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Preparation method of ethylene glycol dimethacrylate

A technology of ethylene glycol dimethacrylate and hydroxyethyl methacrylate, which is applied in the preparation of carboxylate, the preparation of organic compounds, chemical instruments and methods, etc., can solve pollution, poor industrial feasibility and complicated post-processing And other issues

Pending Publication Date: 2021-11-30
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The acid chloride alcoholysis method generally uses acryloyl chloride and ethylene glycol as raw materials, which can react at room temperature without adding a catalyst, but the nature of the acid chloride is very active. During the reaction process of the acid chloride alcoholysis method to synthesize ethylene glycol dimethacrylate It will produce hydrogen chloride, which is easy to cause pollution, and the post-treatment is complicated. It is often suitable for laboratory synthesis, and the feasibility of industrialization is poor.
[0004] Most of the published papers and patents on the preparation of ethylene glycol dimethacrylate mostly use ethylene glycol and methacrylic acid to directly esterify or transesterify methyl methacrylate and ethylene glycol under an acidic catalyst. Preparation, about the use of hydroxyethyl methacrylate as a raw material and methacrylic acid to prepare ethylene glycol dimethacrylate has not yet seen the relevant reports

Method used

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  • Preparation method of ethylene glycol dimethacrylate
  • Preparation method of ethylene glycol dimethacrylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] S1. Reactive distillation tower parameters: tower height: 2m; tower diameter: 20mm; number of trays: 10.

[0031] Weigh 1kg hydroxyethyl methacrylate, 2kg methacrylic acid, 0.06kg concentrated sulfuric acid, 1g hydroquinone, 2g p-hydroxyanisole, dissolve the concentrated sulfuric acid and p-hydroxyanisole in hydroxyethyl methacrylate In the process, the hydroxyethyl methacrylate dissolved with hydroquinone, p-hydroxyanisole and concentrated sulfuric acid is loaded into the storage tank connected to the upper feed port of the reactive distillation device, and the methacrylic acid is loaded into the reactive distillation device The storage tank connected to the lower feed port;

[0032] Put the hydroxyethyl methacrylate dissolved with concentrated sulfuric acid, hydroquinone, and p-hydroxyanisole into the storage tank of the upper and lower feed ports of the reaction rectification device and methacrylic acid into the upper and lower feed of the reaction rectification devi...

Embodiment 2

[0036] S1. Reactive distillation tower parameters: tower height: 2m; tower diameter: 20mm; number of trays: 10.

[0037] Weigh 1kg hydroxyethyl methacrylate, 3kg methacrylic acid, 0.16kg phosphotungstic acid, 3g hydroquinone, 6g p-hydroxyanisole, 3g hydroxytetramethylpiperidine nitroxide free radical and mix catalyst and inhibitor The polymerizing agent is dissolved in hydroxyethyl methacrylate, and the hydroxyethyl methacrylate dissolved in hydroquinone, p-hydroxyanisole, hydroxytetramethylpiperidine nitroxide radical and phosphotungstic acid is charged into the reaction The rectification device is connected to the storage tank of the upper feed port, and the methacrylic acid is loaded into the storage tank connected to the lower feed port of the reactive rectification device. The feed rate of methacrylic acid is 10g / min, the feed rate of methacrylic acid is 30g / min, the temperature of the rectifying column to be reacted is stable at 70°C-80°C, the system pressure is stable a...

Embodiment 3

[0041] S1. Reactive distillation tower parameters: tower height: 5m; tower diameter: 30mm; number of trays: 20.

[0042] Take by weighing 2kg hydroxyethyl methacrylate, 5kg methacrylic acid, 0.42kg p-toluenesulfonic acid, 10g hydroquinone, 50g p-hydroxyanisole, 10g hydroxytetramethylpiperidine nitroxide free radical and catalyst and The polymerization inhibitor is dissolved in hydroxyethyl methacrylate, and the hydroxyethyl methacrylate dissolved with hydroquinone, p-hydroxyanisole, hydroxytetramethylpiperidine nitroxide radical and p-toluenesulfonic acid into the storage tank connected to the upper feed port of the reactive distillation device, and the methacrylic acid is loaded into the storage tank connected to the lower feed port of the reactive rectification device, and the reaction rectification tower is evacuated, and the temperature is raised to control the methacrylic acid hydroxyl The feed rate of ethyl ester is 15g / min, the feed rate of methacrylic acid is 40g / min f...

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Abstract

The invention discloses a preparation method of ethylene glycol dimethacrylate, and aims to provide a preparation method of ethylene glycol dimethacrylate which is high in reaction rate, high in product yield and high in product purity, and a catalyst and a polymerization inhibitor can be repeatedly used. According to the scheme, hydroxyethyl methylacrylate and methacrylic acid are adopted as raw materials, a catalyst and a polymerization inhibitor are directly added into the raw material hydroxyethyl methylacrylate, excessive methacrylic acid is adopted, reactive distillation is carried out in a negative pressure state to realize continuous esterification reaction, and after crude ethylene glycol dimethacrylate is obtained, continuous rectifying is performed so as to obtain a high-purity ethylene glycol dimethacrylate product. The invention belongs to the technical field of fine chemical engineering.

Description

technical field [0001] The invention relates to a preparation method of fine chemicals, in particular to a preparation method of ethylene glycol dimethacrylate, which belongs to the technical field of fine chemicals. Background technique [0002] Ethylene glycol dimethacrylate (EGDMA) is an important crosslinking agent. It is often used as a cross-linking agent in plastics, rubber industry, ethylene-propylene copolymer, ABS, acrylic sheet, pipe, glass fiber reinforced polyester, PVC, ion exchange resin, glazing, etc. Ethylene glycol diethylene glycol is added when the polymer is copolymerized As a cross-linking agent, methacrylate will increase the hardness of the polymer, improve friction, heat resistance, weather resistance and solvent resistance. In addition, it is often used in marble, dental materials, adhesives, inks, coatings and optical materials. [0003] At present, the methods for preparing ethylene glycol dimethacrylate at home and abroad mainly include direct ...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C67/54C07C67/62C07C69/54
CPCC07C67/08C07C67/54C07C67/62C07C69/54Y02P20/10
Inventor 邓联平方岩雄张维刚谭伟蔡晓兰张泽银
Owner GUANGDONG UNIV OF TECH