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Industrial production method for ethoxy quinoline

A technology of ethoxyquinoline and its production method, applied in the direction of organic chemistry, etc., can solve problems such as poor product quality, many side reactions, and slow reaction speed

Inactive Publication Date: 2016-09-28
张加明 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] From the actual production situation, there are obvious defects in the above-mentioned production process, which are as follows: 1. The reaction speed is slow (24-46 hours), 2. The reaction is incomplete, and the residual raw materials are between 3-7%. There are many side reactions and poor product quality. 4. The post-processing is complicated. Most enterprises adopt the method of washing, pickling, alkali washing and rectifying for many times. 5. The pollution of the three wastes is large. A large amount of solid waste, 6. Low overall benefit

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A kind of industrialized production method of ethoxyquin, comprises the following steps:

[0031] In a 3000L reactor, add p-aminophenetole (1000kg), diluent (400kg), and catalyst (100kg) in sequence, raise the temperature to 125°C while stirring, and start adding acetone slowly, keeping the temperature at 125±5 ℃, the dropwise addition of acetone is completed, the reaction is kept for half an hour, and the sample is tested. If the raw material p-aminophenethyl ether at the end of the reaction is less than 0.05%, it is considered qualified, and the temperature is lowered to 60-80°C after passing the test.

[0032] Pump the materials in the above steps into the distillation kettle, and distill under normal pressure at a temperature of 60-140° C. to recover the diluent for mechanical use.

[0033] After the diluent was recovered, fractional distillation under reduced pressure was carried out, and the fraction at 142-160°C was collected under a vacuum of 0.098Mpa to obtain ...

Embodiment 2

[0036] In a 3000L reactor, add p-aminophenetole (1000kg), diluent (400kg), catalyst (100kg) in sequence, raise the temperature to 135°C under stirring, start to add acetone slowly, and keep the dropping temperature at 135°C ±5°C, after the addition of acetone is completed, keep the reaction for half an hour, take a sample test, and at the end of the reaction, if the raw material p-aminophenethyl ether is <0.5%, it is considered qualified, and the temperature is lowered to 60-80°C after passing the test.

[0037] Pump the materials in the above steps into the distillation kettle, and distill under normal pressure at a temperature of 60-140° C. to recover the diluent for mechanical use.

[0038] After the diluent was recovered, fractional distillation under reduced pressure was carried out. Under a vacuum of 0.098Mpa, the fraction at 142-160°C was collected to obtain 1389kg of the product ethoxyquinoline, with a content of 97%, and 0.43% of the raw material residue.

[0039] The...

Embodiment 3

[0041] In a 3000L reactor, add p-aminophenethyl ether (1000kg), diluent (400kg), and catalyst (100kg) in sequence, raise the temperature to 145°C under stirring, start adding acetone slowly, and keep the dropping temperature at 145°C ±5°C, after the addition of acetone is completed, keep the reaction for half an hour, take a sample test, and at the end of the reaction, if the raw material p-aminophenethyl ether is <0.5%, it is considered qualified, and the temperature is lowered to 60-80°C after passing the test.

[0042] Pump the materials in the above steps into the distillation kettle, and distill under normal pressure at a temperature of 60-140° C. to recover the diluent for mechanical use.

[0043] After the diluent was recovered, fractional distillation under reduced pressure was carried out, and the fraction at 142-160°C was collected under a vacuum of 0.098Mpa to obtain 1420kg of the product ethoxyquinoline with a content of 98.9% and 0.01% of the raw material residue. ...

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PUM

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Abstract

The invention relates to an industrial production method for ethoxy quinolone. The industrial production method comprises the following steps: adding p-phenetidine, a diluent and a home-made chelate catalyst serving as raw materials into a reaction kettle; heating to 125-165 DEG C; dropwise adding acetone to perform a synthetic reaction; preserving heat for half an hour after finishing dropwise adding of the acetone; recovering the diluent by distilling; fractionating under a reduced pressure to obtain the ethoxy quinolone. The ethoxy quinolone is over 98 percent in purity, is less than 0.5 percent in raw material residues, and is over 90 percent in total yield.

Description

technical field [0001] The invention relates to the field of organic synthesis and production application, in particular to an industrial production method of ethoxyquinoline. Background technique [0002] Ethoxyquinoline is an excellent feed and one of the antioxidants. It is the most economical antioxidant. It is used in premixes, toners and fat-added products to prevent the oxidation and deterioration of fats such as vitamins A, D, and E. , the natural pigment oxidizes and changes color, and has a certain anti-mildew and insurance effect. It can be used as an antioxidant for food, an insurance for fruits, and an anti-aging agent for bananas. [0003] Ethoxyquinoline is a light yellow viscous liquid, soluble in organic solvents such as benzene, methanol, ethanol, acetone, etc. [0004] The synthesis of ethoxyquinoline is mainly obtained by catalytic synthesis of p-aminophenethyl ether and acetone at present. At present, ethoxyquinoline manufacturers at home and abroad are...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D215/20
CPCC07D215/20
Inventor 薛锋张加明彭盘英
Owner 张加明
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