Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

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
View PDF3 Cites 3 Cited by
  • 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. Comparison of the three wastes produced in the post-treatment process Many; ③Although the catalyst is extensive, the acid will corrode the equipment, the selectivity of the alkaline activity is low, the amount of the organic tin catalyst should be considered, and the organic titanium catalyst is easy to deactivate

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for synthesis of (meth)acrylate diluent
  • Method for synthesis of (meth)acrylate diluent
  • Method for synthesis of (meth)acrylate diluent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0041] A mixture of the following components was added to a 29 cm diameter copper wire mesh packed column with a temperature display / controller, magnetic stirrer, dry air inlet, distillation head, distillate ratio-removal vapor pressure thermostat and In the 100ml four-neck flask of the distillate receiver gradually: 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. During the reaction process, a certain amount of air was introduced, and the reflux was continuously heated under normal pressure, and the reaction azeotropic mixture MA-methanol was removed at the same time. After the reaction reaches the end point, cool the reaction solution to 50°C, add 0.10g of neutral activated carbon, and continue to keep warm and stir for 0.5-1 hour. Diacrylat...

Embodiment 2

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

[0043] A mixture of the following components was added to a 29 cm diameter copper wire mesh packed column with a temperature display / controller, magnetic stirrer, dry air inlet, distillation head, distillate ratio-removal vapor pressure thermostat and In the 100ml four-neck flask of the distillate receiver gradually: 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. During the reaction process, a certain amount of air was introduced, and the reflux was continuously heated under normal pressure, and the reaction azeotropic mixture MA-methanol was removed at the same time. After the reaction reaches the end point, cool the reaction liquid to 50°C, add 0.10g of neutral activated carbon, and continue to heat and stir for 0.5-1 hour. After the end, the reaction liquid is fil...

Embodiment 3

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

[0045] A mixture of the following components was added to a 29 cm diameter copper wire mesh packed column with temperature display / controller, magnetic stirrer, dry air inlet, distillation head, distillate ratio-removal vapor pressure temperature control In the 250ml four-neck flask of the receiver and the step-by-step 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, feed into air and heat up to the reflux of the reaction solution, stabilize the reaction to the end of the reaction. Post-processing: Cool the reaction liquid to 50°C, add 0.10g of neutral activated carbon, and continue to heat and stir for 1 hour. After the end, the reaction liquid is vacuum filtered, and the filtrate is rotary evaporated under reduced pressure. The highest were 77.1% and 90.1% respectively.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com