CN218924678U - Synthesis device of 2- (4-ethylbenzoyl) benzoic acid - Google Patents

Synthesis device of 2- (4-ethylbenzoyl) benzoic acid Download PDF

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Publication number
CN218924678U
CN218924678U CN202223072501.XU CN202223072501U CN218924678U CN 218924678 U CN218924678 U CN 218924678U CN 202223072501 U CN202223072501 U CN 202223072501U CN 218924678 U CN218924678 U CN 218924678U
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China
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tank
photochemical reactor
benzoic acid
ethylbenzoyl
filter
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CN202223072501.XU
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郭梦莉
张猛
孙顺平
宋君
王梓铭
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Shandong Minji New Material Technology Co ltd
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Shandong Minji New Material Technology Co ltd
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/584—Recycling of catalysts

Abstract

The utility model relates to a chemical synthesis device, in particular to a 2- (4-ethyl benzoyl) benzoic acid synthesis device which comprises a mixing tank, wherein the mixing tank is respectively connected with a chlorobenzene storage tank and an ethylbenzene storage tank, the mixing tank is connected with a phthalic anhydride storage tank through a quantitative auger, the mixing tank is connected with a catalyst storage tank through a quantitative feeder, the mixing tank is also connected with a preheater, the preheater is respectively connected with a first photochemical reactor, a second photochemical reactor, a third photochemical reactor and a fourth photochemical reactor, the first photochemical reactor, the second photochemical reactor, the third photochemical reactor and the fourth photochemical reactor are respectively connected with a reaction intermediate tank, the reaction intermediate tank is respectively connected with a first filter and a second filter, and the first filter and the second filter are respectively connected with a product storage tank. The utility model has strong operability and avoids the environment pollution and the equipment corrosion caused by a large amount of acid wastewater.

