A 2-ethylanthraquinone synthesis production line

Abstract

The present invention relates to the field of chemical synthesis technology, and in particular to a 2-ethylanthraquinone synthesis production line. According to the order of synthesis, it includes an acylation hydrolysis reaction module, a precipitation and dehydration module, a closed-loop reaction module, a crude product cleaning and separation module, and a crude product refining module connected by pipelines; acylation and hydrolysis are first completed inside the acylation hydrolysis reaction module. Then enter the precipitation and dehydration module for precipitation and dehydration, and then enter the closed-loop reaction module to complete the closed-loop reaction. After the closed loop is completed, enter the crude product cleaning and separation module for alkali washing separation and water washing separation to obtain a crude product, and these crude products finally enter the crude product refining module for refining to obtain a final product. The synthesis production line of the present invention has a simple structure, can be reacted using a solid catalyst, is more environmentally friendly, and has lower cost.

Description

Technical Field

[0001] The invention relates to the technical field of chemical synthesis, and in particular to a 2-ethylanthraquinone synthesis production line. Background Art

[0002] 2-Ethylanthraquinone (2-EAQ) is an essential reaction carrier for the preparation of hydrogen peroxide by the anthraquinone method. It is also a photopolymerization sensitizer and photosensitizer. 2-Ethylanthraquinone can also be used to prepare photosensitive compounds and is an activator for the air oxidation of alcohols to aldehydes or esters. In short, 2-Ethylanthraquinone is an important organic synthesis intermediate with a wide range of uses. It is widely used in the manufacture of hydrogen peroxide, reduced fuels, dispersed fuels, and active fuels. Most of the existing production of 2-Ethylanthraquinone uses fuming sulfuric acid as a catalyst. This production method is easy to control, the process is mature, and the cost is relatively low. Therefore, the existing 2-Ethylanthraquinone production lines are also designed around this technology. However, this type of production line will produce a large amount of waste acid, resulting in heavy subsequent treatment tasks. Summary of the invention

[0003] In order to solve the defects in the prior art, the present invention provides a 2-ethylanthraquinone synthesis production line, which is specifically achieved by the following technical solutions:

[0004] A 2-ethylanthraquinone synthesis production line comprises, in order of synthesis, an acylation hydrolysis reaction module, a desolventizing and dehydrating module, a closed-loop reaction module, a crude product cleaning and separation module, and a crude product refining module connected by pipelines, wherein the closed-loop reaction module comprises a feed buffer tank, a flash tank, and a plurality of reactors arranged in a row, wherein the desolventizing and dehydrating module is connected to the feed buffer tank through a BE acid delivery pipe, wherein the feed buffer tank is connected to a first feed port of a circulation tank through a second delivery pipe, wherein a feed heater is installed on the second delivery pipe, and a fifth delivery pipe is installed at a discharge port of the circulation tank. A circulation heater is installed on the fifth conveying pipe, a second material conveying pipe connected to the fifth conveying pipe is installed at the bottom of several of the reactors, a third conveying pipe is installed at the second feed port of the circulation tank, a first material conveying pipe connected to the third conveying pipe is installed on the top of several of the reactors, a fourth conveying pipe is installed at the feed port of the flash tank, the fourth conveying pipe is connected to the fifth conveying pipe through a second conveying branch pipe consistent with the number of reactors, a reflux tower is installed on one side of the flash tank, and the discharge port of the reflux tower is connected to a toluene condenser through a pipeline.

[0005] The closed-loop reaction module also includes a toluene washing tank, a first material conveying pipe is installed at the feed port of the toluene washing tank, the first material conveying pipe is connected to the first conveying pipe through a first conveying branch pipe, a sixth conveying pipe is installed at the discharge port of the toluene washing tank, a washing toluene heater is installed on the sixth conveying pipe, and the sixth conveying pipe is connected to the second material conveying pipe through a fourth conveying branch pipe.

[0006] The closed-loop reaction module also includes a vacuum cooler, a second vacuum buffer tank, a third vacuum pump and an exhaust gas cooler which are connected in sequence through pipelines. The feed port of the vacuum cooler is equipped with a vacuum main pipe, and the vacuum main pipe is connected to the corresponding reactor through multiple groups of third delivery branches.

[0007] The acylation hydrolysis reaction module comprises a chlorobenzene cleaning high-level tank, an ethylbenzene storage tank and a feeding bin, all of which are connected to the acylation reaction kettle pipeline. The acylation reaction kettle is connected to the insulation kettle, the acylation liquid sedimentation tank, the acylation liquid buffer tank and the hydrolysis kettle in sequence through pipelines. The insulation kettle, the acylation liquid sedimentation tank and the acylation liquid buffer tank are all connected to the chlorobenzene cleaning high-level tank through a chlorobenzene flushing pipeline; the hydrolysis kettle is connected to the desolventizing and dehydrating module through a hydrolyzate delivery pipeline.

[0008] The ethylbenzene storage tank is also connected to the ethylbenzene intermediate tank via an ethylbenzene delivery pump.

[0009] The desolventizing and dehydrating module includes a hydrolyzate separator connected to a hydrolyzate delivery pipeline, the hydrolyzate separator is connected to a first water washing separator via a first hydrolyzate pump, the first water washing separator is connected to a second water washing separator via a second hydrolyzate pump; the second water washing separator is also connected to a first countercurrent desolventizing tower, a second countercurrent desolventizing tower, a BE acid dehydration kettle, and a BE acid metering tank in sequence via a pipeline, the second countercurrent desolventizing tower, the BE acid dehydration kettle, and the BE acid metering tank are also connected to a vacuum dehydration condenser via a pipeline, the vacuum dehydration condenser is connected to a first vacuum buffer tank and a first vacuum pump in sequence via a pipeline, and the BE acid metering tank is connected to a feed buffer tank via a BE acid delivery pipe.

[0010] The hydrolyzate separator is also connected to the aluminum liquid desolventizing kettle through an aluminum trichloride delivery pump, and the top of the aluminum liquid desolventizing kettle is also connected to the aluminum liquid condenser, the second separation tank, and the chlorobenzene receiving tank in sequence through a pipeline, and the second separation tank is also connected to the second vacuum pump through a pipeline.

[0011] The crude product washing and separation module includes a primary alkali separator, a secondary alkali separator, a primary water separator, a secondary water separator, a toluene azeotropic tower, a plate condenser, a toluene oil-water separator and a first intermediate tank which are sequentially connected through pipelines. The bottom discharge port of the toluene azeotropic tower is connected to a finished product condenser through a pipeline, and the liquid outlet of the finished product condenser is connected to the second intermediate tank through a pipeline. A feed pipe is connected to one side of the primary alkali separator, and the primary alkali separator is connected to the secondary alkali separator through an eighth conveying pipe. The feed pipe and the eighth conveying pipe are also connected to the discharge port of the liquid alkali high-level tank through a liquid distribution pipe, and the second intermediate tank is connected to the crude product refining module through a pipeline.

[0012] The bottom discharge port of the primary alkali separator is connected to the top reflux port through the first reflux pipe, and the first reflux pipe is also connected to the acid precipitation extraction kettle through the seventh delivery pipe. The acid precipitation extraction kettle is connected to the oil-water separation tower and the oil-water separator in sequence through pipelines, the bottom discharge port of the acid precipitation extraction kettle is connected to the third intermediate tank through the fourteenth delivery pipe, and the discharge port of the oil-water separator is connected to the acid precipitation extraction kettle through the fifth reflux pipe.

