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Device and method for preparing benzoic acid from toluene

A technology of benzoic acid and toluene, applied in the field of devices for preparing benzoic acid from toluene, achieving broad industrial application prospects and high atom economy

Active Publication Date: 2019-07-05
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The present invention aims at problems such as the use of acidic solvents in the preparation of existing benzoic acid, and provides a device and method for preparing benzoic acid from toluene

Method used

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  • Device and method for preparing benzoic acid from toluene
  • Device and method for preparing benzoic acid from toluene
  • Device and method for preparing benzoic acid from toluene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Weigh 6g of toluene and dissolve it in 500 mL of ethyl acetate and place it in the liquid storage tank. Set the liquid flow meter to 100 L / h, the gas flow meter to 50 L / h, and the gas phase ozone concentration to be 30 mg / L. The speed is 800 rpm. After reacting for 60min, after removing the reaction solvent with a rotary evaporator, through silica gel column chromatography (eluent is V 石油醚 / V 乙酸乙酯 =5:1) to obtain 3.2 g of benzoic acid with a yield of 40.5%.

[0026] 1 H NMR (600 MHz, CDCl 3 ) δ 10.02 (s, 1H), 7.88 (d, J = 12 Hz, 2H), 7.63 (t, J = 6 Hz, 1H), 7.53 (t, J = 6 Hz, 2H).

Embodiment 2

[0028] Weigh 6 g of toluene dissolved in 500 mL of methanol and put it in the storage tank, add 1.1 g of hydrogen peroxide (30%), set the liquid flow meter to 100 L / h, the gas flow meter to 70 L / h, and the gas phase ozone concentration to 80 mg / L, the rotation speed of the high gravity reactor is 800rpm. Reaction 80min, after removing reaction solvent with rotary evaporator, through silica gel column chromatography (eluent is V 石油醚 / V 乙酸乙酯 =5:1) to obtain 1.79 g of benzoic acid with a yield of 61%.

[0029] 1 H NMR (600 MHz, CDCl 3 ) δ 10.02 (s, 1H), 7.88 (d, J = 12 Hz, 2H), 7.63 (t, J = 6 Hz, 1H), 7.53 (t, J = 6 Hz, 2H).

Embodiment 3

[0031] Weigh 6 g of toluene and dissolve it in 500 mL of ethyl acetate and place it in the storage tank, add 2.2 g of hydrogen peroxide (30%), set the liquid flow meter to 100 L / h, the gas flow meter to 100 L / h, and the gas phase ozone concentration to be 50 mg / L, the rotation speed of the hypergravity reactor is 500 rpm. After reacting for 120 min, remove the reaction solvent with a rotary evaporator, and perform silica gel column chromatography (eluent is V 石油醚 / V 乙酸乙酯 =5:1) to obtain 6.7 g of benzoic acid with a yield of 85%.

[0032] 1 H NMR (600 MHz, CDCl 3 ) δ 10.02 (s, 1H), 7.88 (d, J = 12 Hz, 2H), 7.63(t, J = 6 Hz, 1H), 7.53 (t, J = 6 Hz, 2H).

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Abstract

The invention relates to a device and method for preparing benzoic acid from toluene, and belongs to the technical field of fine organic synthesis. In view of the problems in a current preparation method of benzoic acid, the invention provides the method. According to the method provided by the invention, a super-gravity rotating packed bed is utilized, a fluid is greatly sheared and crushed by utilizing a high-speed rotating filler to generate a huge quickly-updated phase interface, so that the micromixing and mass transfer process are greatly strengthened; ozone is selected as an oxidant, hydrogen peroxide is selected as a catalyst, so that the method has the advantages of greenness, high efficiency and no secondary pollution; low-toxicity low-boiling-point reagents such as dichloromethane and ethyl acetate are selected as a solvent, so that recovery is facilitated; and the method has the advantages of greenness, environmental protection and high atomic economy, thereby having broadindustrial application prospects.

Description

technical field [0001] The invention belongs to the technical field of fine organic synthesis, and in particular relates to a device and a method for preparing benzoic acid from toluene. Background technique [0002] Benzoic acid is the simplest aromatic acid, also known as benzoic acid. Benzoic acid is slightly soluble in water, but easily soluble in organic solvents such as ethyl acetate, dichloromethane, ether, etc. Benzoic acid is an important chemical raw material, which can be used to prepare benzoic acid salicylic acid paste; benzoic acid and sodium benzoate are often used as preservatives in food; used to prepare chemical products such as spices and plasticizers, such as benzoate. In addition, benzoic acid forms corresponding esters with diethylene glycol and triethylene glycol respectively, which are widely used in the fields of resins and coatings. [0003] There are three traditional methods for synthesizing benzoic acid, which are toluene chlorination hydrolysis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/265C07C63/06
CPCC07C51/265C07C63/06
Inventor 焦纬洲高文强刘有智杜磊
Owner ZHONGBEI UNIV
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