Synthetic method of medicinal acetyl trioctyl citrate

Abstract

The invention discloses a synthetic method of medicinal acetyl trioctyl citrate, in particular to a method for catalytic synthesis of acetyl trioctyl citrate by using of mesoporous zeolite supported heteropolyacid. The synthetic method comprises the following steps: (1), citric acid and n-caprylic alcohol are used as raw materials, mesoporous zeolite supported heteropolyacid is used as catalyst, after complete reaction, the obtained reaction mixture layers naturally, and n-caprylic alcohol and water in the mixture are distilled out under reduced pressure directly to obtain a crude product; (2), adding acetic anhydride into the crude product obtained in step (1), after complete reaction, the reaction mixture is left to stand for layering, the substance in the upper layer is subjected to distillation under reduced pressure to obtain a coarse product, and the coarse product is refined and purified to obtain the finished product of acetyl trioctyl citrate. The method provided by the invention is mild in reaction condition and short in reaction time; the same catalyst is used in the reaction of two steps and can be reused, so that the method is suitable for industrial production; besides, the product esterification rate is high, the product yield is high, the quality is good, and the microbial limit is controlled effectively.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and relates to a method for synthesizing medicinal acetyl trioctyl citrate, in particular to a method for catalytically synthesizing medicinal acetyl trioctyl citrate loaded with a heteropolyacid on a mesoporous molecular sieve. Background technique [0002] Citrate plasticizer is an environmentally friendly plasticizer produced from non-petroleum raw materials. It has already been industrialized in developed countries such as Europe, America and Japan. As the second largest producer of citric acid, China also started a small amount of industrial production at the end of the last century and entered the market at the beginning of this century. [0003] Acetyl trioctyl citrate is a citric acid ester plasticizer, non-toxic and safe. It is one of the first choice environment-friendly plasticizers in the plastic industry at home and abroad. It has good compatibility, high growth rate, non-toxic, Low...

AI Technical Summary

Problems solved by technology

Of course, the catalyst can also be adsorbed in the molecular sieve only by the intermolecular force, but this force is extremely weak compared with the covalent bond, and it is easy to cause the catalyst to be desorbed and lost.

However, when metal oxides are used as the carrier to load heteropolyacids, the alkalinity of the carrier itself has a greater effect on the structural damage of heteropolyacids, and the increase in specific surface area is limited; while ion exchange resins are easy to swell and inactivate in solution

Although activated carbon as a carrier has a high specific surface area, a wide range of pH stability, and good catalytic activity, it has a serious problem of elution of heteropolyacid active substances.

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