[0013] The crude product refining module includes an alkali-adding kettle, a rising film evaporator, a condenser, a finished product storage tank, and a high-level finished product tank which are connected in sequence through pipelines. The alkali-adding kettle is connected to the second intermediate tank through a pipeline, the high-level finished product tank is connected to the feed port of a condensation crystallization slicer through a pipeline, the condensation crystallization slicer is located above the silo, the overflow port of the rising film evaporator is connected to the feed port of the scraper evaporator through an overflow pipe, the air outlet of the scraper evaporator is connected to the air collecting port of the rising film evaporator through a steam pipeline, the exhaust port of the condenser is connected to a cold well through a pipeline, the cold well is connected to the first bag dust collector, the second bag dust collector and a Roots vacuum pump group in sequence through a pipeline, the discharge port of the scraper evaporator is connected to the residue kettle through a pipeline, and the air outlet of the residue kettle and the exhaust port of the condenser are both connected to the air inlet of the cold well through a pipeline.

[0014] The technical solution of the present invention has the following advantages:

[0015] The synthesis production line of the present invention has a simple structure, can adapt to the application of more environmentally friendly solid catalysts, greatly reduces the generation of waste, is more environmentally friendly, and has lower costs. At the same time, it also improves the safety of production.

[0016] The acylation hydrolysis reaction module sends the tail gas generated in the hydrolysis kettle to the condenser group for condensation treatment, thereby condensing and recovering the reaction raw materials such as ethylbenzene and chlorobenzene that evaporate due to high temperature. This design reduces costs and avoids waste of raw materials.

[0017] In the desolventizing and dehydrating module, a hydrolyzate separator, a first water washing separator and a second water washing separator are installed to gradually separate various impurities in the BE acid crude liquid, thereby ensuring that the final BE acid has a high purity. At the same time, the separated impurities can be recovered step by step and reused.

[0018] The BE acid-toluene solution in the circulation tank is heated and then enters the reactor, where a closed-loop reaction is carried out under the action of a solid catalyst. The reacted material is returned to the circulation tank through the third delivery pipe, and then sent to the reactor again for several cycles, and finally a crude 2-ethylanthraquinone product is obtained from the circulation tank. The continuous cycle reaction improves the reaction efficiency and yield.

[0019] The crude 2-ethylanthraquinone is subjected to two alkaline washing treatments in the crude cleaning and separation module, which effectively removes impurities in the solution and improves the purity of 2-ethylanthraquinone; the cleanliness of the solution is ensured by two water washings, avoiding pollution problems in subsequent treatments; the washed extract enters the toluene azeotropic tower, the toluene in the extract is evaporated, and is stored in the first intermediate tank after condensation, and 2-ethylanthraquinone is discharged from the toluene azeotropic tower as the extraction bottom liquid, and is stored in the second intermediate tank after condensation, thereby realizing continuous alkaline washing and efficient production of the crude 2-ethylanthraquinone. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] In order to more clearly illustrate the specific implementation methods of the present invention or the technical solutions in the prior art, the drawings required for use in the specific implementation methods or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are some implementation methods of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0021] Figure 1 It is a schematic diagram of the structural framework of the present invention;

[0022] Figure 2 Schematic diagram of the structure of the acylation hydrolysis reaction module;

[0023] Figure 3 Schematic diagram of the structure of the condenser group

[0024] Figure 4 It is a structural schematic diagram of the desolventizing and dehydrating module;

[0025] Figure 5 This is a schematic diagram of the structure of the aluminum liquid desolventizing device.

[0026] Figure 6 It is a structural schematic diagram of a closed-loop reaction module;

[0027] Figure 7 It is a structural schematic diagram of the alkaline washing and water washing system;

[0028] Figure 8 It is a structural diagram of the pickling and water washing system;

[0029] Fig. 9 This is a schematic diagram of the structure of the crude product refining module.

[0030] In the figure, 1-acylation hydrolysis reaction module, 101-chlorobenzene cleaning high-level tank, 102-condenser group, 103-ethylbenzene intermediate tank, 104-ethylbenzene delivery pump, 105-acylation liquid sedimentation tank, 106-hydrolysis kettle, 107-acylation liquid delivery pump, 108-acylation liquid slag discharge pipeline, 109-acylation liquid buffer tank, 110-chlorobenzene flushing pipeline, 111-insulation kettle, 112-acylation reaction kettle, 113-discharger, 114-feeding bin, 115-rotary plate heat exchanger, 116-ethylbenzene storage tank; 117-condensation reflux device, 118-first separation tank;

[0031] 2-desolventizing and dehydrating module, 201-hydrolyzed liquid separator, 202-first hydrolyzed liquid pump, 203-first water washing separator, 204-second hydrolyzed liquid pump, 205-second water washing separator, 206-first countercurrent desolventizing tower, 207-second countercurrent desolventizing tower, 208-water separator, 209-BE acid dehydration kettle, 210-BE acid metering tank, 211-vacuum dehydration condenser, 212-first vacuum buffer tank, 213-first vacuum pump, 214-aluminum trichloride delivery pump, 215-aluminum liquid desolventizing kettle, 216-aluminum liquid condenser, 217-second separation tank, 218-chlorobenzene receiving tank, 219-second vacuum pump, 220-aluminum liquid desolventizing device;

[0032] 3-closed loop reaction module, 301-feed buffer tank, 302-toluene washing tank, 303-first delivery pipe, 304-washing toluene heater, 305-feed heater, 306-second delivery pipe, 307-first delivery branch pipe, 308-catalyst loading barrel, 309-single beam suspension crane, 310-first material delivery pipe, 311-third delivery pipe, 312-nitrogen supply device, 313-airflow delivery pipe, 314-fourth delivery pipe, 315-extraction Vacuum main pipe, 316-toluene condenser, 317-vacuum cooler, 318-tail gas cooler, 319-third vacuum pump, 320-second vacuum buffer tank, 321-reflux tower, 322-flash tank, 323-circulation tank, 324-circulation heater, 325-fifth conveying pipe, 326-second material conveying pipe, 327-second conveying branch pipe, 328-reactor, 329-third conveying branch pipe, 330-fourth conveying branch pipe, 331-sixth conveying pipe;

[0033] 4-crude product cleaning and separation module, 401-feeding pipe, 402-seventh conveying pipe, 403-first reflux pipe, 404-primary alkali separator, 405-secondary alkali separator, 406-liquid alkali high-level tank, 407-alkali preparation tank, 408-primary water separator, 409-secondary water separator, 410-plate condenser, 411-toluene oil-water separator, 412-toluene azeotropic tower, 413-first intermediate tank, 414-finished product condenser, 415-second intermediate tank, 416-tenth conveying pipe, 417-ninth delivery pipe, 418-second reflux pipe, 419-eighth delivery pipe, 420-liquid distribution pipe, 421-third reflux pipe, 422-acid separation extraction kettle, 423-fourth reflux pipe, 424-fifth reflux pipe, 425-sixth reflux pipe, 426-oil-water separator, 427-eleventh delivery pipe, 428-oil-water separation tower, 429-twelfth delivery pipe, 430-recovery tank, 431-third intermediate tank, 432-thirteenth delivery pipe, 433-fourteenth delivery pipe;

[0034] 5-crude product refining module, 501-alkali adding kettle, 502-rising film evaporator, 503-water jet vacuum unit, 504-steam pipeline, 505-overflow pipe, 506-condenser, 507-finished product storage tank, 508-high-level finished product tank, 509-condensation crystallization slicer, 510-silo, 511-reflux storage tank, 512-Roots vacuum pump unit, 513-second bag dust collector, 514-oil removal circulation pump, 515-oil circulation tank, 516-oil dust collector, 517-first bag dust collector, 518-cold well, 519-residue kettle, 520-scraper evaporator. DETAILED DESCRIPTION

[0035] The technical solution of the present invention will be described clearly and completely below in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0036] In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicating the orientation or positional relationship, are based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the modules or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as limiting the present invention. In addition, the terms "first", "second", and "third" are used for descriptive purposes only and cannot be understood as indicating or implying relative importance.

