Supergravity reaction device and application thereof

A reaction device and super-gravity technology, which can be used in feeding devices, chemical/physical/physical-chemical stationary reactors, and ozone oxidation to prepare carboxylic acids, etc. The catalyst can be regenerated to use benzoic acid, which is difficult to separate and purify, and achieve the effects of broad industrial application prospects, short reaction time, and high atom utilization.

Active Publication Date: 2019-07-19
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The thiophenone compounds used in the above two new methods are photocatalysts, which avoid the use of a large amount of acidic solvents and cobalt acetate or manganese acetate in the traditional synthesis of benzoic acid, but there are also shortcomings in this method, such as low utilization of light energy And the problem of light transmittance, resulting in a particularly long reaction time; in addition, the method uses organic small molecule thiophene ketones as catalysts, which will cause certain difficulties in the reproducible use of catalysts and the separation and purification of benzoic acid

Method used

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  • Supergravity reaction device and application thereof
  • Supergravity reaction device and application thereof
  • Supergravity reaction device and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031]Weigh 3 g of benzyl alcohol and dissolve it in 500 mL of ethyl acetate and place it in the storage tank, set the liquid flow meter to 100 L / h, the gas flow meter to 50 L / h, the gas phase ozone concentration to 30 mg / L, and the supergravity The reactor rotation speed was 800 rpm. After reacting for 30min, 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 2.37g of benzaldehyde with a yield of 80.5%.

[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).

Embodiment 2

[0034] Weigh 3 g of benzyl alcohol and dissolve it in 500 mL of methanol and place it in the liquid storage tank. 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 speed is 800 rpm. After reacting for 15min, 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 1.79 g of benzaldehyde with a yield of 61%.

[0035] 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

[0037] Weigh 3 g of benzyl alcohol and dissolve it in 500 mL of ethyl acetate and place it in the storage tank, set the liquid flow meter to 100 L / h, the gas flow meter to 100 L / h, and the gas phase ozone concentration to 50 mg / L, and the hypergravity reaction The engine speed is 500 rpm. After reacting for 30 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 0.44g of benzaldehyde with a yield of 15%.

[0038] 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 discloses a supergravity reaction device and application thereof, belongs to the technical field of fine organic synthesis, and solves the problems existing in existing preparation processes of benzaldehyde and benzoic acid. According to the invention, fluid is greatly sheared and crushed through a supergravity rotating packed bed and a high-speed rotating packing, a huge and rapidlyupdating phase interface is generated, and the microcosmic mixing and mass transfer process is greatly enhanced. Ozone is selected as an oxidizing agent, and the device has the advantages of greenness, high efficiency, no secondary pollution and the like. Low-toxicity low-boiling-point reagents such as dichloromethane and ethyl acetate are selected as solvents, and recycling is facilitated. The method has the advantages of being environmentally friendly, high in atom economy and the like, and has wide industrial application prospects.

Description

technical field [0001] The invention belongs to the technical field of fine organic synthesis, and in particular relates to a supergravity reaction device and its application. Background technique [0002] Benzaldehyde compounds are important organic synthesis intermediates and fine chemical products, widely used in medicine, dyes, spices, resins and other industries. At present, the production of benzaldehyde in China mainly adopts the process of chlorination and hydrolysis of toluene. The process is due to the extensive use of C1 2 The production process is cumbersome and the pollution is serious; and the residual chloride in the product cannot be completely removed, so it is difficult to be used in the fields of food and medicine. Although chlorine-free benzaldehyde can be obtained by direct liquid-phase air oxidation of toluene, it must be carried out under high temperature and pressure, but benzoic acid is the main product, and benzaldehyde is only a small amount of b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J19/18B01J19/00B01J4/02B01J4/00C07C45/40C07C47/54C07C51/34C07C63/06
CPCB01J4/001B01J4/02B01J19/0053B01J19/18B01J2204/002B01J2204/005C07C45/40C07C51/34C07C47/54C07C63/06
Inventor 焦纬洲高文强刘有智张东升
Owner ZHONGBEI UNIV
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