Device for recovering 2-(4 '-ethylbenzoyl) benzoic acid from acylated hydrolysate

Abstract

The utility model discloses a device for recovering 2-(4 '-ethylbenzoyl) benzoic acid from acylation hydrolysate, and relates to the technical field of 2-ethyl anthraquinone production, an outlet of an acylation hydrolysate tank is communicated with a first standing layering tank through a pipeline, an outlet of an organic phase recovery tank is communicated with a reaction kettle through a pipeline, and the reaction kettle is communicated with a second standing layering tank through a pipeline. An outlet of the reaction kettle is communicated with a second standing layering tank through a pipeline, an outlet of the water phase recovery tank is communicated with a neutralization tank through a pipeline, an outlet of the neutralization tank is communicated with a third standing layering tank through a pipeline, and an outlet of the third standing layering tank is communicated with a 2-(4 '-ethylbenzoyl) benzoic acid tank through a pipeline. According to the method, chlorobenzene is subjected to desolvation without heating evaporation, the cost is saved, in addition, the possibility that chlorobenzene overflows at high temperature to damage the environment is greatly reduced, the whole process can be completed at low temperature, the operation safety is high, and meanwhile, the purity of the obtained 2-(4 '-ethylbenzoyl) benzoic acid is high through triple standing separation.

Description

Technical Field

[0001] The utility model relates to the technical field of 2-ethylanthraquinone production, in particular to a device for recovering 2-(4'-ethylbenzoyl)benzoic acid from acylated hydrolyzate. Background Art

[0002] 2-Ethylanthraquinone, light yellow powder or flaky solid, is commonly used in the industry to make hydrogen peroxide, dye intermediates, photocurable resin catalysts, photodegradable films, coatings and photosensitive polymerization initiators. In the domestic industry, ethylbenzene and phthalic anhydride are mainly used with aluminum chloride as a catalyst to generate the intermediate product 2-(4'-ethylbenzoyl) benzoic acid aluminum double salt. 2-(4'-ethylbenzoyl) benzoic acid is hydrolyzed in a hydrochloric acid solution to generate an organic solution of 2-(4'-ethylbenzoyl) benzoic acid.

[0003] At present, the organic solution of 2-(4'-ethylbenzoyl)benzoic acid is often evaporated and desolvated to obtain 2-(4'-ethylbenzoyl)benzoic acid solid, which consumes a lot of heat energy and increases the production cost. At the same time, there is a possibility of high-temperature overflow of the solvent during the evaporation process, which may pollute the environment. In addition, the solvent removal may not be thorough, and the obtained 2-(4'-ethylbenzoyl)benzoic acid has low purity, which affects the quality of subsequent products. Summary of the invention

[0004] The technical problem to be solved by the utility model is: in view of the deficiencies in the prior art, a device for recovering 2-(4'-ethylbenzoyl)benzoic acid from acylated hydrolyzate is provided, and the obtained 2-(4'-ethylbenzoyl)benzoic acid has high purity and low production cost.

[0005] In order to solve the above technical problems, the technical solution of the utility model is:

[0006] A device for recovering 2-(4'-ethylbenzoyl)benzoic acid from an acylated hydrolyzed liquid, comprising an acylated hydrolyzed liquid tank, the outlet of the acylated hydrolyzed liquid tank being connected to a first static stratification tank via a pipeline, the outlet of the first static stratification tank being connected to a hydrochloric acid recovery tank and an organic phase recovery tank via pipelines, the outlet of the organic phase recovery tank being connected to a reactor via a pipeline, the inlet of the reactor being connected to a sodium hydroxide tank via a pipeline, the outlet of the reactor being connected to a second static stratification tank via a pipeline, the outlet of the second static stratification tank being connected to a chlorobenzene recovery tank and an aqueous phase recovery tank via pipelines;

[0007] The outlet of the water phase recovery tank is connected to the neutralization tank through a pipeline, the inlet of the neutralization tank is connected to the dilute hydrochloric acid tank through a pipeline, the outlet of the neutralization tank is connected to the third static stratification tank through a pipeline, and the outlet of the third static stratification tank is connected to the 2-(4'-ethylbenzoyl)benzoic acid tank through a pipeline.

[0008] As an improved technical solution, a first density sensor is provided at the outlet of the first static stratification tank, a first cut-off valve is provided between the first static stratification tank and the hydrochloric acid recovery tank, a second cut-off valve is provided between the first static stratification tank and the organic phase recovery tank, and the first density sensor, the first cut-off valve and the second cut-off valve are interlocked to a control system.

