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Rapid microwave preparation method of glycidyl (meth)acrylate

A technology of glycidyl ester and acrylic acid, applied in the field of microwave rapid preparation of glycidyl (meth)acrylate, can solve the problems of reducing the yield of the target product, difficult to realize industrialization, difficult to remove moisture, etc., and achieves high industrial application value and time. Short, low temperature effect

Inactive Publication Date: 2013-01-09
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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Problems solved by technology

[0005] In addition, there is also a report on the production of GMA by one-step method. In the reaction process, the sodium salt will swell, and a large amount of solvent needs to be used. Because it is difficult to remove the moisture generated in the reaction process, it will cause side reactions and reduce the yield of the target product. Therefore, it is difficult to achieve industrialization

Method used

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  • Rapid microwave preparation method of glycidyl (meth)acrylate
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  • Rapid microwave preparation method of glycidyl (meth)acrylate

Examples

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Embodiment example 1

[0029]Implementation Case 1 Synthesis of (meth)acrylic acid sodium salt

[0030] In this example, the mass ratio of (meth)acrylic acid to 30% metal sodium alkali solution is 1:1 to 1:5, the metal sodium alkali solution is preferably sodium hydroxide aqueous solution, and the metal sodium solution is at a speed of 1 to 10d / s, preferably 3 ~6d / s, add to (meth)acrylic acid, add 0.01%~1% polymerization inhibitor when stirring, preferably 0.01%~0.05%, prevent the polymerization of (meth)acrylic acid sodium salt, reaction temperature 0℃~80℃ , preferably 40°C-60°C, reaction time 0.5-3h, such as 1h, 2h, reaction vacuum 100-650mmHg, such as 200mmHg, 300mmHg, 400mmHg, 500mmHg, 600mmHg. After the reaction, use 5% to 30% inorganic acid, such as 10% hydrochloric acid, to adjust the pH value of the reaction solution to 8 to 10, and dry the reaction solution in vacuum at 0 to 90°C with a vacuum degree of 300 to 760mmHg to obtain a solid (meth)acrylic acid sodium salt , ground into powder, s...

Embodiment example 2

[0031] Implementation Case 2 Microwave Synthesis of Glycidyl Methacrylate

[0032] Take 50g of homemade sodium methacrylic acid, 171g of epichlorohydrin (the ratio of the two substances is 1:4), 0.6% p-hydroxyanisole and 0.6% tetrabutylammonium bromide in a 500mL microwave reaction bottle In the process, adjust the power of the microwave reactor to 500w, the temperature to 105°C, start the microwave to start timing, start sampling at the 8th minute, and stop sampling every two minutes until 20 minutes. The reaction liquid gas phase analysis shows that when the reaction time is 14 minutes, the conversion rate of the reaction reaches 95.4 %, after adding an appropriate amount of hydroquinone, the resulting product was distilled under reduced pressure to obtain a mass of glycidyl methacrylate of 58.9 g and a yield of 89.6%.

Embodiment example 3

[0033] Example 3 Microwave Synthesis of Glycidyl Acrylate

[0034] Take 50g of homemade sodium acrylic acid, 171g of epichlorohydrin (the ratio of the two substances is 1:4), 0.6% p-hydroxyanisole and 0.6% tetrabutylammonium bromide in a 500mL microwave reaction bottle, Adjust the power of the microwave reactor to 500w, the temperature to 105°C, and the reaction time to 20min. Start the microwave reactor to start timing, start sampling in the 8th minute, and take samples every two minutes until 20min, gas phase analysis When the reaction time is 14min, the conversion rate of the reaction reaches 96.6%, after adding an appropriate amount of hydroquinone, the resulting The product was distilled under reduced pressure to obtain glycidyl acrylate with a mass of 58.8 g and a yield of 86.4%.

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Abstract

The invention provides a rapid microwave preparation method of glycidyl (meth)acrylate. The method is characterized in that (meth)acrylic acid, sodium carbonate or sodium hydroxide, and epichlorohydrin are used as raw materials. The preparation method comprises the following steps: preparing sodium (meth)acrylate, performing microwave vacuum drying on the sodium salt; performing a phase transfer catalytic reaction on sodium salt and epichlorohydrin under microwave irradiation, adding a polymerization inhibitor and a phase transfer catalyst in the system and reacting for 14 minutes. Through using the preparation method, the product conversion rate is up to more than 95%; compared with the traditional method, the time is reduced by about ten times; by adopting the method, the reaction rate of the product can be increased and the production period can be shortened; and the method is extremely high in industrial application value.

Description

technical field [0001] This patent relates to a microwave rapid preparation method of glycidyl (meth)acrylate, which is widely used in the fields of organic synthesis, polymer synthesis and polymer modification, coatings, adhesives, leather, chemical fibers, papermaking, printing and dyeing, etc. Background technique [0002] Glycidyl (meth)acrylate is a reactive bifunctional monomer containing carbon-carbon double bonds and epoxy groups in the molecule. It is colorless, transparent, insoluble in water, low in toxicity, and less harmful to the human body. Glycidyl (meth)acrylate has both active vinyl groups and ionic reactive epoxy groups, which can form side chains with epoxy groups, side chains with ethylene groups, and ring-opening through epoxy groups. The long-chain polymer compounds formed, so the modified and grafted polymer materials based on glycidyl (meth)acrylate are widely used in daily life. At present, its application scope includes: improving the hardness, gl...

Claims

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Application Information

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IPC IPC(8): C07D303/16C07D301/30
Inventor 王成章何源峰
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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