[0037] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "installed", "connected", and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0038] In addition, the technical features involved in the different embodiments of the present invention described below can be combined with each other as long as they do not conflict with each other.

[0039] In this embodiment, control valves are provided at the connection points of different pipelines to flexibly adjust and control the flow, pressure and direction of the materials. This is a common setting in the art and will be omitted in the description.

[0040] As attached Figure 1 As shown, the present invention provides a 2-ethylanthraquinone synthesis production line, which includes, in the order of synthesis, an acylation hydrolysis reaction module 1, a desolventizing and dehydrating module 2, a closed-loop reaction module 3, a crude product washing and separation module 4, and a crude product refining module 5 connected by pipelines.

[0041] The acylation hydrolysis reaction module 1 is used for the reaction of phthalic anhydride, ethylbenzene and aluminum chloride to generate 2-ethylbenzoylbenzoic acid aluminum chloride complex salt, and then the 2-ethylbenzoylbenzoic acid aluminum chloride complex salt is reacted with 5% dilute hydrochloric acid to generate 2-ethylbenzoylbenzoic acid (BE acid).

[0042] The desolventizing and dehydrating module 2 is used to contact the BE acid chlorobenzene solution with steam, the temperature reaches about 145°C, chlorobenzene and water are evaporated at normal pressure, and then dehydrated again under reduced pressure.

[0043] The closed-loop reaction module 3 is used to mix 2-ethylbenzoylbenzoic acid and toluene and inject them into a fixed bed reactor for a closed-loop reaction.

[0044] The crude product washing and separation module 4 is used to perform two-stage alkali washing in an alkali washing tower and one-stage water washing on the toluene solution of 2-ethylanthraquinone.

[0045] The crude product refining module 5 is used to distill the crude product to remove toluene, and then perform gasification, condensation and slicing to complete the refining.

[0046] As attached Figure 2 As shown, the acylation hydrolysis reaction module 1 includes a chlorobenzene cleaning high-level tank 101 for containing chlorobenzene, an ethylbenzene storage tank 116 for containing ethylbenzene, a feeding bin 114 and an acylation reaction kettle 112 .

[0047] Specifically, the chlorobenzene cleaning high-level tank 101, the ethylbenzene storage tank 116 and the feeding bin 114 are respectively connected to the acylation reactor 112 through pipelines, the acylation reactor 112 is connected to the hydrolysis reactor 106 through pipelines, and the hydrolysis reactor 106 is connected to the condenser group 102 through pipelines.

[0048] Phthalic anhydride and aluminum chloride are preliminarily mixed in the feeding bin 114 to obtain a mixture. The mixture, ethylbenzene and chlorobenzene are sent to the acylation reactor 112 for acylation reaction. After the reaction is completed, the feed liquid is sent to the hydrolysis reactor 106 for hydrolysis reaction to obtain crude BE acid.

[0049] An insulation kettle 111 and an acylation liquid settling tank 105 are also installed between the acylation reaction kettle 112 and the hydrolysis kettle 106, that is, the acylation reaction kettle 112 is connected to the insulation kettle 111 and the acylation liquid settling tank 105 in sequence through pipelines, and the acylation liquid settling tank 105 is connected to the hydrolysis kettle 106 through the acylation liquid slag discharge pipeline 108.

[0050] The acylation liquid settling tank 105 is connected to the acylation liquid buffer tank 109 through a pipeline, and the acylation liquid buffer tank 109 is connected to the hydrolysis kettle 106 through the acylation liquid delivery pump 107 .

[0051] After the raw materials react in the acylation reaction kettle 112 for a period of time, they are discharged into the insulation kettle 111 to continue the acylation reaction. The acylation reaction kettle 112 after being emptied is then filled with raw materials again to carry out the next batch of acylation reactions. Therefore, by installing the insulation kettle 111, the utilization efficiency of the acylation reaction kettle 112 and the production efficiency of the entire production line are greatly improved.

[0052] After the reaction is completed, the reaction liquid in the insulation kettle 111 enters the hydrolysis kettle 106 for hydrolysis reaction, but aluminum chloride still remains in the reaction liquid, which will affect the subsequent reaction and purification. Therefore, the reaction liquid first enters the acylation liquid settling tank 105 for standing to achieve solid-liquid separation, and the reaction solution on the upper layer will pass through the pipeline to the acylation liquid buffer tank 109, and then be pumped to the hydrolysis kettle 106 by the acylation liquid delivery pump 107 for hydrolysis.

[0053] By installing the acylation liquid buffer tank 109 , it can be avoided that the hydrolysis kettle 106 is hydrolyzing the reaction liquid of the previous batch, resulting in the current batch of reaction liquid being unable to be discharged normally from the acylation liquid settling tank 105 .

[0054] During the hydrolysis reaction, due to the high temperature in the hydrolysis kettle 106, the heated ethylbenzene and chlorobenzene will evaporate and reach the condenser group 102, where heat exchange occurs and the ethylbenzene and chlorobenzene condense to form droplets, which are then converted back into liquid form and collected.

[0055] As attached Figure 3As shown, the condenser group 102 includes three condenser refluxes 117 and a first separation tank 118, and the three condenser refluxes 117 and the first separation tank 118 are connected in series in sequence, wherein the first condenser reflux 117 and the first separation tank 118 are respectively connected to the hydrolysis tank 106 through pipelines.

[0056] The aforementioned acylation reaction kettle 112 is also connected to the rotary plate heat exchanger 115 through a pipeline.

[0057] The temperature in the acylation reaction kettle 112 is relatively high, and part of the raw materials evaporate and escape. This part of the raw materials is heat exchanged in the rotary plate heat exchanger 115, condensed into liquid, and then returned to the acylation reaction kettle 112, thereby realizing raw material recovery.

[0058] The aluminum chloride precipitate remaining in the acylation liquid settling tank 105 is flushed into the hydrolysis kettle 106 during cleaning and discharged together with the cleaning liquid of the hydrolysis kettle 106.

[0059] The heat preservation kettle 111 , the acylation liquid settling tank 105 , and the acylation liquid buffer tank 109 are all connected to the chlorobenzene cleaning high-level tank 101 through the chlorobenzene flushing pipeline 110 .

[0060] Chlorobenzene was used as both reaction solvent and cleaning liquid.

