Process for producing tertiary carbonic acid glycidyl ester

Abstract

A preparation method of neodecanoic acid glycidyl ester has the main raw materials of neodecanoic acid C10, epichlorohydrin, sodium hydroxide and catalyst; the epichlorohydrin and the catalyst are heated to 90 DEG C in a flask with four standard necks of 1 liter with the mechanical stirring, the neodecanoic acid is dripped, the dripping speed is controlled to maintain the temperature at 90 DEG C,the dripping is completed after about half an hour, the esterification reaction is completed after the continual reaction for half an hour; the acid value is less than 0.1 by measurement; the prepared solution containing NaOH is dripped in a reaction bottle for producing a white solid, at this time, a water pump is opened to slowly increase vacuum degree, the residual epichlorohydrin and water inthe reaction bottle are commonly boiled and evaporated, the process needs about one hour; the products are depressurized and vacuum filtrated to remove the NaCl solid substances, the filtrate is subject to vacuum distillation; and the neodecanoic acid glycidyl ester which takes the epoxy as the benchmark and has a content of 96 percent is obtained under the conditions of 90 to 92 DEG C / 140Pa. Thereaction cycle is short, the reaction yield is high, and the yield is above 86 percent. The recovery rate of epichlorohydrin is high. The reaction is smooth, the product quality is good, the operation is simple; and the preparation method is beneficial to the improvement of the product quality.

Description

technical field [0001] The invention belongs to the preparation method of organic compound glyceride, in particular to a preparation method of glycidyl tertiary carbonic acid ester. Background technique [0002] At present, the widely used glycidyl ester of tertiary carbonic acid in the world is actually C-10 glycidyl ester of tertiary carbonic acid, such as CARDURA E10 of Shell Company and GLYDEXX N-10 of EXXON Company. As for the glycidyl ester of C-9 tert-carbonic acid, there is no report. [0003] In numerous Japanese and European and American patents, although there are many synthetic methods of glycidyl tertiary carbonic acid esters, they are basically laboratory preparation methods, and these methods are basically not very suitable for industrial production. The main problem of these methods is: the feeding ratio of epichlorohydrin to tertiary carbonic acid is relatively large, generally 4-7 / 1. The reaction cycle is too long, and the general total reaction time is 4...

AI Technical Summary

Problems solved by technology

The main problem of these methods is: the feeding ratio of epichlorohydrin to tertiary carbonic acid is too large, generally 4-7 / 1

It is very difficult for these documents to repeat the high yields reported, and the results of our repeated experiments are generally 40%-60%

These reported methods lack reaction monitoring methods, resulting in incomplete reactions, which have an impact on product quality and yield

If these methods are fully adopted and implemented in industrialized production, the reaction scale will be too large, the reaction cycle will be too long, the production efficiency will be low, the production cost will be high, and the product quality will be unstable.

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