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Preparation method of phenoxy benzyl acrylic ester

A technology of phenoxybenzyl acrylate and acrylic acid, applied in the field of preparation of phenoxybenzyl acrylate, can solve the problems of limited effect, increase production cost and the like, and achieve cost saving, low chromaticity and low reaction temperature. Effect

Inactive Publication Date: 2014-02-05
SHANGHAI WEIKAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In order to obtain a light-colored product, there is also a method of decolorizing the final product with decolorizers such as activated carbon, activated alumina, and activated clay, but the effect of this method is also very limited, and it is almost impossible to obtain a nearly colorless product.
In addition, because the product needs further post-treatment processes such as decolorization and filtration, the production cost is increased.

Method used

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  • Preparation method of phenoxy benzyl acrylic ester
  • Preparation method of phenoxy benzyl acrylic ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 10 grams of 3-phenoxybenzyl alcohol, 4.32 grams of acrylic acid, 30 grams of cyclohexane, 0.24 grams of methanesulfonic acid, and p-hydroxyl Anisole 0.072 gram, 50wt% hypophosphorous acid aqueous solution 0.286 gram, in the reaction process, lead nitrogen protection always, after reflux reaction at 80~85 ℃ for 5 hours, generate about 0.9 milliliters of water, continue to reflux for 2 hours, the water quantity is constant.

[0033] After the reaction, the reaction mixture was washed twice with 5% aqueous sodium hydroxide solution, then washed three times with distilled water, and finally dried with anhydrous magnesium sulfate, and then 0.02 p-hydroxyanisole, a polymerization inhibitor, was added to the dried solution. gram, at 50 DEG C, vacuum degree is under 0.1MPa condition, removes solvent cyclohexane with rotary evaporator, obtains colorless transparent product-phenoxybenzyl acrylate (11.56 grams, yield is 91%), gas chromatography The analyzer purity was 96.7% an...

Embodiment 2

[0035] Add 10 grams of 3-phenoxybenzyl alcohol, 4.32 grams of acrylic acid, 30 grams of cyclohexane, 0.24 grams of methanesulfonic acid, and p-hydroxyl 0.072 grams of anisole, 0.029 grams of 50wt% hypophosphorous acid aqueous solution, nitrogen protection always in the reaction process, after reflux reaction at 80~85 ℃ for 5 hours, generate about 0.9 milliliters of water, continue to reflux for 2 hours, the amount of water remains unchanged.

[0036] After the reaction, the reaction mixture was washed twice with 5% aqueous sodium hydroxide solution, then washed three times with distilled water, and finally dried with anhydrous magnesium sulfate, and then 0.02 p-hydroxyanisole, a polymerization inhibitor, was added to the dried solution. gram, at 50 DEG C, vacuum degree is under 0.1MPa condition, removes solvent cyclohexane with rotary evaporator, obtains colorless transparent product-phenoxybenzyl acrylate (11.94 grams, yield is 94%), gas chromatography The analyzer purity was...

Embodiment 3

[0038] Add 10 grams of 3-phenoxybenzyl alcohol, 4.32 grams of acrylic acid, 30 grams of cyclohexane, 0.24 grams of methanesulfonic acid, and p-hydroxyl Anisole 0.072 gram, 50wt% hypophosphorous acid aqueous solution 0.572 gram, nitrogen protection is always passed through in the reaction process, after reflux reaction at 80~85 ℃ for 5 hours, generate about 0.9 milliliters of water, continue to reflux 2 hours, the water quantity is constant.

[0039]After the reaction, the reaction mixture was washed twice with 5% aqueous sodium hydroxide solution, then washed three times with distilled water, and finally dried with anhydrous magnesium sulfate, and then 0.02 p-hydroxyanisole, a polymerization inhibitor, was added to the dried solution. gram, at 50 DEG C, vacuum degree is under 0.1MPa condition, removes solvent cyclohexane with rotary evaporator, obtains colorless transparent product-phenoxybenzyl acrylate (12.32 grams, yield is 97%), gas chromatography The analyzer purity was 9...

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Abstract

The invention discloses a preparation method of phenoxy benzyl acrylic ester. The preparation method comprises the steps of: under the protection of nitrogen, taking cyclohexane as a solvent and adopting an organic acid as a catalyst, subjecting 3-phenoxy benzyl alcohol and acrylic acid to an esterification reaction in the presence of a polymerization inhibitor and a reducing agent; and at the end of the esterification reaction, removing the cyclohexane by means of alkali washing, water scrubbing, drying, and pressure reduction, thus obtaining the phenoxy benzyl acrylic ester. The dosage of the reducing agent accounts for 0.1-2wt% of the total weight of 3-phenoxy benzyl alcohol and acrylic acid. The method provided by the invention has the advantages of low reaction temperature and simple process, and can produce aromatic ring containing acrylic ester that has low chroma and is even colorless and transparent.

Description

technical field [0001] The invention relates to a preparation method of aromatic acrylate, in particular to a preparation method of phenoxybenzyl acrylate. Background technique [0002] Acrylate polymers or copolymers containing aromatic rings in the molecular structure are widely used in optical materials such as optical resins, optical coatings, optical adhesives, optical lenses and glasses manufacturing due to their excellent transparency and high refractive index . [0003] Because these fields all require colorless and transparent products, it is necessary to use monomers with low chroma or even colorless products. Generally, low-grade acrylates are obtained by vacuum distillation to obtain colorless and transparent products. However, because of the high boiling point of acrylates containing aromatic rings, even if a polymerization inhibitor is added, polymerization easily occurs during the vacuum distillation process. The distillation method is not suitable for the p...

Claims

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Application Information

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IPC IPC(8): C07C69/54C07C67/08
CPCC07C67/08
Inventor 虞明东王艳梅
Owner SHANGHAI WEIKAI CHEM
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