[0061] The aforementioned ethylbenzene storage tank 116 is also connected to the ethylbenzene intermediate tank 103 via an ethylbenzene delivery pump 104, and the ethylbenzene delivery pump 104 is used to pump ethylbenzene to the ethylbenzene storage tank 116. An ethylbenzene overflow pipe is also connected between the ethylbenzene storage tank 116 and the ethylbenzene intermediate tank 103.

[0062] The hydrolysis kettle 106 is also connected to a hydrochloric acid storage tank, and the hydrochloric acid in the hydrochloric acid storage tank is pumped to the hydrolysis kettle 106 .

[0063] A discharger 113 is installed between the feeding bin 114 and the acylation reaction kettle 112 .

[0064] The hydrolysis kettle 106 is connected to the hydrolysis solution separator 201 of the desolventizing and dehydrating module 2 through a hydrolysis solution delivery pipeline.

[0065] In this embodiment, there are multiple acylation hydrolysis reaction modules 1, and the multiple acylation hydrolysis reaction modules 1 are connected in parallel.

[0066] As attached Figure 4 As shown, the desolventizing and dehydrating module 2 includes a hydrolyzate separator 201 , which is connected to a first water washing separator 203 via a first hydrolyzate pump 202 , and the first water washing separator 203 is connected to a second water washing separator 205 via a second hydrolyzate pump 204 .

[0067] The hydrolyzate separator 201 is used to receive the hydrolyzate from the hydrolysis kettle 106, and perform static stratification to remove the aluminum chloride that has not been removed from the hydrolyzate.

[0068] The hydrolyzate separator 201 is also connected to the aluminum liquid desolventizing device 220 via an aluminum chloride delivery pump 214 .

[0069] The aluminum chloride mixed liquid in the lower layer is pumped to the aluminum liquid desolventizing device 220 by the aluminum chloride delivery pump 214. The hydrolyzed liquid in the upper layer enters the first water washing separator 203 and the second water washing separator 205 in sequence.

[0070] The second water washing separator 205 is also connected to the first countercurrent desolventizing tower 206, the second countercurrent desolventizing tower 207, the BE acid dehydration kettle 209, and the BE acid metering tank 210 in sequence through pipelines.

[0071] The BE acid metering tank 210 is used to contain BE acid and measure the yield of BE acid.

[0072] The BE acid dehydration kettle 209 is used to further remove water from the BE acid.

[0073] The second countercurrent desolventizing tower 207 is also connected to a water separator 208 via a pipeline. The water separator 208 is used to collect the water retained in the second countercurrent desolventizing tower 207 and discharge the collected water.

[0074] The second countercurrent desolventizing tower 207, BE acid dehydration kettle 209, and BE acid metering tank 210 are also connected to the vacuum dehydration condenser 211 through the first vacuum pipeline, the second vacuum pipeline, and the third vacuum pipeline respectively. The vacuum dehydration condenser 211 is connected to the first vacuum buffer tank 212 and the first vacuum pump 213 in sequence through pipelines.

[0075] The gases in the second countercurrent desolventizing tower 207, the BE acid dehydration kettle 209 and the BE acid metering tank 210 enter the vacuum dehydration condenser 211 for condensation, and the liquid obtained after condensation is sent to the first vacuum buffer tank 212 for temporary storage and then discharged uniformly.

[0076] In addition, by installing the first vacuum pump 213, the BE acid does not need to be pumped during the flow from the first countercurrent desolventizing tower 206 to the BE acid metering tank 210. For example, when the BE acid flows from the first countercurrent desolventizing tower 206 to the second countercurrent desolventizing tower 207, the first vacuum pipeline is opened to make the second countercurrent desolventizing tower 207 in a vacuum or negative pressure state, and the BE acid will flow into the second countercurrent desolventizing tower 207 under the action of atmospheric pressure; similarly, when the BE acid flows from the second countercurrent desolventizing tower 207 to the BE acid dehydration kettle 209, the first vacuum pipeline is closed and the second vacuum pipeline is opened, and the BE acid will flow from the second countercurrent desolventizing tower 207 to the BE acid dehydration kettle 209 under the action of atmospheric pressure; similarly, when the BE acid flows from the BE acid dehydration kettle 209 into the BE acid metering tank 210, the second vacuum pipeline is closed and the third vacuum pipeline is opened.

[0077] As attached Figure 5 As shown, the aluminum liquid desolventizing device 220 includes an aluminum liquid desolventizing kettle 215 connected to an aluminum chloride delivery pump 214 through a pipeline, and the aluminum liquid desolventizing kettle 215 is connected to the hydrolyzate separator 201 through a pipeline. Specifically, the aluminum liquid desolventizing kettle 215 is connected to the hydrolyzate separator 201 through the aluminum chloride delivery pump 214.

[0078] The top of the aluminum liquid desolventizing kettle 215 is also connected to the aluminum liquid condenser 216, the second separation tank 217, and the chlorobenzene receiving tank 218 in sequence through a pipeline. The second separation tank 217 is also connected to the second vacuum pump 219 through a pipeline. The solvent removed by the aluminum liquid desolventizing kettle 215 is condensed by the aluminum liquid condenser 216 and then enters the chlorobenzene receiving tank 218 for temporary storage.

[0079] The aluminum chloride after desolventizing is discharged from the bottom of the aluminum liquid desolventizing kettle 215, and the solvent in the chlorobenzene receiving tank 218 enters the chlorobenzene receiving tank 218 for recycling.

[0080] The aforementioned BE acid metering tank 210 is connected to the feed buffer tank 301 of the closed-loop reaction module 3 through a BE acid delivery pipe.

[0081] As attached Figure 6 As shown, the closed-loop reaction module 3 further includes a circulation tank 323, a nitrogen supply device 312, a toluene condenser 316, a flash tank 322 and a plurality of groups of reactors 328 arranged in a row.

[0082] Specifically, the feed buffer tank 301 is connected to the first feed port of the circulation tank 323 through the second delivery pipe 306 , and a feed heater 305 is installed on the second delivery pipe 306 .

[0083] The second feed port of the circulation tank 323 is connected to the third delivery pipe 311, and the discharge port of the circulation tank 323 is connected to the fifth delivery pipe 325. A circulation heater 324 is installed on the fifth delivery pipe 325.

[0084] A second material conveying pipe 326 connected to the fifth conveying pipe 325 is installed at the bottom of each reactor 328 , and a first material conveying pipe 310 connected to the third conveying pipe 311 is installed at the top of each reactor 328 .

[0085] The feed port of the flash tank 322 is equipped with a fourth delivery pipe 314, which is connected to the corresponding reactor 328 through a second delivery branch pipe 327 having the same number as the reactor 328. A reflux tower 321 is installed on one side of the flash tank 322, and the discharge port of the reflux tower 321 is connected to the toluene condenser 316 through a pipeline.

[0086] The reactor 328 is filled with a solid catalyst. When the reactor 328 needs to be added with catalyst, the catalyst in the catalyst loading barrel 308 is added to the reactor 328 using a single-beam suspension crane 309 erected above the reactor 328 .

[0087] First, a predetermined amount of toluene is fed into the feed buffer tank 301 , and then the BE acid in the BE acid metering tank 210 is fed into the feed buffer tank 301 , stirred evenly, and prepared into a BE acid-toluene solution, ie, a closed-loop reaction solution.