[0009] As an improved technical solution, a second density sensor is provided at the outlet of the second static stratification tank, a third cut-off valve is provided between the second static stratification tank and the chlorobenzene recovery tank, a fourth cut-off valve is provided between the second static stratification tank and the water phase recovery tank, and the second density sensor, the third cut-off valve and the fourth cut-off valve are interlocked to a control system.

[0010] As an improved technical solution, the outlet of the third static stratification tank is connected to a sodium salt tank through a pipeline.

[0011] As an improved technical solution, a third density sensor is provided at the outlet of the third static stratification tank, a fifth cut-off valve is provided between the third static stratification tank and the 2-(4'-ethylbenzoyl)benzoic acid tank, a sixth cut-off valve is provided between the third static stratification tank and the sodium salt tank, and the third density sensor, the fifth cut-off valve and the sixth cut-off valve are interlocked to a control system.

[0012] As an improved technical solution, liquid level sensors are provided in the first static stratification tank, the second static stratification tank and the third static stratification tank.

[0013] As a preferred technical solution, the outlet of the organic phase recovery tank is provided with a first feed pump, and the outlet of the first feed pump is connected to the inlet of the first static stratification tank and the reactor through pipelines.

[0014] As a preferred technical solution, a second feed pump is provided at the outlet of the water phase recovery tank, and the outlet of the second feed pump is connected to the inlets of the second static stratification tank and the neutralization tank through pipelines.

[0015] Due to the adoption of the above technical solution, the beneficial effects of the utility model are:

[0016] The utility model discloses a device for recovering 2-(4'-ethylbenzoyl)benzoic acid from an acylated hydrolyzed liquid. The device comprises an acylated hydrolyzed liquid tank, the outlet of the acylated hydrolyzed liquid tank is connected with a first standing and stratification tank through a pipeline, the outlet of the first standing and stratification tank is respectively connected with a hydrochloric acid recovery tank and an organic phase recovery tank through pipelines, the outlet of the organic phase recovery tank is connected with a reactor through a pipeline, the inlet of the reactor is connected with a sodium hydroxide tank through a pipeline, the outlet of the reactor is connected with a second standing and stratification tank through a pipeline, the outlet of the second standing and stratification tank is respectively connected with a chlorobenzene recovery tank and a water phase recovery tank through pipelines; the outlet of the water phase recovery tank is connected with a neutralization tank through a pipeline, the inlet of the neutralization tank is connected with a dilute hydrochloric acid tank through a pipeline, the outlet of the neutralization tank is connected with a third standing and stratification tank through a pipeline, and the outlet of the third standing and stratification tank is connected with a 2-(4'-ethylbenzoyl)benzoic acid tank through a pipeline. The organic phase in the acylated water washing liquid is first separated by a first standing and stratification tank. At this time, the components of the organic phase are a mixed solution of 2-(4'-ethylbenzoyl)benzoic acid and chlorobenzene. Then, sodium hydroxide is added to react to generate 2-(4'-ethylbenzoyl)benzoic acid sodium salt which is dissolved in sodium hydroxide. Chlorobenzene is recovered by a second standing and stratification tank. Then, dilute hydrochloric acid is added to the 2-(4'-ethylbenzoyl)benzoic acid sodium salt. After the reaction, 2-(4'-ethylbenzoyl)benzoic acid is recovered. Since 2-(4'-ethylbenzoyl)benzoic acid is insoluble in dilute hydrochloric acid, it is precipitated from the solution, thereby realizing the recovery of 2-(4'-ethylbenzoyl)benzoic acid. There is no need to heat and evaporate the chlorobenzene for desolventizing, which saves costs and greatly reduces the possibility of damage to the environment caused by high-temperature overflow of chlorobenzene. The entire process can be completed at low temperature with high operational safety. At the same time, through triple static separation, the obtained 2-(4'-ethylbenzoyl)benzoic acid has high purity.

[0017] The outlet of the first static stratification tank of the utility model is provided with a first density sensor, a first cut-off valve is provided between the first static stratification tank and the hydrochloric acid recovery tank, a second cut-off valve is provided between the first static stratification tank and the organic phase recovery tank, and the first density sensor, the first cut-off valve and the second cut-off valve are interlocked to a control system. The control system can switch the opening and closing of the first cut-off valve and the second cut-off valve according to the value of the first density sensor, thereby improving the purity of the organic phase.

