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Anti-aging agent AW preparation method

A technology of anti-aging agent and catalyst, applied in the direction of organic chemistry, etc., can solve the problems of low conversion rate of aminophenethyl ether, long production cycle, high equipment requirements, etc., and achieve the effect of low catalyst consumption, low production cost and good product quality

Active Publication Date: 2019-04-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the traditional synthetic method of anti-aging agent AW, whether acid is used as a catalyst, or the composite catalyst of acid, ferric chloride and halide, there are problems of large amount of three wastes and serious corrosion, and the use of supported acid catalysts is expensive. Expensive, highly toxic or non-recyclable problems restrict the safety and sustainability of the production of antioxidant AW
At the same time, the conversion rate of raw material p-aminophenethyl ether is low, the product quality is poor, the pollution of three wastes is serious, or the requirements for equipment are high and the production cycle is long.
Using solid strong acid as catalyst, the method is easy to operate and the amount of waste water is small, but solid acid catalyst is difficult to be used in the industrial production of this process, and there is no report of industrial application in the antioxidant AW industry at present

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Put 250g of p-aminophenethyl ether and 5g of diisopropyl titanate into four outlets of 1000m1 with agitator, thermometer and discharge pipeline (connected to a fractionation tower so that acetone and the water produced by the reaction enter the fractionation tower) in the flask. Under normal pressure, 1500g of acetone was continuously fed by a metering pump, the feeding reaction time was 6 hours, and the reaction temperature was controlled at 160°C to prepare the anti-aging agent AW reaction liquid. The water produced during the reaction and excess acetone pass through the fractionation tower, the acetone can be recovered at the same time, and the water produced by the reaction can be separated. The single-pass conversion rate of p-aminophenethyl ether in the reaction can reach 97.3%. Finally, add 3g of liquid caustic soda to neutralize the anti-aging agent AW reaction liquid, and statically stratify. The waste water in the lower layer is carried out to the waste water ...

Embodiment 2

[0021] Put 250g of p-aminophenethyl ether and 2g of tetra-n-butyl titanate catalyst into 1000m1 quadruple with stirrer, thermometer and discharge pipeline (connected to a fractionation tower so that acetone and the water produced by the reaction enter into the fractionation tower) In the flask, 1600g of acetone was fed by a metering pump continuous feed, and the feed reaction time was 4 hours. Under normal pressure, the reaction temperature is controlled at 140°C, and the reaction water and excess acetone pass through the fractionation tower to recover acetone and separate the reaction water at the same time. The waste water is used in the waste water treatment system. After the upper material liquid is subjected to vacuum distillation at -0.098MPa to recover the unreacted p-aminophenethyl ether (the recovered p-aminophenethyl ether continues to be used in the reaction), the AW is further distilled and the gas phase temperature is 145 The distillate at -155 ℃ produced 357g of ...

Embodiment 3-16

[0023] Adopt the experimental method of embodiment 1. Under the condition that other conditions are constant, by changing the ratio of p-aminophenethyl ether to acetone during the reaction, the ratio of p-aminophenethyl ether to the catalyst, different reaction temperatures and reaction times, and the reaction form to investigate the single-pass conversion rate and product of the reaction The effective body content, the results are shown in Table 1.

[0024] Table 1 Antiaging agent AW synthesis test data table

[0025] implement

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Abstract

The invention belongs to the technical field of fine chemical industry, and relates to an anti-aging agent AW preparation method, wherein the anti-aging agent AW is prepared under the action of a catalyst by using p-phenetidine and acetone as raw materials, the catalyst is a titanate-based catalyst, the reaction temperature is 100-200 DEG C, the reaction time is 3-10 h, a molar ratio of p-phenetidine to acetone is 1:1-6, a molar ratio of titanate to p-phenetidine is 0.0005-0.05:1, the single-pass conversion rate can achieve more than 97% based on p-phenetidine, and the AW content of the product can reach 99.5%. According to the present invention, the anti-aging agent AW is prepared by using the titanate-based catalyst, such that the advantages of simple operation, low catalyst consumption,low cost, high content of effective body and the like can be achieved.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, relates to a preparation method of anti-aging agent AW, and is a green and environment-friendly preparation process. Background technique [0002] Antiaging agent AW, also known as ethoxyquinoline, chemically named 6-ethoxy-2,2,4-trimethyl-1,2-dihydroquinoline, is one of the excellent and economical feed antioxidants , suitable for premix, fishmeal and fat-added products, can prevent vitamin A, D, E, etc. and fat oxygen from deteriorating, natural pigments from oxidative discoloration, and has certain anti-mildew and fresh-keeping effects, and can also be used as Food antioxidant, fruit preservative, rubber anti-aging agent. [0003] The synthesis of anti-aging agent AW generally adopts the reaction of p-aminophenethyl ether and acetone, and the product is obtained under the action of different catalysts. Romanian patent RO65302 provides a method for producing ethoxyquinoline by reacting...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D215/20
CPCC07D215/20
Inventor 韦志强付春史乐萌黄伟高留冕
Owner CHINA PETROLEUM & CHEM CORP
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