[0088] The closed-loop reaction liquid in the feed buffer tank 301 is pumped by the feed pump, along the second delivery pipe 306 and heated by the feed heater 305 thereon, and then pumped into the circulation tank 323. When the liquid level of the circulation tank 323 reaches 50%, the closed-loop reaction liquid enters the fifth delivery pipe 325 through the circulation pump, and enters each reactor 328 for cyclic closed-loop reaction after being heated by the circulation heater 324. Then the closed-loop reaction liquid returns to the circulation tank 323 through the third delivery pipe 311, and is sent to the reactor 328 again after being heated, and is circulated several times.

[0089] In this embodiment, there are four reactors 328. When a closed-loop reaction is performed, the closed-loop reaction liquid in the circulation tank 323 can be pumped into four reactors 328 at a time for circulation as described above. However, this circulation method easily causes the catalysts in the four reactors 328 to be replaced at the same time. In this case, the entire closed-loop reaction module 3 needs to be shut down. Therefore, the closed-loop reaction liquid in the circulation tank 323 can be first pumped into one of the reactors 328, or two reactors 328. When the catalyst of one reactor 328 or two reactors 328 is replaced, the closed-loop reaction liquid can be pumped into other reactors 328.

[0090] When the conversion rate of BE acid at the inlet of the reactor 328 reaches a preset value, the reaction product is sent to the flash tank 322 along the fourth delivery pipe 314. The toluene evaporated from the top of the reflux tower 321 is condensed into a liquid phase by the toluene condenser 316 and stored in a toluene receiving tank (not shown). The liquid phase at the bottom of the flash tank 322, i.e., the crude 2-ethylanthraquinone, enters the crude product washing and separation module 4 through a pipeline.

[0091] The closed-loop reaction module 3 also includes a vacuum pumping device connected to the reactor 328, which includes a vacuum cooler 317, a second vacuum buffer tank 320, a third vacuum pump 319 and an exhaust gas cooler 318 connected in sequence through pipelines. A vacuum main pipe 315 is installed at the feed port of the vacuum cooler 317, and the nitrogen supply device 312 is connected to the vacuum main pipe 315 through an air flow conveying pipe 313.

[0092] The vacuum main pipe 315 is connected to the corresponding reactors 328 through third delivery branch pipes 329 whose number is the same as that of the reactors 328 .

[0093] After the cyclic closed-loop reaction is completed, the catalyst inlet, catalyst outlet and cleaning port at the bottom of the reactor 328 are opened, and the deactivated catalyst is unloaded by vacuum unloading. The remaining deactivated catalyst at the bottom is swept out through the cleaning port, and then the wire mesh and part of the regenerated active catalyst are laid through the cleaning port. The catalyst outlet and cleaning port are sealed, and the catalyst is placed in the catalyst loading barrel 308 at the catalyst inlet to complete the catalyst loading. The catalyst inlet is sealed, and the nitrogen pressure is tested. After checking that there is no leakage, the reactor is ready for use and the next closed-loop operation is carried out.

[0094] The closed-loop reaction module 3 includes a reactor washing device, which includes a toluene washing tank 302. The feed port of the toluene washing tank 302 is connected to a first delivery pipe 303, and the first delivery pipe 303 is connected to a corresponding first material delivery pipe 310 through a first delivery branch pipe 307 having the same number as the reactor 328. The discharge port of the toluene washing tank 302 is connected to a sixth delivery pipe 331, and a washing toluene heater 304 is installed on the sixth delivery pipe 331.

[0095] The sixth conveying pipe 331 is connected to the corresponding second material conveying pipe 326 through the fourth conveying branch pipes 330 whose number is the same as the reactors 328 .

[0096] After the cyclic closed-loop reaction ends, the washing program is started. The washing toluene heater 304 heats the toluene solution to increase its temperature and flushing effect. The heated toluene solution is sent to the bottom of each reactor 328 through the sixth delivery pipe 331 and the fourth delivery branch pipe 330. The toluene solution rises in the reactor 328 and soaks the catalyst bed, and the catalyst is immersed and flushed. The toluene solution after flushing returns to the toluene washing tank 302 from the top outlet of the reactor 328 for circulating flushing. When the flushing reaches the predetermined effect, the flushing program is stopped, and the toluene solution in the reactor 328 is emptied. The toluene solution after washing is stored in the toluene washing tank 302, and these toluene solutions can be reused for the allocation of the feed buffer tank 301, reducing the waste of resources.

[0097] As attached Figure 7 and attached Figure 8 As shown, the crude product cleaning and separation module 4 includes a liquid alkali high-level tank 406, an alkali preparation tank 407 and an alkali washing and water washing system.

[0098] According to the alkali washing and water washing process, the alkali washing and water washing system includes a primary alkali separator 404, a secondary alkali separator 405, a primary water separator 408, a secondary water separator 409, a toluene azeotropic column 412, a plate condenser 410, a toluene oil-water separator 411 and a first intermediate tank 413 which are sequentially connected through pipelines. The bottom discharge port of the toluene azeotropic column 412 is connected to the finished product condenser 414 through a pipeline, and the liquid outlet of the finished product condenser 414 is connected to the second intermediate tank 415 through a pipeline.

[0099] The aforementioned flash tank 322 is connected to the primary alkali separator 404 via a 2-ethylanthraquinone delivery pipe.

[0100] The bottom discharge port of the primary alkali separator 404 is connected to the reflux port at the top thereof through the first reflux pipe 403 to form a circulating reflux, thereby ensuring a longer contact time and more sufficient reaction between the liquid alkali and the crude 2-ethylanthraquinone, thereby more effectively removing impurities.

[0101] The upper liquid discharge port of the primary alkali separator 404 is connected to the secondary alkali separator 405 via the eighth delivery pipe 419. The eighth delivery pipe 419 is provided with a first alkali washing delivery pump.

[0102] The bottom drain port of the secondary alkali separator 405 is connected to the reflux port at the top thereof through the second reflux pipe 418 to form a circulating reflux.

[0103] The reflux pipe 418 is also connected to the feed pipe 401 through the third reflux pipe 421, and the feed pipe 401 is connected to the primary alkali separator 404; while the secondary alkali separator 405 forms a circulation reflux, part of the solution is re-sent into the feed pipe 401 through the third reflux pipe 421, and enters the primary alkali separator 404 again for treatment together with the new 2-ethylanthraquinone crude product. This circulation reflux design not only improves the utilization rate of liquid caustic soda, but also ensures the adequacy and effectiveness of the alkali washing process. It helps to reduce the residual amount of impurities and improve the purity and quality of the product. At the same time, since the liquid caustic soda continuously reacts with the 2-ethylanthraquinone crude product during the circulation process, the consumption of new liquid caustic soda can also be reduced, reducing production costs.

[0104] The aforementioned 2-ethylanthraquinone delivery pipe and the third reflux pipe 421 are both connected to the input end of the second alkali washing delivery pump of the feed pipe 401 .

[0105] After the crude 2-ethylanthraquinone in the primary alkali separator 404 is alkali-washed, the upper layer of liquid enters the secondary alkali separator 405 along the eighth delivery pipe 419 for secondary alkali washing. After the alkali washing, the lower layer of liquid in the primary alkali separator 404 enters the primary alkali separator 404 again along the first reflux pipe 403, is mixed with the new crude 2-ethylanthraquinone and then alkali-washed again.