[0018] The outlet of the second static stratification tank is provided with a second density sensor, a third cut-off valve is provided between the second static stratification tank and the chlorobenzene recovery tank, a fourth cut-off valve is provided between the second static stratification tank and the water phase recovery tank, and the second density sensor, the third cut-off valve and the fourth cut-off valve are interlocked to a control system. The control system can switch the opening and closing of the third cut-off valve and the fourth cut-off valve according to the value of the second density sensor to prevent chlorobenzene from entering the water phase, resulting in the loss of 2-(4'-ethylbenzoyl)benzoic acid and the reduction of purity.

[0019] The outlet of the third static stratification tank is connected to a sodium salt tank through a pipeline. By collecting the sodium salt, a sodium chloride solution can be obtained, and sodium chloride can be produced as a byproduct later, thereby improving the economic benefits of production.

[0020] The outlet of the third static stratification tank is provided with a third density sensor, a fifth cut-off valve is provided between the third static stratification tank and the 2-(4'-ethylbenzoyl)benzoic acid tank, a sixth cut-off valve is provided between the third static stratification tank and the sodium salt tank, and the third density sensor, the fifth cut-off valve and the sixth cut-off valve are interlocked to a control system. The control system can switch the opening and closing of the fifth cut-off valve and the sixth cut-off valve according to the value of the third density sensor, and the separation effect of 2-(4'-ethylbenzoyl)benzoic acid and sodium salt is better, thereby improving the purity of subsequent products.

[0021] The first static stratification tank, the second static stratification tank and the third static stratification tank are all provided with liquid level sensors to maintain a suitable static liquid level and avoid overflow and low static efficiency caused by too low liquid level.

[0022] The outlet of the organic phase recovery tank is provided with a first feed pump, and the outlet of the first feed pump is connected to the inlet of the first static stratification tank and the reactor through pipelines. The liquid after static separation can be re-injected into the first static stratification tank for re-refining and recovery, and the separation is complete.

[0023] The outlet of the water phase recovery tank is provided with a second feed pump, and the outlet of the second feed pump is connected to the inlet of the second static stratification tank and the neutralization tank through pipelines. The liquid after static separation can be re-injected into the second static stratification tank for re-refining and recovery, and the separation is complete. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] The utility model is further described below in conjunction with the accompanying drawings and embodiments.

[0025] Figure 1 It is a schematic diagram of the structure of an embodiment of the utility model;

[0026] Wherein: 1. acylation hydrolysis liquid tank; 2. first standing stratification tank; 3. hydrochloric acid recovery tank; 4. organic phase recovery tank; 5. reactor; 6. sodium hydroxide tank; 7. second standing stratification tank; 8. chlorobenzene recovery tank; 9. aqueous phase recovery tank; 10. neutralization tank; 11. dilute hydrochloric acid tank; 12. third standing stratification tank; 13. 2-(4'-ethylbenzoyl)benzoic acid tank; 14. first density sensor; 15. first shut-off valve; 16. second shut-off valve; 17. second density sensor; 18. third shut-off valve; 19. fourth shut-off valve; 20. sodium salt tank; 21. third density sensor; 22. fifth shut-off valve; 23. sixth shut-off valve; 24. liquid level sensor; 25. first feed pump; 26. second feed pump. DETAILED DESCRIPTION

[0027] The present invention is further described below in conjunction with the accompanying drawings and embodiments.

