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Synthesis method of 2-(4 '-ethylbenzoyl) benzoic acid

A technology of ethyl benzoyl and synthesis method, which is applied in the field of synthesis of 2-benzoic acid, can solve problems such as high chemical oxygen demand of aluminum trichloride wastewater, increased production cost, and difficulty in wastewater treatment, and achieve solvent recovery Difficulty, low product cost, and reduced processing difficulty

Pending Publication Date: 2020-10-09
WEIFANG MENJIE CHEM
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  • Abstract
  • Description
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Problems solved by technology

[0007] However, the above preparation methods have the following disadvantages respectively: Method 1, ethylbenzene and phthalic anhydride are used as raw materials, chlorobenzene, dichlorobenzene, etc. are used as solvents, and the Friedel-Crafts acylation reaction is carried out under aluminum chloride as a catalyst
Although it is a good solution to the problem of chlorine, because N-methylpyrrolidone is soluble in water, it has a higher boiling point
It cannot be recovered after reaction hydrolysis, and the chemical oxygen demand of aluminum trichloride wastewater is extremely high, which brings great difficulties to wastewater treatment and increases the production cost too much

Method used

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  • Synthesis method of 2-(4 '-ethylbenzoyl) benzoic acid
  • Synthesis method of 2-(4 '-ethylbenzoyl) benzoic acid
  • Synthesis method of 2-(4 '-ethylbenzoyl) benzoic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0026] The present embodiment adopts following raw materials, specifically see Table 1:

[0027] Table 1. Composition of raw materials

[0028] serial number raw material name Dosage percentage content 1 ethylbenzene 500g 99.5% 2 Nitrobenzene 75g 99.0% 3 Phthalic anhydride 150g 99.0% 4 Aluminum trichloride 270g 98.5% 5 hydrochloric acid 900g 5%

[0029] The synthetic method of 2-(4'-ethylbenzoyl) benzoic acid comprises the steps:

[0030] 1) In a 1000ml glass reactor, add 500g of ethylbenzene and 75g of nitrobenzene, start stirring, add 150g of phthalic anhydride (phthalic anhydride), start the cooling system, cool the system down to 15°C, and slowly add 270g of trichloro Aluminum, the dosing time is about 1.5h. With the input of aluminum trichloride, the temperature of the system will rise slowly, and the temperature of the control system will rise slowly to 19°C. After adding aluminum trichloride in batches, the rea...

Embodiment 2

[0036] The synthetic method of 2-(4'-ethylbenzoyl) benzoic acid comprises the steps:

[0037] 1) In a 1000ml glass reactor, add 500g of ethylbenzene and 75g of nitrobenzene, start stirring, add 150g of phthalic anhydride (phthalic anhydride), start the cooling system, cool the system down to 15°C, and slowly add 270g of trichloro Aluminum, the dosing time is about 1.5h. With the input of aluminum trichloride, the temperature of the system will rise slowly. The temperature of the control system is not higher than 20°C. After rising to 27°C, the cooling system was turned off, and the state continued for 2 hours to obtain a reaction liquid.

[0038] 2) Add 900g of dilute sulfuric acid with a concentration of 5% into a 2000ml glass reaction kettle, slowly put the reaction material liquid into hydrochloric acid for hydrolysis, control the hydrolysis temperature at 85°C, and the hydrolysis is complete.

[0039] 3) After the hydrolysis is completed, the lower water layer is separate...

Embodiment 3

[0041] In this example, on the basis of the methods in Example 1 and Example 2, one reaction condition was changed to ensure that the remaining reaction conditions remained unchanged, and the reactants (type and amount of acid), system temperature, hydrolysis temperature and hydrolysis time were studied respectively. impact on the product.

[0042] Table 2 records the effect on the product of using dilute hydrochloric acid and dilute sulfuric acid and changing the dosage of dilute hydrochloric acid and dilute sulfuric acid. Wherein group 1 is the experimental result of embodiment 1, and group 2, 3, 4 is to change the consumption of phthalic anhydride, the consumption of nitrobenzene, the consumption of dilute hydrochloric acid respectively on the basis of embodiment 1, group 5 is The experimental result of embodiment 2. It can be seen from the results that the different amounts of reactants will affect the content of 2-(4'-ethylbenzoyl)benzoic acid in the final product.

[0...

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Abstract

In order to prepare the 2-(4 '-ethylbenzoyl) benzoic acid which is low in chlorine content, capable of being industrially implemented, mild in production condition and relatively low in cost, the invention provides a synthesis method of the 2-(4'-ethylbenzoyl) benzoic acid. The synthesis method comprises the following steps: (1) adding nitrobenzene or nitromethane into ethylbenzene; (2) adding phthalic anhydride; (3) adding aluminum trichloride; (4) after the reaction is finished, adding a reaction solution into diluted hydrochloric acid or dilute sulfuric acid for hydrolysis; and (5) after the hydrolysis is finished, removing the water layer, distilling the solution after the water layer is removed by using water vapor, evaporating ethylbenzene and nitrobenzene, and filtering the remaining feed liquid to obtain the 2-(4 '-ethylbenzoyl) benzoic acid. According to the invention, the problems of high chlorine content and difficult solvent recovery in the product are solved, the reactionconditions are mild, and the temperature does not exceed 30 DEG C; meanwhile, the wastewater treatment difficulty is reduced, and the product cost is relatively low.

Description

technical field [0001] The invention relates to the field of compound synthesis, in particular to a method for synthesizing 2-(4'-ethylbenzoyl)benzoic acid. Background technique [0002] 2-(4'-Ethylbenzoyl)benzoic acid is an essential intermediate for the industrial production of 2-ethylanthraquinone, which is an organic intermediate with a wide range of uses. It is also the main auxiliary agent for the synthesis of hydrogen peroxide. Its reaction principle is as follows: [0003] [0004] [0005] However, during the hydrogen peroxide synthesis process, the control of chlorine and sulfur is very strict. Therefore, it is required that the chlorine content of 2-ethylanthraquinone is less than 40ppm and the sulfur content is less than 10ppm. And the source of chlorine is mainly in the chlorine content of 2-(4'-ethylbenzoyl)benzoic acid. How to prepare 2-(4'-ethylbenzoyl)benzoic acid with lower chlorine content has been an urgent problem in this industry. [0006] Th...

Claims

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Application Information

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IPC IPC(8): C07C51/083C07C51/42C07C51/44C07C65/34
CPCC07C51/083C07C51/42C07C51/445C07C65/34
Inventor 刘泉军唐建业周怀国
Owner WEIFANG MENJIE CHEM
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