A kind of production method of ethoxyquinoline

Abstract

The invention discloses a production method of ethoxyquinoline, which adopts the circulation between the static mixer and the reactor. Compared with the reactor, the static mixer can ensure the forced mixing and contact of the whole liquid flow, greatly The mass transfer effect is increased, and the pressure drop and energy consumption of the static mixer are low, which reduces the production cost. The total reaction time is 23-26 hours, the conversion rate of p-aminophenetole is greater than 97.0%, and the content of p-aminophenethyl ether in the ethoxyquinoline product is less than 0.4wt%.

Description

technical field

[0001] The invention relates to a production method of an organic compound, in particular to a production method of ethoxyquinoline, which is added to feed as an antioxidant. Background technique

[0002] Ethoxyquinoline, whose chemical name is 6-ethoxy-2,2,4-trimethyl-1,2-dihydroquinoline, is a high-efficiency antioxidant feed additive and is widely used in the world use. A production method of ethoxyquinoline is disclosed in Chinese patent 200910064564.0. During the reaction, a circulation pump is used to circulate the material through the axial adiabatic fixed-bed reactor and the reaction kettle filled with metal corrugated orifice plates. Method Due to the great resistance of the axial adiabatic fixed-bed reactor filled with metal corrugated orifice plates, the energy consumption is also increased and the production cost is increased. Contents of the invention

[0003] The object of the invention is to provide a kind of production method of ethoxyqui...

Examples

Embodiment 1

[0010] Add 1000 kilograms of p-aminophenethyl ether, 100 kilograms of toluene and 125 kilograms of p-toluenesulfonic acid in the reactor, open the circulating pump under heating to circulate the material between the static mixer and the reactor, when the temperature of the reactor material reaches Add 1050 kg of acetone dropwise at 140°C for 24 hours to carry out dehydration and cyclization, stop adding acetone after the conversion rate of p-aminophenethyl ether reaches 97.0% by gas chromatography, and then keep warm for 1 hour to neutralize Wash with water, distill the obtained organic layer, separate and remove toluene and unreacted p-aminophenetole, distill at 150-200°C at still temperature to obtain 1500 kilograms of ethoxyquinoline, and the content of ethoxyquinoline is 96.5wt%. The aminophenetole content is 0.30wt%.

Embodiment 2

[0012] Add 1000 kilograms of p-aminophenethyl ether, 100 kilograms of toluene and 125 kilograms of p-toluenesulfonic acid in the reactor, open the circulating pump under heating to circulate the material between the static mixer and the reactor, when the temperature of the reactor material reaches Add 1050 kg of acetone dropwise at 150°C for 26 hours for dehydration and cyclization, stop adding acetone after the conversion rate of p-aminophenethyl ether reaches 98.5% by gas chromatography, and then keep warm for 1 hour to neutralize Wash with water, distill the obtained organic layer, separate and remove toluene and unreacted p-aminophenetole, distill at 150-200°C at still temperature to obtain 1450 kilograms of ethoxyquinoline, and the content of ethoxyquinoline is 97.5wt%. The content of aminophenetole is 0.1wt%.

technical field

[0001] The invention relates to a production method of an organic compound, in particular to a production method of ethoxyquinoline, which is added to feed as an antioxidant. Background technique

[0002] Ethoxyquinoline, whose chemical name is 6-ethoxy-2,2,4-trimethyl-1,2-dihydroquinoline, is a high-efficiency antioxidant feed additive and is widely used in the world use. A production method of ethoxyquinoline is disclosed in Chinese patent 200910064564.0. During the reaction, a circulation pump is used to circulate the material through the axial adiabatic fixed-bed reactor and the reaction kettle filled with metal corrugated orifice plates. Method Due to the great resistance of the axial adiabatic fixed-bed reactor filled with metal corrugated orifice plates, the energy consumption is also increased and the production cost is increased. Contents of the invention

[0003] The object of the invention is to provide a kind of production method of ethoxyqui...

Examples

Embodiment 1

[0010] Add 1000 kilograms of p-aminophenethyl ether, 100 kilograms of toluene and 125 kilograms of p-toluenesulfonic acid in the reactor, open the circulating pump under heating to circulate the material between the static mixer and the reactor, when the temperature of the reactor material reaches Add 1050 kg of acetone dropwise at 140°C for 24 hours to carry out dehydration and cyclization, stop adding acetone after the conversion rate of p-aminophenethyl ether reaches 97.0% by gas chromatography, and then keep warm for 1 hour to neutralize Wash with water, distill the obtained organic layer, separate and remove toluene and unreacted p-aminophenetole, distill at 150-200°C at still temperature to obtain 1500 kilograms of ethoxyquinoline, and the content of ethoxyquinoline is 96.5wt%. The aminophenetole content is 0.30wt%.

Embodiment 2

[0012] Add 1000 kilograms of p-aminophenethyl ether, 100 kilograms of toluene and 125 kilograms of p-toluenesulfonic acid in the reactor, open the circulating pump under heating to circulate the material between the static mixer and the reactor, when the temperature of the reactor material reaches Add 1050 kg of acetone dropwise at 150°C for 26 hours for dehydration and cyclization, stop adding acetone after the conversion rate of p-aminophenethyl ether reaches 98.5% by gas chromatography, and then keep warm for 1 hour to neutralize Wash with water, distill the obtained organic layer, separate and remove toluene and unreacted p-aminophenetole, distill at 150-200°C at still temperature to obtain 1450 kilograms of ethoxyquinoline, and the content of ethoxyquinoline is 97.5wt%. The content of aminophenetole is 0.1wt%.

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