A kind of preparation method of pentaerythritol tetrakis (3-mercapto propionate) ester

Abstract

The invention provides a method for preparing pentaerythritol tetrakis(3-mercaptopropionate), comprising the following steps: a) mixing pentaerythritol, mercaptopropionic acid, methanesulfonic acid and a composite water-absorbing agent, and reacting until mercaptopropionic acid The remaining 1wt% of the reaction is regarded as the reaction end point, and the reaction mixture is obtained; the composite water-absorbing agent is composed of 4A molecular sieve, water-absorbing silica gel and water-absorbing resin; b) vacuum-filter the reaction mixture obtained in step a) to obtain the used Composite water-absorbing agent and reaction crude product; c) sequentially washing, liquid-liquid separation, dehydration and filtering the reaction crude product obtained in step b) to obtain pentaerythritol tetrakis (3-mercaptopropionate) ester. Compared with the prior art, the present invention uses a composite water-absorbing agent of specific components to synthesize pentaerythritol tetrakis (3-mercaptopropionate) ester under specific steps and conditions of each step, without affecting the quality of the product. Improve water removal efficiency, thereby speeding up the reaction rate.

Description

technical field [0001] The invention relates to the technical field of pentaerythritol tetrakis (3-mercaptopropionate), more specifically, to a preparation method of pentaerythritol tetrakis (3-mercaptopropionate). Background technique [0002] Pentaerythritol tetrakis (3-mercaptopropionate) is mainly used as an intermediate in organic synthesis, as a modifier in polymerization reactions such as UV coatings, inks, and adhesives, as a crosslinking agent, as an acidic ion exchange catalyst, and as a low-temperature curing agent. Wait. [0003] The production of pentaerythritol tetrakis (3-mercaptopropionic acid) ester is usually synthesized by esterification of raw materials pentaerythritol and mercaptopropionic acid in the presence of catalysts. The catalysts mainly include sulfuric acid and sulfonic acids; the water generated by the reaction needs to be removed from the reaction system to make the esterification The reaction proceeds in the direction of esterification, and ...

AI Technical Summary

Problems solved by technology

This process has the problem that the water removal efficiency is low and the reaction speed is slow, mainly due to the following two reasons: (1) pentaerythritol is a tetrahydric alcohol, and the molecular weight of mercaptopropionic acid is relatively large, so the steric hindrance of the special product generated is relatively large, which makes the reaction The speed is slow; (2) Usually, water has a certain solubility in general water-carrying agents, and at the same time, the water-carrying agent and water have entrainment phenomenon, which makes it difficult for water to be separated from the water-carrying agent quickly, and the system contains more water , especially in the later stage of the reaction, even if there is a small amount of water in the system, it will make the reaction difficult to proceed, and the reaction time will be longer, which will not only increase energy consumption, but also cause side reactions and affect product quality