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A method for synthesizing trimethylolpropane trimethacrylate and trimethylolpropane triacrylate by transesterification

A technology of trimethylolpropane trimethacrylate and trimethylolpropane triacrylate, which is applied in the reaction preparation of ester group and hydroxyl group, organic chemistry and other directions, can solve the problems of easy polymerization of raw materials and products, complicated processing technology, Solvent recovery is difficult and other problems, to achieve the effect of convenient product quality control, simple treatment process and less side reactions

Active Publication Date: 2021-12-14
江苏华星新材料科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are problems such as complicated follow-up treatment process, difficult solvent recovery, easy polymerization of raw materials and products, and equipment corrosion.

Method used

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  • A method for synthesizing trimethylolpropane trimethacrylate and trimethylolpropane triacrylate by transesterification

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The synthesis process of trimethylolpropane trimethacrylate (TMPTMA):

[0034] Add respectively 100g of trimethylolpropane, 350g of methyl methacrylate, 2g of polymerization inhibitor TEMPO and 6g of hydroquinone, calcium oxide, potassium carbonate and chloride Lithium mixture 5g, heating and stirring, continue to feed air into the reactor, gradually warming up to the generation of reflux, the control reflux ratio is 2. As the reaction proceeds, the generated methanol and methyl methacrylate are discharged from the top of the fractionating column in the form of azeotrope. After a period of reaction, samples are taken from the flask for liquid chromatography analysis. The detection conditions of liquid chromatography are: chromatographic column C18 , 4.6×250mm, 5μm; mobile phase methanol-water volume ratio 30:70; flow rate 1.0mL / min; column temperature: 30°C; detection wavelength 254nm, injection volume: 10μL. When the product content ≥ 95%, the reaction is complete. C...

Embodiment 2

[0036] The synthesis process of trimethylolpropane trimethacrylate (TMPTMA):

[0037] Add trimethylolpropane 100g, methyl methacrylate 350g, polymerization inhibitor TEMPO 2g and p-hydroxyanisole 6g respectively in the reaction flask that thorn-shaped fractionating column and reflux device are housed, the catalyst that reclaims among the embodiment 1 , heating and stirring, continuously feed air into the reactor, gradually raise the temperature until reflux occurs, and control the reflux ratio to 2. As the reaction proceeds, the generated methanol and methyl methacrylate are extracted from the top of the fractionating column in the form of azeotrope. After a period of reaction, samples are taken from the flask for liquid chromatography analysis. The detection conditions of liquid chromatography are: chromatographic column C18, 4.6×250mm, 5μm; mobile phase methanol-water volume ratio: 30:70; flow rate: 1.0mL / min; column temperature: 30°C; detection wavelength: 254nm, injection ...

Embodiment 3

[0039] The synthesis process of trimethylolpropane triacrylate (TMPTA):

[0040]Add trimethylolpropane 100g, acrylate 300g, polymerization inhibitor 7052g and p-hydroxyanisole 6g, mixture 7g of salt of wormwood and lithium chloride in the reaction flask that thorn-shaped fractionating column and reflux device are housed respectively, heat Stir, continuously feed air into the reactor, gradually heat up until reflux occurs, and control the reflux ratio to 1.5. As the reaction proceeds, the generated methanol and methyl acrylate are extracted from the top of the fractionating column in the form of azeotropes. After a period of reaction, samples are taken from the flask for liquid chromatography analysis. The liquid chromatography detection conditions are: chromatographic column C18, 4.6×250mm, 5μm; mobile phase methanol-water volume ratio: 30:70; flow rate: 1.0mL / min; column temperature: 30°C; detection wavelength: 254nm, injection volume: 10μL. When the product content ≥ 95%, t...

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Abstract

The invention discloses a method for synthesizing trimethylolpropane trimethacrylate and trimethylolpropane triacrylate through transesterification, and belongs to the technical field of fine chemicals. Put MMA or MA and TMP into the reactor, add acidic or alkaline catalyst and polymerization inhibitor, and heat to generate reflux. As the reaction proceeds, the azeotrope formed by the raw material MMA or MA and the by-product methanol is continuously discharged, so that The chemical equilibrium continues to shift toward product formation until the reaction is complete. After the reaction is completed, the catalyst and polymerization inhibitor are removed by alkali washing or filtration, excess MMA or MA is recovered, and the product can be obtained after decolorization. The present invention adopts transesterification reaction and has few side reactions. The conversion rate of trimethylolpropane reaches more than 99%, and the recovery rate of methyl methacrylate reaches more than 98%, of which the triester content is more than 95%.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a method for synthesizing trimethylolpropane trimethacrylate and trimethylolpropane triacrylate through transesterification. Background technique [0002] Trimethylolpropane trimethacrylate (TMPTMA for short) and trimethylolpropane triacrylate (TMPTA for short) are very important acrylic acid multifunctional group ester monomers, which can be used as comonomers to synthesize special Acrylic resin can also be used as a crosslinking agent for rubber and plastics. Due to its high double bond content and fast curing speed, the cured film formed by it is wear-resistant and solvent-resistant. It is the most widely used multifunctional acrylate reactive diluent in the field of radiation curing. It is mainly used in paints, flexographic prints, solder resists, Photoresists, photocurable coatings and photocurable inks, etc. [0003] At present, the methods for synthes...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/03C07C69/54
CPCC07C67/03C07C69/54
Inventor 潘从多石泽宾李炉航刘淑龙
Owner 江苏华星新材料科技股份有限公司
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