Description

Synthesis device of 2- (4-ethylbenzoyl) benzoic acid
Technical Field
The utility model relates to a chemical synthesis device, in particular to a synthesis device of 2- (4-ethyl benzoyl) benzoic acid.
Background
2- (4-ethylbenzoyl) benzoic acid is abbreviated as BE acid, and the chemical formula is C 16 H 14 O 3 The method is widely used as hydrogen peroxide working carrier, dye intermediates, photosensitive material raw materials and the like, and is an important intermediate for synthesizing 2-ethyl anthraquinone.
The existing preparation method of 2- (4-ethyl benzoyl) benzoic acid takes ethyl benzene and phthalic anhydride as raw materials, and takes Friedel-crafts reaction in an organic solvent under the catalysis of aluminum trichloride to synthesize an aluminum complex BE salt; the BE acid aluminum double salt is hydrolyzed in an acidic aqueous solution to generate an organic solution of BE acid, and the reaction solvent is removed to obtain pure BE acid.
The existing catalyst for synthesizing 2- (4-ethyl benzoyl) benzoic acid is mainly anhydrous aluminum trichloride, and has the defects of complex two-step reaction process, large catalyst dosage, easy formation of complex, serious environmental pollution caused by a large amount of acid wastewater, no recycling and the like, although the activity is high, and the requirement of green development cannot be met.
Chinese patent CN 111747839A discloses a method for synthesizing 2- (4-ethylbenzoyl) benzoic acid, comprising the steps of: 1) In a 1000ml glass reaction kettle, adding 500g of ethylbenzene and 75g of nitrobenzene, starting stirring, adding 150g of phthalic anhydride (phthalic anhydride), starting a cooling system, cooling the system to 15 ℃, slowly adding 270g of aluminum trichloride, adding for about 1.5h, slowly increasing the system temperature along with the aluminum trichloride, controlling the system temperature to slowly increase to 19 ℃, and after the aluminum trichloride is added in multiple times, increasing the reaction temperature to 27 ℃, closing the cooling system, and continuously maintaining the state for 2h to obtain a reaction solution. 2) 900g of 5% diluted hydrochloric acid is added into a 2000ml glass reaction kettle, and the reaction liquid is slowly put into hydrochloric acid for hydrolysis, the hydrolysis temperature is controlled at 85 ℃, and the hydrolysis is carried out for 2 hours. 3) After the hydrolysis is finished, separating a lower water layer, distilling an upper water layer by using steam to remove chlorobenzene and nitrobenzene, adding water, cooling, separating out a large amount of white solid by using a system, filtering, and drying to obtain 246g of product. In the patent, aluminum trichloride is used as a catalyst to prepare 2- (4-ethyl benzoyl) benzoic acid in a conventional reaction kettle, the process is complicated, and a large amount of acid wastewater produced not only pollutes the environment but also severely corrodes equipment.
Disclosure of Invention
According to the defects in the prior art, the technical problems to be solved by the utility model are as follows: the synthesis device of the 2- (4-ethylbenzoyl) benzoic acid is provided, so that a large amount of acid wastewater is avoided, and the equipment maintenance cost is reduced.
The technical scheme adopted for solving the technical problems is as follows:
the utility model relates to a device for synthesizing 2- (4-ethylbenzoyl) benzoic acid, which comprises a mixing tank, wherein the mixing tank is respectively connected with a chlorobenzene storage tank and an ethylbenzene storage tank, the mixing tank is connected with a phthalic anhydride storage tank through a quantitative auger, the mixing tank is connected with a catalyst storage tank through a quantitative feeder, the mixing tank is also connected with a preheater, the preheater is respectively connected with a first photochemical reactor, a second photochemical reactor, a third photochemical reactor and a fourth photochemical reactor, the first photochemical reactor, the second photochemical reactor, the third photochemical reactor and the fourth photochemical reactor are respectively connected with a reaction intermediate tank, the reaction intermediate tank is respectively connected with a first filter and a second filter, and the first filter and the second filter are respectively connected with a product storage tank.
The mixing tank is internally provided with a first stirrer.
A first centrifugal pump is arranged between the mixing tank and the preheater.
The reaction intermediate tank is respectively connected with the first filter and the second filter through a second centrifugal pump.
The catalyst storage tank, the muffle furnace, the grinder, the dryer and the aging tank are sequentially connected with the stirring tank, and the stirring tank is respectively connected with the first stirring tank and the second stirring tank.
The inside of stirred tank be provided with the second agitator.
The top of first agitator tank be provided with first feed inlet.
The first stirring tank is internally provided with a third stirrer.
The top of the second stirring tank is provided with a second feeding hole.
The second stirring tank is internally provided with a fourth stirrer.
The utility model adopts a sol-gel method to prepare the photocatalyst Nd/ZnO-TiO 2 By Nd/ZnO-TiO 2 The photocatalyst is used for carrying out photocatalysis synthesis on 2- (4-ethyl benzoyl) benzoic acid which is an intermediate of 2-ethyl anthraquinone.
Working principle and process:
firstly, absolute ethyl alcohol is added into a first stirring tank from a first feed inlet, tetrabutyl titanate is added into the first stirring tank from the first feed inlet, and a third stirrer is started to stir, so that a material A is obtained; firstly, absolute ethyl alcohol is added into a second stirring tank from a second feed port, deionized water, glacial acetic acid, zinc nitrate and neodymium nitrate are sequentially added into the second stirring tank from the second feed port, and a fourth stirrer is started to stir, so that a material B is obtained; firstly, adding a material A into a stirring kettle, then adding a material B into the stirring kettle, and starting a second stirrer to stir to obtain gel; the gel enters an aging tank for aging, then sequentially enters a dryer for drying, is ground in a grinder, is calcined for 2 hours at 400-700 ℃ in a muffle furnace, and then Nd/ZnO-TiO is obtained 2 Photocatalyst, nd/ZnO-TiO 2 The photocatalyst enters a catalyst storage tank for storage for standby.
