CN-122010726-A - Method for preparing 2-methyl-2-acrylic acid-2-butoxyethyl ester by taking aluminum isopropoxide as catalyst

Abstract

The invention provides a method for preparing 2-methyl-2-acrylic acid-2-butoxyethyl ester by taking aluminum isopropoxide as a catalyst, belonging to the technical field of chemical synthesis. The invention takes aluminum isopropoxide as a catalyst for transesterification reaction, has less side reaction and high product purity. The results of the examples show that the purity of the product obtained by the method provided by the invention is higher than 99.5%.

Inventors

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

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 method for preparing 2-methyl-2-butoxyethyl 2-acrylate by using aluminum isopropoxide as a catalyst, which comprises the following steps: Methyl methacrylate, ethylene glycol monobutyl ether, aluminum isopropoxide and a polymerization inhibitor are mixed and subjected to transesterification reaction to obtain a crude product; adding an organic solvent, an acid solution and an alkali metal salt solution into the crude product, and then carrying out solid-liquid separation to obtain a liquid phase; Oil-water separation is carried out on the liquid phase, and the obtained oil phase is subjected to first reduced pressure distillation to obtain a crude product of 2-methyl-2-acrylic acid-2-butoxyethyl ester; Rectifying the crude product of the 2-methyl-2-acrylic acid-2-butoxyethyl ester to obtain the 2-methyl-2-acrylic acid-2-butoxyethyl ester.
2. 2. The method of claim 1, wherein the molar ratio of methyl methacrylate to ethylene glycol monobutyl ether is (3-5): 1.
3. 3. The method according to claim 1 or 2, wherein the molar ratio of methyl methacrylate to aluminum isopropoxide is 4 (0.05-0.15).
4. 4. The method according to claim 1, wherein the transesterification reaction is carried out at a temperature of 90-100 ℃.
5. 5. The method according to claim 1 or 4, wherein the transesterification reaction is carried out for 2 to 6 hours.
6. 6. The method according to claim 1, wherein the polymerization inhibitor is used in an amount of 0.01 to 0.02% by mass of methyl methacrylate.
7. 7. The method of claim 1, wherein the acid solution is hydrochloric acid or sulfuric acid.
8. 8. The method according to claim 1, wherein the first reduced pressure distillation has a vacuum degree of-0.09 to-0.1 MPa and a temperature of 90 to 120 ℃.
9. 9. The method according to claim 1, wherein the obtained system is subjected to second reduced pressure distillation after the transesterification reaction is completed to obtain a crude product, and the second reduced pressure distillation has a vacuum degree of-0.09 to-0.1 MPa and a temperature of 90-120 ℃.
10. 10. The method according to claim 1, wherein the rectification is vacuum rectification, and the vacuum degree of the vacuum rectification is-0.09 to-0.1 MPa, and the temperature is 110-130 ℃.

Description

Method for preparing 2-methyl-2-acrylic acid-2-butoxyethyl ester by taking aluminum isopropoxide as catalyst Technical Field The invention belongs to the technical field of chemical synthesis, and particularly relates to a method for preparing 2-methyl-2-acrylic acid-2-butoxyethyl ester by taking aluminum isopropoxide as a catalyst. Background The 2-methyl-2-acrylic acid-2-butoxyethyl ester is a functional acrylic ester monomer, can be used for synthesizing high polymer materials, coatings, adhesives and the like, and has wide application in the field of organic synthesis. At present, the preparation method of the 2-methyl-2-acrylic acid-2-butoxyethyl ester mainly uses Methyl Methacrylate (MMA) and ethylene glycol monobutyl ether as raw materials, uses protonic acid as a catalyst, and adds a solvent to prepare the catalyst. The method has the advantages of byproduct generation, low purity of the product obtained after rectification, and yellowing of the product. Disclosure of Invention The invention aims to provide a method for preparing 2-methyl-2-acrylic acid-2-butoxyethyl ester by taking aluminum isopropoxide as a catalyst. The method provided by the invention has no byproduct generation and high product purity. In order to achieve the above object, the present invention provides the following technical solutions: the invention provides a method for preparing 2-methyl-2-acrylic acid-2-butoxyethyl ester by taking aluminum isopropoxide as a catalyst, which comprises the following steps: Methyl methacrylate, ethylene glycol monobutyl ether, aluminum isopropoxide and a polymerization inhibitor are mixed and subjected to transesterification reaction to obtain a crude product; adding an organic solvent, an acid solution and an alkali metal salt solution into the crude product, and then carrying out solid-liquid separation to obtain a liquid phase; Oil-water separation is carried out on the liquid phase, and the obtained oil phase is subjected to first reduced pressure distillation to obtain a crude product of 2-methyl-2-acrylic acid-2-butoxyethyl ester; Rectifying the crude product of the 2-methyl-2-acrylic acid-2-butoxyethyl ester to obtain the 2-methyl-2-acrylic acid-2-butoxyethyl ester. Preferably, the molar ratio of the methyl methacrylate to the ethylene glycol monobutyl ether is (3-5): 1. Preferably, the molar ratio of the methyl methacrylate to the aluminum isopropoxide is 4 (0.05-0.15). Preferably, the temperature of the transesterification reaction is 90-100 ℃. Preferably, the transesterification reaction time is 2-6 hours. Preferably, the amount of the polymerization inhibitor is 0.01-0.02% of the mass of the methyl methacrylate. Preferably, the acid solution is hydrochloric acid or sulfuric acid. Preferably, the vacuum degree of the first reduced pressure distillation is-0.09 to-0.1 MPa, and the temperature is 90-120 ℃. Preferably, after the transesterification reaction is completed, performing second reduced pressure distillation on the obtained system to obtain a crude product, wherein the vacuum degree of the second reduced pressure distillation is-0.09 to-0.1 MPa, and the temperature is 90-120 ℃. Preferably, the rectification is vacuum rectification, wherein the vacuum degree of the vacuum rectification is-0.09 to-0.1 MPa, and the temperature is 110-130 ℃. The invention provides a method for preparing 2-methyl-2-butoxyethyl acrylate by taking aluminum isopropoxide as a catalyst, which comprises the steps of mixing methyl methacrylate, ethylene glycol monobutyl ether, aluminum isopropoxide and a polymerization inhibitor, performing transesterification reaction to obtain a crude product, adding an organic solvent, an acid solution and an alkali metal salt solution into the crude product, then performing solid-liquid separation to obtain a liquid phase, performing oil-water separation on the liquid phase, performing first reduced pressure distillation on an obtained oil phase to obtain a crude product of 2-methyl-2-butoxyethyl acrylate, and rectifying the crude product of 2-methyl-2-butoxyethyl acrylate to obtain 2-butoxyethyl 2-methyl-2-acrylate. The invention takes aluminum isopropoxide as a catalyst for transesterification reaction, has less side reaction and high product purity. The results of the examples show that the purity of the product obtained by the method provided by the invention reaches 99.5%. Drawings FIG. 1 is a chromatogram of a crude 2-methyl-2-propenoic acid-2-butoxyethyl ester obtained in example 1 of the present invention; FIG. 2 is a chromatogram of a crude 2-methyl-2-propenoic acid-2-butoxyethyl ester obtained in example 2 of the present invention; FIG. 3 is a chromatogram of a crude 2-methyl-2-propenoic acid-2-butoxyethyl ester obtained in example 3 of the present invention; FIG. 4 is a chromatogram of a crude 2-methyl-2-propenoic acid-2-butoxyethyl ester obtained in comparative example 1 of the present invention; FIG. 5 is a chromatogram of a crude 2-methyl-2-propenoic aci