[0106] The upper liquid discharge port of the secondary alkali separator 405 is connected to the primary water separator 408 through the ninth delivery pipe 417 .

[0107] After the crude 2-ethylanthraquinone in the secondary alkali separator 405 is subjected to secondary alkali washing, the upper layer of liquid enters the primary water separator 408 along the ninth conveying pipe 417 for water washing, and the lower layer of liquid enters the secondary alkali separator 405 again along the second reflux pipe 418 or enters the feed pipe 401 along the third reflux pipe 421, and enters the primary alkali separator 404 together with the new crude 2-ethylanthraquinone for treatment.

[0108] The upper liquid discharge port of the primary water separator 408 is connected to the secondary water separator 409 through the tenth delivery pipe 416. The upper liquid discharge port of the secondary water separator 409 is connected to the toluene azeotropic column 412 through the tenth delivery pipe 416.

[0109] The bottom of the primary water separator 408 is also connected to the alkali preparation tank 407 and the ninth delivery pipe 417 through pipelines, wherein the alkali preparation tank 407 is connected to the liquid alkali high-level tank 406 through a pipeline.

[0110] The liquid caustic soda high-level tank 406 is connected to the primary alkali separator 404 and the secondary alkali separator 405 respectively through the liquid distribution pipe 420. Specifically, the liquid distribution pipe 420 is connected to the feed pipe 401 and the eighth conveying pipe 419 respectively, thereby realizing the connection with the primary alkali separator 404 and the secondary alkali separator 405.

[0111] The bottom drain port of the secondary water separator 409 is also connected to the ninth delivery pipe 417, the tenth delivery pipe 416, and the middle of the toluene azeotropic tower 412 through pipelines.

[0112] The top exhaust port of the toluene azeotropic tower 412 is connected to the plate condenser 410, the toluene oil-water separator 411, and the first intermediate tank 413 in sequence through pipelines.

[0113] The bottom liquid discharge port of the toluene azeotropic tower 412 is connected to the finished product condenser 414 and the second intermediate tank 415 in sequence through a pipeline.

[0114] After washing in the primary water separator 408, the upper organic phase enters the secondary water separator 409 along the tenth conveying pipe 416 for secondary washing, and the upper organic phase after the secondary washing enters the toluene azeotropic column 412 for further separation and purification. Toluene with a lower boiling point is evaporated to generate toluene vapor, which is condensed by the plate condenser 410 and extracted by the toluene oil-water separator 411 and then stored in the first intermediate tank 413 to obtain liquid toluene. The remaining solution in the toluene azeotropic column 412 is cooled by the finished product condenser 414 and then stored in the second intermediate tank 415 to obtain a 2-ethylanthraquinone solution.

[0115] After washing in the primary water separator 408, the lower water phase enters the alkali preparation tank 407 along the pipeline to participate in the liquid alkali preparation or enters the ninth delivery pipe 417 along the pipeline for further washing. After washing in the secondary water separator 409, if the lower water phase contains a high concentration of liquid alkali, it enters the ninth delivery pipe 417 along the pipeline, if it contains a relatively high concentration of liquid alkali, it enters the tenth delivery pipe 416 along the pipeline, and if it contains a low concentration of liquid alkali, it enters the toluene azeotropic tower 412 along the pipeline.

[0116] The first reflux pipe 403 is connected to the pickling and water washing system through the seventh delivery pipe 402. According to the pickling and water washing process, the pickling and water washing system includes an acid precipitation extraction kettle 422, an oil-water separation tower 428 and an oil-water separator 426 which are sequentially connected through pipelines. One end of the seventh delivery pipe 402 is connected to the acid precipitation extraction kettle 422, and the bottom discharge port of the acid precipitation extraction kettle 422 is connected to the third intermediate tank 431 through the fourteenth delivery pipe 433.

[0117] The bottom discharge port of the oil-water separation tower 428 is connected to the reflux port of the oil-water separation tower 428 through the fourth reflux pipe 423, the bottom discharge port of the oil-water separator 426 is connected to the reflux port of the oil-water separator 426 through the sixth reflux pipe 425, and the discharge port at the top of the oil-water separator 426 is connected to the acid precipitation extraction kettle 422 through the fifth reflux pipe 424.

[0118] A recovery tank 430 is installed on one side of the third intermediate tank 431, the fourth reflux pipe 423 is connected to the recovery tank 430 through the twelfth delivery pipe 429, the twelfth delivery pipe 429 is connected to the oil-water separator 426 through the eleventh delivery pipe 427, and the fourteenth delivery pipe 433 is connected to the recovery tank 430 through the thirteenth delivery pipe 432.

[0119] The crude 2-ethylanthraquinone treated by the crude cleaning and separation module 4 is the after-product of the closed-loop reaction. The solution after one or two alkali washes contains sodium 2-ethylbenzoylbenzoate, sodium hydroxide and part of 2-ethylbenzoylbenzoic acid, which enters the acid precipitation extraction kettle 422 along the seventh delivery pipe 402. 98% sulfuric acid is added to the acid precipitation extraction kettle 422 to acidify the solution. Sulfuric acid reacts with sodium 2-ethylbenzoylbenzoate to generate BE acid and sodium sulfate. After the acidification of the acid precipitation extraction kettle 422 is completed, the upper layer liquid enters the third intermediate tank 431 along the fourteenth delivery pipe 433 to store BE acid. The lower layer liquid enters the recovery tank 430 through the thirteenth delivery pipe 432 to store sodium sulfate. Since there will still be some BE acid in the lower layer liquid, in order to recover it, after separation and extraction in the oil-water separation tower 428 and the oil-water separator 426 in turn, the upper layer liquid enters the acid precipitation extraction kettle 422 along the fifth reflux pipe 424 to be re-acidified with the new solution, and the lower layer liquid enters the recovery tank 430 along the twelfth delivery pipe 429 or the eleventh delivery pipe 427.

[0120] As attached Fig. 9 As shown, the aforementioned crude product refining module 5 includes an alkali adding kettle 501, a rising film evaporator 502, a condenser 506, a finished product storage tank 507, a high-level finished product tank 508 and a silo 510 which are sequentially connected through pipelines.

[0121] The alkali adding kettle 501 is connected to the second intermediate tank 415 through a crude product conveying pipe.

[0122] A condensation crystallization slicer 509 is installed above the silo 510, and the feed port of the condensation crystallization slicer 509 is connected to the discharge port of the high-level finished product tank 508 through a pipeline, so that the product output from the high-level finished product tank 508 can directly enter the condensation crystallization slicer 509 for condensation crystallization and slicing. Finally, the refined 2-ethylanthraquinone product is sent to the silo 510 for storage. Among them, the finished product storage tank 507 is used as a buffer and storage container for temporarily storing the condensed 2-ethylanthraquinone.

[0123] The discharge port of the condensation crystallization slicer 509 is connected to the reflux storage tank 511 through a pipeline, and the reflux storage tank 511 is connected to the high-level finished product tank 508 through a pipeline. During the slicing process, the 2-ethylanthraquinone fine product that is not completely condensed and crystallized enters the reflux storage tank 511 through the discharge port of the condensation crystallization slicer 509 for temporary storage. When needed, these 2-ethylanthraquinone fine products are pumped back into the high-level finished product tank 508, mixed with new 2-ethylanthraquinone fine products, and sliced ​​again. This circulation loop not only improves the utilization rate of raw materials, but also improves the purity of the final product.