The phthalic anhydride is discharged from a phthalic anhydride storage tank and enters a mixing tank through a quantitative auger; chlorobenzene is discharged from a chlorobenzene storage tank and enters a mixing tank, ethylbenzene is discharged from an ethylbenzene storage tank and enters the mixing tank, and Nd/ZnO-TiO in a catalyst storage tank 2 The photocatalyst enters a mixing tank through a quantitative feeder, a first stirrer is started to stir, and the mixture is mixedPumping the good materials into a preheater through a first centrifugal pump for preheating, wherein the preheating temperature is 35-45 ℃; the preheated materials enter a first photochemical reactor, a second photochemical reactor, a third photochemical reactor and a fourth photochemical reactor, react for 2 hours under ultraviolet irradiation, then enter a reaction intermediate tank for continuous reaction, the materials obtained after the reaction are filtered and separated into a first filter and a second filter through a second centrifugal pump to obtain 2- (4-ethylbenzoyl) benzoic acid, and the 2- (4-ethylbenzoyl) benzoic acid enters a product storage tank for storage.
The utility model has the beneficial effects that: compared with the prior art that aluminum trichloride is adopted to prepare 2- (4-ethylbenzoyl) benzoic acid in a reaction kettle by a two-step method, the utility model adopts the photochemical reactor to prepare 2- (4-ethylbenzoyl) benzoic acid by one-step photocatalysis, has strong operability, and avoids producing a large amount of acid waste water to pollute the environment and corrode equipment.
Drawings
FIG. 1 is a schematic diagram of the structure of the present utility model;
in the figure: 1. a mixing tank; 2. a chlorobenzene storage tank; 3. an ethylbenzene storage tank; 4. a phthalic anhydride storage tank; 5. quantitative auger; 6. a catalyst storage tank; 7. a quantitative feeder; 8. a preheater; 9. a first photochemical reactor; 10. a second photochemical reactor; 11. a third photochemical reactor; 12. a fourth photochemical reactor; 13. a reaction intermediate tank; 14. a first filter; 15. a second filter; 16. a product storage tank; 17. a first agitator; 18. a first centrifugal pump; 19. a second centrifugal pump; 20. a muffle furnace; 21. a grinder; 22. a dryer; 23. an aging tank; 24. stirring kettle; 25. a first stirring tank; 26. a second stirring tank; 27. a second stirrer; 28. a first feed port; 29. a third agitator; 30. a second feed inlet; 31. and a fourth stirrer.
Detailed Description
Embodiments of the utility model are further described below with reference to the accompanying drawings:
as shown in FIG. 1, the utility model comprises a mixing tank 1, wherein the mixing tank 1 is respectively connected with a chlorobenzene storage tank 2 and an ethylbenzene storage tank 3, the mixing tank 1 is connected with a phthalic anhydride storage tank 4 through a quantitative auger 5, the mixing tank 1 is connected with a catalyst storage tank 6 through a quantitative feeder 7, the mixing tank 1 is also connected with a preheater 8, the preheater 8 is respectively connected with a first photochemical reactor 9, a second photochemical reactor 10, a third photochemical reactor 11 and a fourth photochemical reactor 12, the first photochemical reactor 9, the second photochemical reactor 10, the third photochemical reactor 11 and the fourth photochemical reactor 12 are respectively connected with a reaction intermediate tank 13, the reaction intermediate tank 13 is respectively connected with a first filter 14 and a second filter 15, and the first filter 14 and the second filter 15 are respectively connected with a product storage tank 16.
The mixing tank 1 is provided with a first stirrer 17 inside.
A first centrifugal pump 18 is arranged between the mixing tank 1 and the preheater 8.
The reaction intermediate tank 13 is connected to the first filter 14 and the second filter 15 by a second centrifugal pump 19, respectively.
The catalyst storage tank 6, the muffle furnace 20, the grinder 21, the dryer 22 and the aging tank 23 are sequentially connected with the stirring kettle 24, and the stirring kettle 24 is respectively connected with the first stirring tank 25 and the second stirring tank 26.
The inside of the agitation tank 24 is provided with a second agitator 27.
The top of the first agitator tank 25 is provided with a first feed port 28.
The first agitator tank 25 is provided with a third agitator 29 inside.
The top of the second agitator tank 26 is provided with a second feed port 30.
A fourth agitator 31 is provided inside the second agitator tank 26.
Firstly, absolute ethyl alcohol is added into a first stirring tank 25 from a first feed inlet 28, tetrabutyl titanate is added into the first stirring tank 25 from the first feed inlet 28, and a third stirrer 29 is started to stir, so that a material A is obtained; firstly, absolute ethyl alcohol is added into a second stirring tank 26 from a second feed port 30, deionized water, glacial acetic acid, zinc nitrate and neodymium nitrate are sequentially added into the second stirring tank 26 from the second feed port 30, and a fourth stirrer 31 is started to stir, so that a material B is obtained; the material A is added into the stirring kettle 24, the material B is added into the stirring kettle 24, and the second stirrer is started27, stirring to obtain gel; the gel enters an aging tank 23 for aging, then sequentially enters a dryer 22 for drying, is ground in a grinder 21, is calcined for 2 hours at 600 ℃ in a muffle furnace 20, and thus Nd/ZnO-TiO is obtained 2 Photocatalyst, nd/ZnO-TiO 2 The photocatalyst enters a catalyst storage tank 6 for storage.
Phthalic anhydride is discharged from a phthalic anhydride storage tank 4 and enters a mixing tank 1 through a quantitative auger 5; chlorobenzene is discharged from a chlorobenzene storage tank 2 and enters a mixing tank 1, ethylbenzene is discharged from an ethylbenzene storage tank 3 and enters the mixing tank 1, and Nd/ZnO-TiO in a catalyst storage tank 6 2 The photocatalyst enters the mixing tank 1 through the quantitative feeder 7, a first stirrer 17 is started to stir, and the mixed materials are pumped into the preheater 8 through a first centrifugal pump 18 to be preheated, wherein the preheating temperature is 40 ℃; the preheated materials enter a first photochemical reactor 9, a second photochemical reactor 10, a third photochemical reactor 11 and a fourth photochemical reactor 12, react for 2 hours under the irradiation of ultraviolet light, then enter a reaction intermediate tank 13 for continuous reaction, the materials obtained after the reaction enter a first filter 14 and a second filter 15 through a second centrifugal pump 19 for filtering and separating the catalyst, and the obtained 2- (4-ethylbenzoyl) benzoic acid and the 2- (4-ethylbenzoyl) benzoic acid enter a product storage tank 16 for storage.