[0028] like Figure 1As shown, a device for recovering 2-(4'-ethylbenzoyl)benzoic acid from an acylated hydrolyzed liquid comprises an acylated hydrolyzed liquid tank 1, the outlet of the acylated hydrolyzed liquid tank 1 is connected to a first standing and stratification tank 2 through a pipeline, the outlet of the first standing and stratification tank 2 is respectively connected to a hydrochloric acid recovery tank 3 and an organic phase recovery tank 4 through pipelines, the outlet of the organic phase recovery tank 4 is connected to a reactor 5 through a pipeline, the inlet of the reactor 5 is connected to a sodium hydroxide tank 6 through a pipeline, the outlet of the reactor 5 is connected to a second standing and stratification tank 7 through a pipeline, the outlet of the second standing and stratification tank 7 is respectively connected to a chlorobenzene recovery tank 8 and an aqueous phase recovery tank 9 through pipelines; the outlet of the aqueous phase recovery tank 9 is connected to a neutralization tank 10 through a pipeline, the inlet of the neutralization tank 10 is connected to a dilute hydrochloric acid tank 11 through a pipeline, the outlet of the neutralization tank 10 is connected to a third standing and stratification tank 12 through a pipeline, and the outlet of the third standing and stratification tank 12 is connected to a 2-(4'-ethylbenzoyl)benzoic acid tank through a pipeline. The organic phase in the acylated water washing liquid is first separated by the first standing and stratification tank 2. At this time, the components of the organic phase are a mixed solution of 2-(4'-ethylbenzoyl)benzoic acid and chlorobenzene. Then, sodium hydroxide is added to react to generate 2-(4'-ethylbenzoyl)benzoic acid sodium salt which is dissolved in sodium hydroxide. The chlorobenzene is recovered by the second standing and stratification tank 7. Then, dilute hydrochloric acid is added to the 2-(4'-ethylbenzoyl)benzoic acid sodium salt. After the reaction, 2-(4'-ethylbenzoyl)benzoic acid is recovered. Since 2-(4'-ethylbenzoyl)benzoic acid is insoluble in dilute hydrochloric acid, it is precipitated from the solution, thereby realizing the recovery of 2-(4'-ethylbenzoyl)benzoic acid. There is no need to heat and evaporate the chlorobenzene for desolventizing, which saves costs and greatly reduces the possibility of damage to the environment caused by high-temperature overflow of chlorobenzene. The entire process can be completed at low temperature with high operational safety. At the same time, through triple static separation, the obtained 2-(4'-ethylbenzoyl)benzoic acid has high purity.

[0029] A first density sensor 14 is provided at the outlet of the first static stratification tank 2, a first cut-off valve 15 is provided between the first static stratification tank 2 and the hydrochloric acid recovery tank 3, a second cut-off valve 16 is provided between the first static stratification tank 2 and the organic phase recovery tank 4, and the first density sensor 14, the first cut-off valve 15 and the second cut-off valve 16 are interlocked to the control system. The control system can switch the opening and closing of the first cut-off valve 15 and the second cut-off valve 16 according to the value of the first density sensor 14, thereby improving the purity of the organic phase.

[0030] A second density sensor 17 is provided at the outlet of the second static stratification tank 7, a third cut-off valve 18 is provided between the second static stratification tank 7 and the chlorobenzene recovery tank 8, a fourth cut-off valve 19 is provided between the second static stratification tank 7 and the water phase recovery tank 9, and the second density sensor 17, the third cut-off valve 18 and the fourth cut-off valve 19 are interlocked to the control system. The control system can switch the opening and closing of the third cut-off valve 18 and the fourth cut-off valve 19 according to the value of the second density sensor 17 to prevent chlorobenzene from entering the water phase, resulting in the loss of 2-(4'-ethylbenzoyl)benzoic acid and the reduction of purity.

[0031] The outlet of the third static stratification tank 12 is connected to the sodium salt tank 20 through a pipeline. By collecting the sodium salt, a sodium chloride solution can be obtained, and sodium chloride can be produced as a byproduct later, thereby improving the economic benefits of production.

[0032] The outlet of the third static stratification tank 12 is provided with a third density sensor 21, a fifth cut-off valve 22 is provided between the third static stratification tank 12 and the 2-(4'-ethylbenzoyl)benzoic acid tank, a sixth cut-off valve 23 is provided between the third static stratification tank 12 and the sodium salt tank 20, and the third density sensor 21, the fifth cut-off valve 22 and the sixth cut-off valve 23 are interlocked to the control system. The control system can switch the opening and closing of the fifth cut-off valve 22 and the sixth cut-off valve 23 according to the value of the third density sensor 21, and the separation effect of 2-(4'-ethylbenzoyl)benzoic acid and sodium salt is better, thereby improving the purity of subsequent products.

[0033] The first static stratification tank 2, the second static stratification tank 7 and the third static stratification tank 12 are all provided with liquid level sensors 24 to maintain a suitable static liquid level to avoid overflow and low static efficiency caused by too low liquid level.

[0034] The outlet of the organic phase recovery tank 4 is provided with a first feed pump 25, and the outlet of the first feed pump 25 is connected to the inlet of the first static stratification tank 2 and the reactor 5 through pipelines. The liquid after static separation can be pumped back into the first static stratification tank 2 for re-refining and recovery, and the separation is complete.