[0124] The overflow port of the rising film evaporator 502 is connected to the feed port of the scraper evaporator 520 through an overflow pipe 505 .

[0125] A gas collecting port is also installed on one side of the middle of the rising film evaporator 502 , and the gas collecting port is connected to the gas outlet of the scraper evaporator 520 through a steam pipe 504 .

[0126] The liquid discharge port of the scraper evaporator 520 is connected to the residue kettle 519 through a pipeline.

[0127] When the crude 2-ethylanthraquinone in the rising film evaporator 502 reaches a preset liquid level, the excess material will enter the scraper evaporator 520 through the overflow port to ensure that the rising film evaporator 502 will not be overloaded. In the scraper evaporator 520, the crude 2-ethylanthraquinone solution is evaporated to form gaseous 2-ethylanthraquinone, which is introduced into the rising film evaporator 502 through the steam pipe 504, mixed with the gaseous 2-ethylanthraquinone formed by the rising film evaporator 502, and finally sent to the condenser 506 from the top of the rising film evaporator 502 for condensation. The crude 2-ethylanthraquinone solution is heated in the scraper evaporator 520 and gradually converted into gaseous 2-ethylanthraquinone. As the evaporation proceeds, the concentration of impurities in the scraper evaporator 520 gradually increases, and finally a residue containing a high concentration of impurities is formed. The residue containing high concentration of impurities is collected and stored in the residue kettle 519. The residue in the residue kettle 519 is regarded as temporarily stored hazardous waste and needs to be entrusted to a qualified unit for disposal.

[0128] The crude product refining module 5 also includes a water jet vacuum unit 503, and the air suction end of the water jet vacuum unit 503 is connected to the finished product storage tank 507 and the high-position finished product tank 508 through pipelines. The water jet vacuum unit 503 provides power for the transportation of materials by generating a negative pressure environment. When the high-position finished product tank 508 is in a negative pressure state and the finished product storage tank 507 is at normal pressure, due to the existence of the pressure difference, the material in the finished product storage tank 507 is sucked into the high-position finished product tank 508 under the action of the negative pressure.

[0129] The exhaust port of the condenser 506 is connected to a non-condensable gas treatment device through a pipeline. The non-condensable gas treatment device includes a cold well 518, a first bag filter 517, a second bag filter 513 and a Roots vacuum pump group 512 which are sequentially connected along the gas treatment route. The air inlet of the cold well 518 is connected to the air outlet of the residue kettle 519 and the exhaust port of the condenser 506 through pipelines.

[0130] The dust removal capacity of the first bag filter 517 and the second bag filter 513 is limited, and they can only remove larger particles, but cannot filter out finer particles. In order to protect the Roots vacuum pump unit 512, a fine dust removal device is connected between the first bag filter 517 and the second bag filter 513. The fine dust removal device includes an oil dust collector 516, an oil circulation tank 515, and an oil removal circulation pump 514. The air outlet of the first bag filter 517 is connected to the air inlet of the oil dust collector 516 through a pipeline, and the air outlet of the oil dust collector 516 is connected to the air inlet of the second bag filter 513 through a pipeline. A liquid distributor is installed on the inner top of the oil dust collector 516, and the bottom of the oil dust collector 516 is connected to the input end of the oil removal circulation pump 514 through a pipeline, and the output end of the oil removal circulation pump 514 is connected to the liquid distributor through a pipeline.

[0131] During dust removal, the oil removal circulation pump 514 pumps the oil in the oil circulation tank 515 to the liquid distributor in the oil dust collector 516. The oil mist formed by the liquid distributor through spraying will collide with the particulate impurities in the gas and adhere to them, thereby removing fine particles. The oil containing the particles flows out from the bottom of the oil dust collector 516, and is sent back to the oil circulation tank 515 after filtration, thereby realizing the recycling of the oil.

[0132] The crude 2-ethylanthraquinone solution is pumped to the alkali adding kettle 501, and then 0.2% of the crude weight of the flake caustic soda is added and mixed, and the temperature of the alkali adding kettle 501 is controlled at 150°C. The mixed solution in the alkali adding kettle 501 is sent to the rising film evaporator 502 for film formation, and the temperature of the rising film evaporator 502 is controlled at 160°C. The mixed solution exceeding the set liquid level overflows to the scraper evaporator 520, and the temperature of the scraper evaporator 520 is controlled at 200°C. The gas phase 2-ethylanthraquinone evaporated from the scraper evaporator 520 is merged into the gas phase 2-ethylanthraquinone of the rising film evaporator 502 through the steam pipe 504. After the gas phase 2-ethylanthraquinone is condensed by the condenser 506, it enters the finished product storage tank 507 and the high-level finished product tank 508 in turn. The condensate in the high-level finished product tank 508 is transported to the condensation crystallization slicer 509 for slicing to form solid 2-ethylanthraquinone fine products.

[0133] With the above equipment, 2-ethylanthraquinone can be produced using a solid catalyst. Acylation is first completed inside the acylation hydrolysis reaction module 1, and then the measured 5% hydrochloric acid is pumped into the hydrolysis kettle 106, and the hydrolysis temperature is controlled at about 80°C with jacket cooling water to generate an organic mixture of 2-ethylbenzoylbenzoic acid, aluminum chloride and chlorobenzene. After the reaction, the reaction is kept warm and allowed to stand for stratification. The lower layer of acidic waste water containing aluminum chloride is sent to the polyaluminum chloride workshop to produce polyaluminum chloride after vacuum distillation, and the upper layer of 2-ethylbenzoylbenzoic acid and chlorobenzene solution remain in the hydrolysis kettle 106. Then, after washing with water, it enters the desolventizing and dehydrating module 2 for desolventizing and dehydrating, and then enters the closed-loop reaction module 3 in sequence. After the closed loop is completed, it enters the crude product cleaning and separation module 4 for alkali washing separation and water washing separation to obtain the crude product, which finally enters the crude product refining module 5 for refining to obtain the final product.

[0134] Obviously, the above embodiments are merely examples for the purpose of clear explanation, and are not intended to limit the implementation methods. For those skilled in the art, other different forms of changes or modifications can be made based on the above description. It is not necessary and impossible to list all the implementation methods here. The obvious changes or modifications derived therefrom are still within the scope of protection of the invention.

Claims

1. A 2-ethylanthraquinone synthesis production line, characterized in that: The invention comprises, in order of synthesis, an acylation hydrolysis reaction module (1), a desolventizing and dehydrating module (2), a closed-loop reaction module (3), a crude product washing and separation module (4), and a crude product refining module (5) connected by pipelines, wherein the closed-loop reaction module (3) comprises a feed buffer tank (301), a flash tank (322), and a plurality of reactors (328) arranged in a row, wherein the desolventizing and dehydrating module (2) is connected to the feed buffer tank (301) via a BE acid delivery pipe, wherein the feed buffer tank (301) is connected to a first feed port of a circulation tank (323) via a second delivery pipe (306), wherein a feed heater (305) is installed on the second delivery pipe (306), wherein a fifth delivery pipe (325) is installed at the discharge port of the circulation tank (323), wherein a A circulation heater (324), a second material conveying pipe (326) connected to a fifth conveying pipe (325) is installed at the bottom of a plurality of the reactors (328), a third conveying pipe (311) is installed at the second feed port of the circulation tank (323), a first material conveying pipe (310) connected to the third conveying pipe (311) is installed at the top of a plurality of the reactors (328), a fourth conveying pipe (314) is installed at the feed port of the flash tank (322), the fourth conveying pipe (314) is connected to the fifth conveying pipe (325) through a second conveying branch pipe (327) having the same number as the reactors (328), a reflux tower (321) is installed at one side of the flash tank (322), and the discharge port of the reflux tower (321) is connected to a toluene condenser (316) through a pipeline; The flash tank (322) is connected to the crude product cleaning and separation module (4) via a pipeline.