Claims (10)

1. The utility model provides a synthesizer of 2- (4-ethyl benzoyl) benzoic acid, including blending tank (1), its characterized in that blending tank (1) links to each other with chlorobenzene storage tank (2) respectively, ethylbenzene storage tank (3), blending tank (1) is connected phthalic anhydride storage tank (4) through ration auger (5), blending tank (1) is connected catalyst storage tank (6) through ration feeder (7), blending tank (1) still links to each other with preheater (8), preheater (8) link to each other with first photochemical reactor (9) respectively, second photochemical reactor (10), third photochemical reactor (11), fourth photochemical reactor (12), first photochemical reactor (9), second photochemical reactor (10), third photochemical reactor (11) and fourth photochemical reactor (12) link to each other with reaction intermediate tank (13) respectively, reaction intermediate tank (13) link to each other with first filter (14), second filter (15), first filter (14) and second filter (15) link to each other with product storage tank (16) respectively.
2. The synthesis apparatus of 2- (4-ethylbenzoyl) benzoic acid according to claim 1, wherein the mixing tank (1) is internally provided with a first stirrer (17).
3. The synthesis apparatus of 2- (4-ethylbenzoyl) benzoic acid according to claim 1, characterized in that a first centrifugal pump (18) is arranged between the mixing tank (1) and the preheater (8).
4. The device for synthesizing 2- (4-ethylbenzoyl) benzoic acid according to claim 1, wherein the reaction intermediate tank (13) is connected with the first filter (14) and the second filter (15) through a second centrifugal pump (19), respectively.
5. The device for synthesizing 2- (4-ethylbenzoyl) benzoic acid according to claim 1, wherein the catalyst storage tank (6), the muffle furnace (20), the grinder (21), the dryer (22) and the aging tank (23) are sequentially connected with the stirring tank (24), and the stirring tank (24) is respectively connected with the first stirring tank (25) and the second stirring tank (26).
6. The apparatus for synthesizing 2- (4-ethylbenzoyl) benzoic acid according to claim 5 wherein a second stirrer (27) is provided inside the stirring vessel (24).
7. The apparatus for synthesizing 2- (4-ethylbenzoyl) benzoic acid according to claim 5, wherein a first feed port (28) is provided at the top of the first stirring tank (25).
8. The apparatus for synthesizing 2- (4-ethylbenzoyl) benzoic acid according to claim 5 wherein a third stirrer (29) is provided inside the first stirring tank (25).
9. The apparatus for synthesizing 2- (4-ethylbenzoyl) benzoic acid according to claim 5, wherein a second feed port (30) is provided at the top of the second stirring tank (26).
10. The apparatus for synthesizing 2- (4-ethylbenzoyl) benzoic acid according to claim 5, wherein a fourth agitator (31) is provided inside the second agitation tank (26).
CN202223072501.XU 2022-11-18 2022-11-18 Synthesis device of 2- (4-ethylbenzoyl) benzoic acid Active CN218924678U (en)

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CN202223072501.XU CN218924678U (en) 2022-11-18 2022-11-18 Synthesis device of 2- (4-ethylbenzoyl) benzoic acid

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Application Number Priority Date Filing Date Title
CN202223072501.XU CN218924678U (en) 2022-11-18 2022-11-18 Synthesis device of 2- (4-ethylbenzoyl) benzoic acid

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CN218924678U true CN218924678U (en) 2023-04-28

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