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4-hydroxybutyl methacrylate and preparation method thereof

A technology of methacrylic acid and hydroxybutyl ester, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, etc., to achieve the effects of improving conversion rate, product yield, and excellent catalytic effect

Active Publication Date: 2020-12-11
WENZHOU GUOSHIBANG POLYMER MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the generation of by-products and the hydrolysis of esters in the presence of water still cause many problems in the reaction system.

Method used

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  • 4-hydroxybutyl methacrylate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] A method for preparing 4-hydroxybutyl methacrylate, comprising the following steps;

[0038] Stoichiometry is performed first, the molar ratio of tetrahydrofuran to methacrylic acid is 2:1.

[0039] (1) Nitrogen replacement to an oxygen content of ≤100ppm, adding methacrylic acid and 1 / 2 mass inhibitor, heating up to 105°C, vacuum dehydration for 1.5h, and detecting moisture ≤0.5%; dehydrated methacrylic acid is obtained;

[0040] (2) Mix deionized water and sodium bicarbonate and stir evenly to obtain a saturated sodium bicarbonate solution; add tetrahydrofuran to the saturated sodium bicarbonate solution, stir for 30 minutes, and separate to obtain dehydrated tetrahydrofuran;

[0041] (3) dissolving boron trifluoride in capric acid ester solution and dispersing at high speed to obtain a catalyst; the boron fluoride content in the catalyst is 4%, and the capric acid ester content is 96%.

[0042] (4) Take dehydrated tetrahydrofuran, the remaining 1 / 2 mass of the polym...

Embodiment 2

[0044]A method for preparing 4-hydroxybutyl methacrylate, comprising the following steps;

[0045] Stoichiometry was performed first, the molar ratio of tetrahydrofuran to methacrylic acid was 2.5:1.

[0046] (1) Nitrogen replacement to an oxygen content of ≤ 100ppm, adding methacrylic acid and 1 / 2 mass inhibitor, heating up to 105°C, vacuum dehydration for 1.8h, and detecting moisture ≤ 0.5%; to obtain dehydrated methacrylic acid;

[0047] (2) Mix deionized water and sodium bicarbonate and stir evenly to obtain a saturated sodium bicarbonate solution; add tetrahydrofuran to the saturated sodium bicarbonate solution, stir for 37 minutes, and separate to obtain dehydrated tetrahydrofuran;

[0048] (3) dissolving boron trifluoride in capric acid ester solution and dispersing at high speed to obtain a catalyst; the boron fluoride content in the catalyst is 5%, and the capric acid ester content is 95%.

[0049] (4) Take dehydrated tetrahydrofuran, the remaining 1 / 2 mass of the po...

Embodiment 3

[0051] A method for preparing 4-hydroxybutyl methacrylate, comprising the following steps;

[0052] Stoichiometry is performed first, the molar ratio of tetrahydrofuran to methacrylic acid is 3:1.

[0053] (1) Nitrogen replacement to an oxygen content of ≤ 100ppm, adding methacrylic acid and 1 / 2 mass inhibitor, heating up to 105°C, vacuum dehydration for 1.8h, and detecting moisture ≤ 0.5%; to obtain dehydrated methacrylic acid;

[0054] (2) Mix deionized water and sodium bicarbonate and stir evenly to obtain a saturated sodium bicarbonate solution; add tetrahydrofuran to the saturated sodium bicarbonate solution, stir for 43 minutes, and separate to obtain dehydrated tetrahydrofuran;

[0055] (3) dissolving boron trifluoride in capric acid ester solution and dispersing at high speed to obtain a catalyst; the boron fluoride content in the catalyst is 5%, and the capric acid ester content is 95%.

[0056] (4) Take dehydrated tetrahydrofuran, the remaining 1 / 2 mass of the polym...

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Abstract

The invention discloses 4-hydroxybutyl methacrylate and a preparation method thereof. The 4-hydroxybutyl methacrylate is mainly prepared by carrying out ring-opening addition reaction on tetrahydrofuran, methacrylic acid and a polymerization inhibitor under the action of a catalyst and then separating tetrahydrofuran through distillation, wherein the catalyst is prepared by mixing boron trifluoride and decanoate, the content of boron fluoride in the catalyst is 4%-8%, and the content of decanoate in the catalyst is 92%-96%. The preparation method has the advantages of high reaction activity, high reaction selectivity, high yield, no environmental pollution, no by-product, easiness in industrial quantitative production and the like, and the prepared 4-hydroxybutyl methacrylate can be applied to the fields of coatings, printing ink, automobile coating, special functional resin and the like.

Description

technical field [0001] The invention relates to the technical field of organic monomer synthesis, in particular to 4-hydroxybutyl methacrylate and a preparation method thereof. Background technique [0002] 4-hydroxybutyl methacrylate is a new type of special functional monomer, which is mainly used in the fields of synthetic resin, ink, architectural coatings, automotive metal coating, etc.; Coating resins have excellent weather resistance, scratch resistance, and radiation resistance. At present, the production sites of 4-hydroxybutyl methacrylate are mainly concentrated in Germany and Japan; my country's domestic demand is heavily dependent on imports, which brings about the problem of high cost and limited application. Therefore, it is very necessary to develop a production method suitable for mass production and cost controllable. [0003] At present, there are few reports on the synthesis process of 4-hydroxybutyl methacrylate; Zhang Yuchuan introduced 1,4-butyl A p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/54C07C67/24B01J31/02
CPCC07C67/24C07C69/54B01J31/0209C07C2531/02B01J2231/49
Inventor 张善志
Owner WENZHOU GUOSHIBANG POLYMER MATERIALS