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Preparation method of pentaerythritol triacrylate

A technology of pentaerythritol triacrylate and pentaerythritol trisodium salt, which is applied in the field of compound synthesis, can solve the problems of unsuitable modern chemical industry greening, unsatisfactory, cumbersome operation, etc., and achieve the effect of easy control of reaction, short reaction time and reliable process

Active Publication Date: 2016-06-15
SINOPHARM CHEM REAGENT
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  • Abstract
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Problems solved by technology

The synthetic method reported in existing literature is: take pentaerythritol, acrylic acid, water-carrying agent, esterification catalyst, polymerization inhibitor as raw material to carry out dehydration esterification reaction, the material that this method obtains is a mixture, simultaneously has diester, triester, Tetraester, which cannot meet the demand for high-purity pentaerythritol triacrylate in high-end light-curing coatings
In addition, the post-treatment process is cumbersome and produces a large amount of waste water, which does not meet the requirements of modern chemical greening

Method used

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  • Preparation method of pentaerythritol triacrylate
  • Preparation method of pentaerythritol triacrylate

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[0019] A preparation method of pentaerythritol triacrylate, comprising the following steps:

[0020] (1) Pentaerythritol and sodium hydroxide are dissolved in an organic solvent, and pentaerythritol trisodium salt is made by heating to reflux with water;

[0021] (2) Cool the obtained pentaerythritol trisodium salt, add a polymerization inhibitor, then dropwise add acryloyl chloride solution, and continue the reflux treatment for 2-3h;

[0022] (3) The obtained organic phase is washed and dried to obtain pentaerythritol triacrylate.

[0023] Wherein, the molar ratio of pentaerythritol and acryloyl chloride is 1:3-3.1, the molar ratio of pentaerythritol and sodium hydroxide is 1:3-3.1, and the mass volume ratio of pentaerythritol and organic solvent is 1:2.5-4.0%, and the resistance The amount of the polymerizing agent is 500-2000 ppm of the pentaerythritol weight.

Embodiment 1

[0025] Add 136.2g (1.0mol) of pentaerythritol, 120g (3.0mol) of sodium hydroxide in the reaction flask, then add 400mL of toluene as an organic solvent, heat to reflux with water under stirring, to generate the trisodium salt of pentaerythritol, then cool to room temperature , add 0.1 g of polymerization inhibitor phenothiazine, start dropwise adding a solution of 271.5 g (3.0 mol) of acryloyl chloride in 100 mL of toluene under controlled temperature, and continue the reflux reaction for 2 h after the dropwise addition. After the reaction is finished, after cooling, the inorganic salt sodium chloride generated is directly filtered off, and the obtained organic phase is washed with 200 mL of distilled water, and then dried with 40 g of anhydrous magnesium sulfate. Acrylic acid ester weighed 290.2g, the yield was 97.4%, and the gas phase purity was over 98%.

Embodiment 2

[0027] Add 136.2g (1.0mol) pentaerythritol, 122g (3.05mol) sodium hydroxide in reaction bottle, add 400mL benzene again as solvent, stir and be heated to reflux band water, to generate the trisodium salt of pentaerythritol, be cooled to room temperature subsequently, Add 0.15 g of a polymerization inhibitor pyrogallol, start to drop a solution of 276.0 g (3.05 mol) of acryloyl chloride in 100 mL of benzene under controlled temperature, and continue to reflux for 3 hours after the dropwise addition. After the reaction is finished, after cooling, the inorganic salt sodium chloride generated is directly filtered off, and the obtained organic phase is washed with 200 mL of distilled water, and then dried with 40 g of anhydrous magnesium sulfate. Acrylic acid ester weighed 287.6g, the yield was 96.5%, and the gas phase purity was over 98%.

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Abstract

The invention belongs to the technical field of synthesis of compounds and particularly relates to a preparation method of pentaerythritol triacrylate. The preparation method comprises the following steps: (1) dissolving pentaerythritol and sodium hydroxide into an organic solvent, and carrying out heating reflux in water so as to prepare pentaerythritol trisodium salt; (2) cooling pentaerythritol trisodium salt, adding a polymerization inhibitor, then dropwise adding an acryloyl chloride solution, and continuing to carry out reflux; and (3) washing and drying an obtained organic phase, so as to obtain pentaerythritol triacrylate. According to the preparation method, pentaerythritol triacrylate can be quantitatively synthesized, synthesized pentaerythritol triacrylate is high in purity and yield, the operation is simple, the reaction is easily controlled, and the process is reliable.

Description

technical field [0001] The invention belongs to the technical field of compound synthesis, and in particular relates to a preparation method of pentaerythritol triacrylate. Background technique [0002] Pentaerythritol triacrylate is an important fine chemical raw material, especially as a diluent in light-curing coatings. The synthetic method reported in existing literature is: take pentaerythritol, acrylic acid, water-carrying agent, esterification catalyst, polymerization inhibitor as raw material to carry out dehydration esterification reaction, the material that this method obtains is a mixture, simultaneously has diester, triester, Tetraesters cannot meet the demand for high-purity pentaerythritol triacrylate in high-end light-curing coatings. In addition, the post-treatment process is cumbersome and produces a large amount of waste water, which does not meet the requirements of modern chemical industry. Contents of the invention [0003] The invention mainly provi...

Claims

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Application Information

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IPC IPC(8): C07C67/14C07C69/54
CPCC07C67/14C07C69/54
Inventor 吴孝兰柯德宏张东臧云骏凌芳
Owner SINOPHARM CHEM REAGENT
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