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Method for producing ethoxyquinoline

A technology of ethoxyquinoline and production method, which is applied in the direction of chemical instruments and methods, animal feed, additional food elements, etc., can solve the problems of low production efficiency, strong corrosion of equipment, slow synthesis reaction speed, etc., and achieve convenient scale The effects of efficient production, no discharge of waste water, and increased product yield

Inactive Publication Date: 2009-08-26
SANMENXIA XIAWEI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method is cumbersome to operate, resulting in a large amount of waste of solvents, the use of strong acid catalysts is highly corrosive to equipment, and a large amount of waste water is generated to cause environmental pollution, and the synthesis reaction speed is slow, the production efficiency is low, and it is not suitable for large-scale industrial production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0009] Example 1, the production method of ethoxyquinoline, 1600kg p-aminophenethyl ether, 180kg catalyst p-toluenesulfonic acid and 5kg zinc chloride, 500kg toluene are added in the reactor successively, under heating state, make material pass through by circulation pump Circulate between the axial adiabatic fixed-bed reactor with metal corrugated orifice packing and the reactor. Control the temperature of the kettle and start adding 1600kg of acetone dropwise at 120°C. Add acetone dropwise for about 22-24 hours to perform cyclization and detect the cyclization rate. After reaching 90.0%, stop dripping, keep warm for 2 hours, wash with water, let it stand, discharge the washing water to recover the catalyst, transfer the upper layer material to the distillation kettle, carry out vacuum distillation, distill toluene at the kettle temperature of 100-160°C, and distill the toluene at the kettle temperature of 160 Distill unreacted p-aminophenethyl ether and the generated ethoxyqu...

example 2

[0010] Example 2, the production method of ethoxyquinoline, 2000kg p-aminophenethyl ether, 200kg catalyst p-toluenesulfonic acid and 5kg zinc chloride, 650kg toluene are added in the reactor successively, under heating state, make material pass through by circulation pump Circulate between the axial adiabatic fixed-bed reactor with metal corrugated orifice packing and the reactor. Control the temperature of the kettle and start adding 1980kg of acetone dropwise at 130°C. Add acetone dropwise for about 22-24 hours to perform cyclization and detect the cyclization rate. After reaching 90.0%, stop dripping, keep warm for 2 hours, wash with water, let it stand, discharge the washing water to recover the catalyst, transfer the upper layer material to the distillation kettle, carry out vacuum distillation, distill toluene at the kettle temperature of 100-160°C, and distill the toluene at the kettle temperature of 160 Distill unreacted p-aminophenethyl ether and the generated ethoxyqu...

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Abstract

The invention discloses a method for producing ethoxyquinoline. The method comprises the following steps: adding materials, namely para aminophenyl ethyl ether, a composite catalyst and toluene, into a reaction kettle in sequence; under a heating state, circulating the materials between an axial adiabatic fixed bed reactor filled through a metal corrugated pore plate by a circulating pump; dripping acetone into the kettle at a temperature of between 120 and 145 DEG C for about 22 to 24 hours to carry out cyclize; stopping dripping after cyclization rate is detected to reach 90.0 percent; preserving the temperature for 2 hours; washing and keeping the mixture stand; draining scouring water and reclaiming the catalyst; transferring upper materials into a distillation still to be distilled; distilling toluene at the still temperature of between 100 and 160 DEG C; distilling a low-boiling-point substance at the still temperature of between 160 and 175 DEG C; distilling front-end volatiles at the still temperature of between 175 and 190 DEG C; and distilling the product at the still temperature of between 190 and 240 DEG C. The method has the advantages of reduction of synthesis time, improvement of product yield, high production efficiency, non waste water drainage and scale production convenience.

Description

technical field [0001] The invention relates to a production method of a feed additive, in particular to a production method of ethoxyquinoline. Background technique [0002] Ethoxyquinoline, whose chemical name is 6-ethoxy-2,2,4-trimethyl-1,2-dihydroquinoline, is a high-efficiency feed additive and is also widely used as a rubber antioxidant . The Chinese patent No. 200510023419.X discloses a production method of ethoxyquinoline, which uses p-aminophenethyl ether and acetone as raw materials, in the presence of an acid catalyst and a solvent, under the condition of 140°C to 160°C Carry out the dehydration condensation reaction, replace the solvent in the water trap at the later stage of the reaction, so that the p-aminophenetole is completely converted in one reaction. The method is cumbersome to operate, resulting in a large amount of solvent waste, the use of a strong acid catalyst is highly corrosive to equipment, and a large amount of waste water is generated to cause...

Claims

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Application Information

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IPC IPC(8): C07D215/20B01J31/02B01J27/10A23K1/16C08K5/3437A23K20/132
CPCY02P20/584
Inventor 薛建启赵峰张小峡
Owner SANMENXIA XIAWEI CHEM
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