Method for synthesis of (meth)acrylate diluent

A technology of acrylates and alkyl acrylates, which is applied in the field of transesterification synthesis, can solve the problems of easy deactivation of organic titanium catalysts, high consumption of raw materials and energy consumption, low selectivity of alkaline activity, etc., and achieve stable and easy production of products. Effects of separation, improved processing capacity, and simple equipment

Inactive Publication Date: 2016-08-10
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But there are following deficiencies: 1. The methanol generated by the reaction will form an azeotropic mixture with the raw material MA (MMA), and the distillation will take away the methanol and the raw material ester, resulting in higher consumption of raw materials and energy consumption; 2. Compariso

Method used

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  • Method for synthesis of (meth)acrylate diluent
  • Method for synthesis of (meth)acrylate diluent
  • Method for synthesis of (meth)acrylate diluent

Examples

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Example Embodiment

[0040] Example 1 Preparation of diethylene glycol di(meth)acrylate

[0041] Add the mixture of the following components to a 29cm diameter copper wire mesh packing column with a temperature indicator / temperature controller, a magnetic stirrer, a dry air inlet, a distillation head, a distillate ratio-a vapor pressure removal thermostat and In the 100ml four-necked flask of the gradually distilled liquid receiver: 5.31g (0.05mol) diethylene glycol (DEG), 25.83g (0.3mol) methyl acrylate (MA), 0.03g (0.0002mol) p-hydroxybenzene Methyl ether and, 0.11g (0.0002mol) dibutyltin dilaurate. The mixture was then warmed to reflux. In the course of the reaction, a certain amount of air is introduced, and heating is continued under normal pressure to reflux, while removing the reaction azeotropic mixture MA-methanol. After the reaction reaches the end, the reaction solution is cooled to 50°C, 0.10g neutral activated carbon is added, and the temperature is kept agitated for 0.5-1 hour. After ...

Example Embodiment

[0042] Example 2 Preparation of ethylene glycol di(meth)acrylate

[0043] Add the mixture of the following components to a 29cm diameter copper wire mesh packing column with a temperature indicator / temperature controller, a magnetic stirrer, a dry air inlet, a distillation head, a distillate ratio-a vapor pressure removal thermostat and In the 100ml four-necked flask of the gradually distilled liquid receiver: 3.1g (0.05mol) ethylene glycol, 25.83g (0.3mol) methyl acrylate (MA), 0.03g (0.0002mol) p-hydroxyanisole and 0.11g ( 0.0002mol) dibutyltin dilaurate. The mixture was then warmed to reflux. In the course of the reaction, a certain amount of air is introduced, and heating is continued under normal pressure to reflux, while removing the reaction azeotropic mixture MA-methanol. After the reaction reaches the end, the reaction solution is cooled to 50°C, 0.10g neutral activated carbon is added, and the temperature is kept and stirred for 0.5-1 hour. After completion, the react...

Example Embodiment

[0044] Example 3 Preparation of trimethylolpropane tri(meth)acrylate

[0045] Add the mixture of the following components to a copper wire mesh packing column with a diameter of 29 cm with a temperature indicator / temperature controller, a magnetic stirrer, a dry air inlet, and a distillation head, and the distillate ratio-removal of vapor pressure and temperature control In the 250ml four-necked flask of the receiver and the stepwise distillate receiver: 13.42g (0.5mol) trimethylolpropane (TMP), 77.5g (0.9mol) MA, 0.07g (0.0006mol) MEHQ, 0.50g (0.004mol) ) Anhydrous potassium carbonate, air is introduced and the temperature is raised to the reflux of the reaction solution, and the reaction is stabilized to the end of the reaction. After post-treatment, the reaction solution was cooled to 50℃, 0.10g neutral activated carbon was added, and the temperature was kept and stirred for 1 hour. After the completion, the reaction solution was filtered under reduced pressure, and the filtra...

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Abstract

The invention discloses a method for synthesizing (meth)acrylate diluent, which belongs to the field of organic synthesis. The (meth)acrylate and alcohol are used as raw materials, a reaction-rectification coupling process is adopted, and a copper wire mesh is used. The modified rectification column of packing, adding organic monotin catalyst, can obtain sufficient product purity and yield after simple post-treatment process. Compared with the traditional transesterification method, the method of the present invention can improve the total yield and processing capacity, utilize the reaction heat to supply the separation needs, reduce energy consumption, and reduce investment. The method of the invention is short in technical process, easy to obtain raw materials, simple in equipment and easy to control the reaction conditions. The method has mild reaction conditions, simple purification and purification process, stable and easy separation of products, and is not easy to cause polymerization.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and relates to a transesterification synthesis method for preparing monomeric (meth)acrylates from alcohols and (meth)acrylates. Background technique [0002] Reactive diluent is one of the key components of UV curable materials and is used in large amounts. Research and practical applications have shown that (meth)acrylate reactive diluents have the characteristics of low viscosity, high functionality and high curing activity. Coatings, adhesives, fiber treatment agents, paper finishing agents, leather, chemical fibers, printing and dyeing, functional polymers, etc. [0003] [0004] R=H,CH 3 , R'O = alkoxide of at least one alcohol [0005] Formula II (meth)acrylate reactive diluent chemical structure [0006] According to existing literature reports, the synthesis of (meth)acrylic ester reactive diluents can be prepared by one-step reaction of (meth)acrylic acid and alcohol as raw mater...

Claims

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Application Information

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IPC IPC(8): C07C69/54C07C67/03C07C67/54
CPCC07C67/03C07C67/54
Inventor 冯筱晴李文倩宋国强杨北
Owner CHANGZHOU UNIV
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