outlet of the second water separator (9) is connected with the toluene azeotrope tower (12), the conveying pipe (16) and the conveying pipe (17) through a pipeline respectively.

4. The washing separation apparatus of crude 2-ethylanthraquinone according to claim 1, characterized by: The bottom liquid outlet of the first alkali separator (4) is connected with the reflux inlet of the first alkali separator (4) through a reflux pipe (3), the bottom liquid outlet of the second alkali separator (5) is connected with the reflux inlet of the second alkali separator (5) through a reflux pipe (18), and the reflux pipe (18) is connected with the feed pipe (1) through a reflux pipe (21).

5. The washing separation apparatus of crude 2-ethylanthraquinone according to claim 4, characterized by: The reflux pipe (3) is connected with an acid washing water washing system through a conveying pipe (2).

6. The washing separation apparatus of crude 2-ethylanthraquinone according to claim 5, characterized by: According to the acid washing water washing process, the acid washing water washing system comprises an acid extraction still (22), an oil-water separation tower (28) and an oil-water separator (26) connected in sequence, one end of the conveying pipe (2) is connected to the acid extraction still (22), and the bottom liquid outlet of the acid extraction still (22) is connected with an intermediate tank (31) through a conveying pipe (33).

7. The washing separation apparatus of crude 2-ethylanthraquinone according to claim 6, characterized by: The bottom liquid outlet of the oil-water separation tower (28) is connected with the reflux inlet of the oil-water separation tower (28) through a reflux pipe (23), the bottom liquid outlet of the oil-water separator (26) is connected with the reflux inlet of the oil-water separator (26) through a reflux pipe (25), and the discharge outlet of the oil-water separator (26) is connected to the acid extraction still (22) through a reflux pipe (24).

8. The washing separation apparatus of crude 2-ethylanthraquinone according to claim 7, characterized by: One side of the middle tank three (31) is provided with a recovery tank (30), the backflow pipe four (23) is connected with the recovery tank (30) through the conveying pipe six (29), the backflow pipe six (25) is connected with the conveying pipe six (29) through the conveying pipe five (27), and the conveying pipe eight (33) is connected with the recovery tank (30) through the conveying pipe seven (32).

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