[0035] The outlet of the water phase recovery tank 9 is provided with a second feed pump 26, and the outlet of the second feed pump 26 is connected to the inlet of the second static stratification tank 7 and the neutralization tank 10 through pipelines. The liquid after static separation can be re-injected into the second static stratification tank 7 for re-refining and recovery, and the separation is complete.

[0036] It should be understood that these embodiments are only used to illustrate the present invention and are not used to limit the scope of the present invention. In addition, it should be understood that after reading the content taught by the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms also fall within the scope defined by the claims attached to this application.

Claims

1. A device for recovering 2-(4'-ethylbenzoyl)benzoic acid from an acylated hydrolyzate, comprising an acylated hydrolyzate tank, characterized in that: The outlet of the acylated hydrolyzed liquid tank is connected to a first static stratification tank through a pipeline, the outlet of the first static stratification tank is respectively connected to a hydrochloric acid recovery tank and an organic phase recovery tank through pipelines, the outlet of the organic phase recovery tank is connected to a reactor through a pipeline, the inlet of the reactor is connected to a sodium hydroxide tank through a pipeline, the outlet of the reactor is connected to a second static stratification tank through a pipeline, and the outlet of the second static stratification tank is respectively connected to a chlorobenzene recovery tank and an aqueous phase recovery tank through pipelines; The outlet of the water phase recovery tank is connected to the neutralization tank through a pipeline, the inlet of the neutralization tank is connected to the dilute hydrochloric acid tank through a pipeline, the outlet of the neutralization tank is connected to the third static stratification tank through a pipeline, and the outlet of the third static stratification tank is connected to the 2-(4'-ethylbenzoyl)benzoic acid tank through a pipeline.

2. A device for recovering 2-(4'-ethylbenzoyl)benzoic acid from an acylated hydrolyzate as claimed in claim 1, characterized in that: A first density sensor is provided at the outlet of the first static stratification tank, a first cut-off valve is provided between the first static stratification tank and the hydrochloric acid recovery tank, a second cut-off valve is provided between the first static stratification tank and the organic phase recovery tank, and the first density sensor, the first cut-off valve and the second cut-off valve are interlocked to a control system.

3. A device for recovering 2-(4'-ethylbenzoyl)benzoic acid from an acylated hydrolyzate as claimed in claim 1, characterized in that: A second density sensor is provided at the outlet of the second static stratification tank, a third cut-off valve is provided between the second static stratification tank and the chlorobenzene recovery tank, a fourth cut-off valve is provided between the second static stratification tank and the water phase recovery tank, and the second density sensor, the third cut-off valve and the fourth cut-off valve are interlocked to a control system.

4. A device for recovering 2-(4'-ethylbenzoyl)benzoic acid from an acylated hydrolyzate as claimed in claim 1, characterized in that: The outlet of the third static stratification tank is connected to the sodium salt tank through a pipeline.

5. A device for recovering 2-(4'-ethylbenzoyl)benzoic acid from an acylated hydrolyzate as claimed in claim 4, characterized in that: A third density sensor is provided at the outlet of the third static stratification tank, a fifth cut-off valve is provided between the third static stratification tank and the 2-(4'-ethylbenzoyl)benzoic acid tank, a sixth cut-off valve is provided between the third static stratification tank and the sodium salt tank, and the third density sensor, the fifth cut-off valve and the sixth cut-off valve are interlocked to a control system.

6. A device for recovering 2-(4'-ethylbenzoyl)benzoic acid from an acylated hydrolyzate as claimed in claim 1, characterized in that: Liquid level sensors are provided in the first static stratification tank, the second static stratification tank and the third static stratification tank.

7. A device for recovering 2-(4'-ethylbenzoyl)benzoic acid from an acylated hydrolyzate as claimed in claim 1, characterized in that: The outlet of the organic phase recovery tank is provided with a first feed pump, and the outlet of the first feed pump is connected to the inlet of the first static stratification tank and the reactor through pipelines.

8. A device for recovering 2-(4'-ethylbenzoyl)benzoic acid from an acylated hydrolyzate as claimed in claim 1, characterized in that: The outlet of the water phase recovery tank is provided with a second feed pump, and the outlet of the second feed pump is connected to the inlet of the second static stratification tank and the neutralization tank through pipelines.

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