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Pentaerythritol tetraacrylate preparation method

A technology of pentaerythritol acrylate and pentaerythritol, which is applied in the field of esterification, can solve the problems of poor decolorization effect of pentaerythritol acrylate, and achieve the effect of obvious decolorization effect, simple operation and easy control

Active Publication Date: 2015-09-02
SHANGHAI PHICHEM MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problem of poor decolorization effect of pentaerythritol acrylate in the prior art, the embodiment of the present invention provides a preparation method of pentaerythritol acrylate

Method used

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Embodiment 1

[0028] As attached figure 1 As shown, the embodiment of the present invention provides a method for preparing pentaerythritol acrylate, the method including:

[0029] Step 101: Add pentaerythritol, acrylic acid, solvent, catalyst and first polymerization inhibitor to the reactor, and heat the reactor to a preset temperature.

[0030] Step 102: Make the reaction system reflux and react at the preset temperature, and track the molar ratio of pentaerythritol triacrylate to pentaerythritol tetraacrylate in the reaction system, when the molar ratio of pentaerythritol triacrylate to pentaerythritol tetraacrylate is 1:3- At 10 o'clock, the reflux reaction was ended.

[0031] Step 103: After the reaction system is cooled, the reaction system is washed with water and alkali washed, and the first organic phase is taken.

[0032] Step 104: Wash the first organic phase with a reducing agent, then wash the first organic phase with water until it is neutral, and take the second organic phase.

[003...

Embodiment 2

[0036] As attached figure 2 As shown, the embodiment of the present invention provides a method for preparing pentaerythritol acrylate, the method including:

[0037] Step 201: Add pentaerythritol, acrylic acid, solvent, catalyst and first polymerization inhibitor to a four-necked flask equipped with thermometer, water trap, serpentine condenser and stirring blade, and heat the reactor to 80-100°C .

[0038] Specifically, the molar ratio of pentaerythritol and acrylic acid is 1:4-8, preferably 1:4-6.5. In the embodiment of the present invention, to ensure that the molar ratio of pentaerythritol triacrylate to pentaerythritol tetraacrylate is 1:3-10, and to ensure a higher conversion rate of pentaerythritol and acrylic acid, the molar ratio of pentaerythritol to acrylic acid is determined to be 1:4 -8, preferably 1:4-6.5. The desired low hydroxyl value pentaerythritol acrylate is prepared by the above-mentioned ratio of pentaerythritol and acrylic acid.

[0039] Wherein, the firs...

Embodiment 3

[0054] 28.87g pentaerythritol, 61.13g acrylic acid, 49.5g toluene, 48.7g cyclohexane, 1.35g methanesulfonic acid, 1.35g HND-6 solid super acid, 0.3g copper sulfate pentahydrate, 0.045g p-hydroxyanisole Put it into a 500ml four-necked flask equipped with a thermometer, a water trap, a serpentine condenser and a stirring blade, and add 13.2 g of toluene and 12.4 g of cyclohexane into the water trap.

[0055] Turn on the oil bath heating device, heat the reaction system to a temperature of 90°C, and reflux for 15 hours. When the ratio of pentaerythritol triacrylate to pentaerythritol tetraacrylate in the reaction system reaches 1:3, the reflux reaction is terminated by high performance liquid chromatography.

[0056] Cool the reaction system down to 35°C, then wash the reaction system twice with a 10% sodium chloride solution, stand for layering, take the upper organic phase to determine the acid value; use an excess of 10% by weight according to the measured acid value 10% sodium hy...

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Abstract

The present invention discloses a pentaerythritol tetraacrylate preparation method, and belongs to the technical field of esterification product preparation. The method comprises: adding pentaerythrotol, acrylic acid, a solvent, a catalyst and a first polymerization inhibitor to a reactor; carrying out a reflux reaction of the reaction system at a preset temperature, and stopping the reaction when tracking a molar ratio of the pentaerythritol triacrylate to pentaerythritol tetraacrylate at 1:3-10; after cooling the reaction system, carrying out waster washing and alkali washing, and taking a first organic phase; washing the first organic phase with a reducing agent, carrying out water washing until achieving a neutral state, and taking a second organic phase; and adding a second polymerization inhibitor to the second organic phase, and carrying out pressure reducing distillation and filtering to obtain the pentaerythritol tetraacrylate. According to the present invention, the reducing agent reacting with the oxidized polymerization inhibitor is adopted as the decoloration agent to prepare the pentaerythritol tetraacrylate with characteristics of low hydroxyl value and low chrominance; and the method of the present invention is simple, is easy to control, and is suitable for scale industrial production.

Description

Technical field [0001] The invention relates to the technical field of esterification preparation, in particular to a preparation method of pentaerythritol acrylate. Background technique [0002] Pentaerythritol acrylate is a multifunctional polymerizable monomer, including pentaerythritol triacrylate and pentaerythritol tetraacrylate. Pentaerythritol acrylate contains a high-density carbon-carbon double bond structure, has excellent light curing speed and high crosslinking density, and can be widely used in light curing coatings, light curing adhesives, liquid photoresists, optical films, and adhesives. Focus on accelerators and other fields. [0003] At present, pentaerythritol acrylate is often prepared by the following method: adding toluene, p-toluenesulfonic acid, phenolic polymerization inhibitor, pentaerythritol and acrylic acid into the reactor, and at a certain temperature, the reaction system is refluxed and dehydrated for esterification. After the esterification react...

Claims

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Application Information

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IPC IPC(8): C07C69/54C07C67/08C07C67/62
CPCC07C67/08C07C67/62C07C69/54
Inventor 严帅帅金亮曹松
Owner SHANGHAI PHICHEM MATERIAL CO LTD
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