CN-122010727-A - Preparation method of 2-butoxyethyl methacrylate

Abstract

The invention provides a preparation method of 2-butoxyethyl methacrylate, belonging to the technical field of methacrylate. The catalyst for the transesterification reaction takes tetrabutyl titanate as the catalyst for the transesterification reaction, can effectively reduce the activation energy of the transesterification reaction, enables the transesterification reaction to be carried out at a lower temperature in a shorter time, reduces the reaction temperature due to the mild reaction condition and the high selectivity of the tetrabutyl titanate to the transesterification reaction, reduces the self-polymerization of MMA and the dehydration of ethylene glycol monobutyl ether, improves the purity of the product, has more uniform active sites and smaller volume effect of the tetrabutyl titanate, can not influence the contact of a substrate and the catalyst to increase byproducts due to the uneven acidity and steric hindrance of the surface of the catalyst even if a solvent is not used, can convert the tetrabutyl titanate into titanium dioxide precipitate through simple acid washing in the post-treatment, and can be effectively removed through filtration.

Inventors

• HU SHUANGSHUANG
• Guo you
• HE YU
• JI HUI
• ZHANG YAWEN
• HE YIFAN
• LIU KUNHONG

Assignees

• 陕西大美化工科技有限公司

Dates

Publication Date

20260512

Application Date

20260327

Claims (10)

1. 1. A preparation method of 2-butoxyethyl methacrylate comprises the following steps: Mixing methyl methacrylate, ethylene glycol monobutyl ether, a polymerization inhibitor and tetrabutyl titanate for transesterification reaction to obtain a crude product, wherein the temperature of the transesterification reaction is 90-100 ℃; Adding an organic solvent, acid liquor and alkali metal salt solution into the crude product, and then filtering to obtain filtrate; And (3) oil-water separation is carried out on the filtrate, and the obtained oil phase is subjected to reduced pressure distillation to obtain the 2-butoxyethyl methacrylate.
2. 2. The method according to claim 1, wherein the transesterification reaction time is 4 to 6 hours.
3. 3. The preparation method of claim 1, wherein the molar ratio of tetrabutyl titanate to ethylene glycol monobutyl ether is (1-4) 20.
4. 4. The preparation method of claim 1, wherein the mass ratio of the methyl methacrylate to the ethylene glycol monobutyl ether is 3.4 (1-1.5).
5. 5. The method according to claim 1, wherein the polymerization inhibitor is a phenolic polymerization inhibitor.
6. 6. The preparation method according to claim 1 or 5, wherein the mass ratio of the polymerization inhibitor to methyl methacrylate is 0.02 (50-150).
7. 7. The process according to claim 1, wherein after the transesterification reaction, the reaction system is distilled under reduced pressure to obtain a crude product.
8. 8. The method according to claim 1, wherein the acid solution is hydrochloric acid or sulfuric acid.
9. 9. The method according to claim 1, wherein the filter material used for the filtration is diatomaceous earth.
10. 10. The method according to claim 1, wherein the reduced pressure distillation is performed at a temperature of 90 to 120 ℃.

Description

Preparation method of 2-butoxyethyl methacrylate Technical Field The invention belongs to the technical field of methacrylate, and particularly relates to a preparation method of 2-butoxyethyl methacrylate. Background 2-Butoxyethyl methacrylate, having the structural formula: 。 The 2-butoxyethyl methacrylate is used as a functional (methyl) acrylate monomer, and the butoxyethyl ester group in the molecular structure of the functional (methyl) acrylate monomer has excellent solubility, flexibility and reactivity, has important value in the aspects of preparing weather-resistant coatings, flexible electronic device packaging materials and the like, and is widely applied to the fields of photo-curing coatings, printing inks, adhesives and bio-based high polymer materials. The preparation method of the 2-butoxyethyl methacrylate mainly comprises a direct esterification method and a transesterification method. The direct esterification method has the advantages of easily available raw materials, mature process, more side reactions, complex post-treatment and difficulty in obtaining a high-purity product. The transesterification method has less side reaction and can obtain a product with higher purity. In order to ensure smooth progress of the transesterification reaction, a higher temperature is required to activate the substrate, however, the substrate of the transesterification reaction contains c=c unsaturated bonds, and the higher the temperature, the more easily self-polymerization occurs, reducing the conversion rate. In the prior art, the reaction is carried out in a solvent system by adding a solvent, the reaction temperature is reduced, the transesterification reaction is ensured, and the self-polymerization of a reaction substrate is reduced, however, the reaction substrate is diluted by the use of the solvent, so that the reaction rate is reduced, the purity of a final product can only reach 90%, and the purity is required to be further improved. Disclosure of Invention The invention aims to provide a preparation method of 2-butoxyethyl methacrylate. The preparation method provided by the invention does not need to use a solvent in the transesterification reaction stage, and the prepared product has high purity. In order to achieve the above object, the present invention provides the following technical solutions: The invention provides a preparation method of 2-butoxyethyl methacrylate, which comprises the following steps: Mixing methyl methacrylate, ethylene glycol monobutyl ether, a polymerization inhibitor and tetrabutyl titanate for transesterification reaction to obtain a crude product, wherein the temperature of the transesterification reaction is 90-100 ℃; Adding an organic solvent, acid liquor and alkali metal salt solution into the crude product, and then filtering to obtain filtrate; And (3) oil-water separation is carried out on the filtrate, and the obtained oil phase is subjected to reduced pressure distillation to obtain the 2-butoxyethyl methacrylate. Preferably, the transesterification reaction time is 4-6 hours. Preferably, the molar ratio of the tetrabutyl titanate to the ethylene glycol monobutyl ether is (1-4) to 20. Preferably, the mass ratio of the methyl methacrylate to the ethylene glycol monobutyl ether is 3.4 (1-1.5). Preferably, the polymerization inhibitor is a phenolic polymerization inhibitor. Preferably, the mass ratio of the polymerization inhibitor to the methyl methacrylate is 0.02 (50-150). Preferably, after the transesterification reaction is finished, the reaction system is distilled under reduced pressure to obtain a crude product. Preferably, the acid solution is hydrochloric acid or sulfuric acid. Preferably, the filtering material used in the filtering is diatomite. Preferably, the temperature of the reduced pressure distillation is 90-120 ℃. The invention provides a preparation method of 2-butoxyethyl methacrylate, which comprises the steps of mixing methyl methacrylate, ethylene glycol monobutyl ether, a polymerization inhibitor and tetrabutyl titanate for transesterification reaction to obtain a crude product, adding an organic solvent, an acid solution and an alkali metal salt solution into the crude product, filtering to obtain a filtrate, carrying out oil-water separation on the filtrate, and carrying out reduced pressure distillation on an obtained oil phase to obtain the 2-butoxyethyl methacrylate. The invention takes tetrabutyl titanate as the catalyst of the transesterification reaction, which can effectively reduce the activation energy of the transesterification reaction, so that the transesterification reaction can be carried out at a lower temperature in a shorter time; the mild reaction condition and the high selectivity of tetrabutyl titanate to transesterification reduce the reaction temperature, reduce the self-polymerization of Methyl Methacrylate (MMA) and the dehydration of ethylene glycol monobutyl ether, improve the purity of the product