2. The 2-ethylanthraquinone synthesis production line according to claim 1, characterized in that: The closed-loop reaction module (3) further comprises a toluene washing tank (302), a first delivery pipe (303) being installed at a feed port of the toluene washing tank (302), the first material delivery pipe (310) being connected to the first delivery pipe (303) via a first delivery branch pipe (307), a sixth delivery pipe (331) being installed at a discharge port of the toluene washing tank (302), a washing toluene heater (304) being installed on the sixth delivery pipe (331), and the sixth delivery pipe (331) being connected to the second material delivery pipe (326) via a fourth delivery branch pipe (330).

3. The 2-ethylanthraquinone synthesis production line according to claim 1, characterized in that: The closed-loop reaction module (3) further comprises a vacuum cooler (317), a second vacuum buffer tank (320), a third vacuum pump (319) and an exhaust gas cooler (318) which are connected in sequence via pipelines; a vacuum main pipe (315) is installed at the feed port of the vacuum cooler (317); and the vacuum main pipe (315) is connected to the corresponding reactor (328) via a plurality of sets of third delivery branches (329).

4. The 2-ethylanthraquinone synthesis production line according to claim 1, characterized in that: The acylation hydrolysis reaction module (1) comprises a chlorobenzene cleaning high-level tank (101), an ethylbenzene storage tank (116), and a feeding bin (114), all of which are connected to the acylation reaction kettle (112) through a pipeline. The acylation reaction kettle (112) is connected to the insulation kettle (111), the acylation liquid settling tank (105), the acylation liquid buffer tank (109), and the hydrolysis kettle (106) in sequence through pipelines. The insulation kettle (111), the acylation liquid settling tank (105), and the acylation liquid buffer tank (109) are all connected to the chlorobenzene cleaning high-level tank (101) through a chlorobenzene flushing pipeline (110); and the hydrolysis kettle (106) is connected to the desolventizing and dehydrating module (2) through a hydrolyzate delivery pipeline.

5. The 2-ethylanthraquinone synthesis production line according to claim 4, characterized in that: The ethylbenzene storage tank (116) is also connected to the ethylbenzene intermediate tank (103) via an ethylbenzene delivery pump (104).

6. The 2-ethylanthraquinone synthesis production line according to claim 4, characterized in that: The desolventizing and dehydrating module (2) comprises a hydrolyzate separator (201) connected to a hydrolyzate delivery pipeline; the hydrolyzate separator (201) is connected to a first water-washing separator (203) via a first hydrolyzate pump (202); the first water-washing separator (203) is connected to a second water-washing separator (205) via a second hydrolyzate pump (204); the second water-washing separator (205) is also connected to a first countercurrent desolventizing tower (206), a second countercurrent desolventizing tower (207), and a BE acid desolventizing tower (208) via pipelines. The water kettle (209) and the BE acid metering tank (210) are connected in sequence; the second countercurrent desolventizing tower (207), the BE acid dehydration kettle (209), and the BE acid metering tank (210) are also connected to the vacuum dehydration condenser (211) through pipelines; the vacuum dehydration condenser (211) is connected to the first vacuum buffer tank (212) and the first vacuum pump (213) in sequence through pipelines; and the BE acid metering tank (210) is connected to the feed buffer tank (301) through a BE acid delivery pipe.

7. The 2-ethylanthraquinone synthesis production line according to claim 6, characterized in that: The hydrolyzate separator (201) is also connected to the aluminum liquid desolventizing kettle (215) via an aluminum chloride delivery pump (214); the top of the aluminum liquid desolventizing kettle (215) is also connected to an aluminum liquid condenser (216), a second separation tank (217), and a chlorobenzene receiving tank (218) in sequence via a pipeline; and the second separation tank (217) is also connected to a second vacuum pump (219) via a pipeline.

8. The 2-ethylanthraquinone synthesis production line according to claim 6, characterized in that: The crude product washing and separation module (4) comprises a primary alkali separator (404), a secondary alkali separator (405), a primary water separator (408), a secondary water separator (409), a toluene azeotropic tower (412), a plate condenser (410), a toluene oil-water separator (411), and a first intermediate tank (413) which are sequentially connected via pipelines. The bottom drain port of the toluene azeotropic tower (412) is connected to a finished product condenser (414) via a pipeline. The finished product condenser (414) The liquid outlet of the first alkali separator (404) is connected to a second intermediate tank (415) via a pipeline; one side of the first alkali separator (404) is connected to a feed pipe (401); the first alkali separator (404) is connected to a second alkali separator (405) via an eighth delivery pipe (419); the feed pipe (401) and the eighth delivery pipe (419) are also connected to the outlet of the liquid alkali high-level tank (406) via a liquid distribution pipe (420); and the second intermediate tank (415) is connected to a crude product refining module (5) via a pipeline.

9. The 2-ethylanthraquinone synthesis production line according to claim 8, characterized in that: The bottom discharge port of the primary alkali separator (404) is connected to the top reflux port via a first reflux pipe (403); the first reflux pipe (403) is also connected to the acid precipitation extraction kettle (422) via a seventh delivery pipe (402); the acid precipitation extraction kettle (422) is sequentially connected to the oil-water separation tower (428) and the oil-water separator (426) via pipelines; the bottom discharge port of the acid precipitation extraction kettle (422) is connected to the third intermediate tank (431) via a fourteenth delivery pipe (433); and the discharge port of the oil-water separator (426) is connected to the acid precipitation extraction kettle (422) via a fifth reflux pipe (424).

10. The 2-ethylanthraquinone synthesis production line according to claim 8, characterized in that: The crude product refining module (5) comprises an alkali adding kettle (501), a rising film evaporator (502), a condenser (506), a finished product storage tank (507), and a high-position finished product tank (508) which are sequentially connected via pipelines. The alkali adding kettle (501) is connected to the second intermediate tank (415) via a pipeline. The high-position finished product tank (508) is connected to the feed port of a condensation crystallization slicer (509) via a pipeline. The condensation crystallization slicer (509) is located above the silo (510). The overflow port of the rising film evaporator (502) is connected to the feed port of a scraper evaporator (520) via an overflow pipe (505). The air outlet of the scraper evaporator (520) is connected to the air collecting port of the rising film evaporator (502) through a steam pipe (504); the exhaust port of the condenser (506) is connected to the cold well (518) through a pipe; the cold well (518) is connected to the first bag filter (517), the second bag filter (513) and the Roots vacuum pump unit (512) in sequence through a pipe; the liquid discharge port of the scraper evaporator (520) is connected to the residue kettle (519) through a pipe; the air outlet of the residue kettle (519) and the exhaust port of the condenser (506) are both connected to the air inlet of the cold well (518) through a pipe.

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