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Preparation method of anti-aging agent AW

A technology of anti-aging agents and catalysts, which is applied in chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., and can solve high process costs, large solvent consumption, and long production cycles, etc. problems, and achieve the effects of simple preparation process, shortened reaction time and low production cost

Pending Publication Date: 2022-04-12
SINOPEC NANJING RES INST OF CHEM IND CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Chinese patent CN101823998 solves the problem of continuous separation of reaction mixture and recycling of reaction raw materials through the coupling of reaction system and simulated moving bed chromatographic separation system. The purity of ethoxyquinoline is increased to more than 98%, but the production cycle of this process is long More than 36 hours, there are also problems such as long production cycle, large amount of solvent consumption, and high process cost
[0010] In the traditional synthetic method of anti-aging agent AW, there are problems such as the use of hydrochloric acid, sulfuric acid, ferric chloride, benzenesulfonic acid, p-toluenesulfonic acid, halide catalysts, etc. There are problems of high price, high toxicity or non-recyclability, which restrict the safety and sustainability of AW production
At the same time, the conversion rate of raw material p-aminophenethyl ether is low, the product quality is poor, and the production cycle is long.
Using solid strong acid as catalyst, this 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 AW industry at present

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Composite catalyst preparation: Add 10g of hydrochloric acid with a mass water content of 31% into a four-necked bottle, then add 10g of anti-aging agent AW, stir and heat up to 120°C, test after 2h, the water content is 0.74%, add 8.6g of p-toluenesulfonic acid , Stir evenly, keep at 140°C, check after 2 hours, the water content is 0.31%, cool down, and seal it for storage.

[0031] Put 200g of p-aminophenethyl ether and 3.0g of the above-mentioned composite catalyst into a 1000ml four-necked flask with a stirrer, a thermometer and a discharge pipeline. Under normal pressure, 1200g of acetone was continuously fed by a metering pump, the reaction time of the feeding was 1.2 hours, and the reaction temperature was controlled at 150°C to prepare the anti-aging agent AW reaction liquid. It was detected that the conversion rate of p-aminophenetole in the reaction was 99.3%. The water produced during the reaction and excess acetone pass through the fractionation tower, acet...

Embodiment 2

[0033] Composite catalyst is prepared with embodiment 1.

[0034] Put 250g of p-aminophenethyl ether and 2g of composite catalyst into a 1000m1 four-necked flask equipped with a stirrer, a thermometer and a discharge pipeline at one time, and feed 1600g of acetone by means of continuous feeding with a metering pump, and the feeding reaction time is 0.9 hours . Under normal pressure, the reaction temperature is controlled at 160 °C, and the reaction water and excess acetone are separated from the system through the fractionating tower in the discharge pipeline. The kettle liquid is AW reaction liquid, and the conversion rate of p-aminophenetole in the reaction is 99.8%. Add 3g of liquid caustic soda to neutralize, static stratification, the waste water of the lower layer is carried out to the waste water treatment system, and the upper layer of feed liquid is subjected to -0.098MPa vacuum, and the unreacted p-aminophenethyl ether is recovered by vacuum distillation (the recover...

Embodiment 3-16

[0036] 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.

[0037] Table 1:

[0038] Example catalyst p-aminophenethyl ether / acetone molar ratio Catalyst / p-aminophenetole mass ratio Reaction temperature (°C) Reaction time (h) AW content (%) One-way yield (%) 3 The molar ratio of hydrochloric acid to benzenesulfonic acid is 1:1 1 / 1.2 0.002 / 1 145 0.8 99.5 97.0 4 The molar ratio of hydrochloric acid to benzenesulfonic acid is 1:1 1 / 1.5 0.02 / 1 150 1.2 99.7 97.4 5 The molar ratio of hydrochloric acid to benzenesulfonic acid is 1:1 1 / 2 0.01...

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Abstract

The invention belongs to the technical field of fine chemical engineering, and relates to an anti-aging agent AW and a preparation method thereof. The anti-aging agent AW is prepared by taking p-aminophenetole and acetone as raw materials under the action of a composite catalyst consisting of hydrochloric acid and a sulfonic acid catalyst. According to the technical scheme provided by the invention, p-aminophenetole and acetone are used as raw materials to prepare the anti-aging agent AW under the action of the composite catalyst, and an intermittent or continuous production process can be adopted. The conversion per pass of p-aminophenetole can reach 99% or above, the AW content of the product can reach 99.5-99.8%, and compared with the prior art, the method has the advantages that the operation is simple, the catalyst consumption is low, the cost is lower, and the content is higher.

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 fresh-keeping agent, rubber anti-aging agent (especially styrene-butadiene rubber, which has good oxidation resistance and ozone resistance, and good weather resistance and flex crack resistance). [0003] The synthesis of AW generally adopts the reaction of p-aminophenethyl ether and acetone, and the prod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D215/20B01J31/02B01J27/10
Inventor 韦志强付春祝东红黄伟高留冕郁铭吕明倩
Owner SINOPEC NANJING RES INST OF CHEM IND CO LTD
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