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Preparation method of pentaerythritol tetraacrylate mixture

A technology of pentaerythritol acrylate and pentaerythritol, which is applied in the field of preparation of pentaerythritol acrylate mixtures, can solve the problems of many impurities, high chroma, and low yield, and achieve high purity, simple preparation process, and less impurities.

Active Publication Date: 2015-04-15
ANQING FEIKAI NEW 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 problems of more impurities, lower purity, lower yield and higher chroma in the prior art, the embodiment of the present invention provides a preparation method of pentaerythritol acrylate mixture

Method used

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  • Preparation method of pentaerythritol tetraacrylate mixture
  • Preparation method of pentaerythritol tetraacrylate mixture

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Embodiment 1

[0029] Such as figure 1 As shown, the embodiment of the present invention provides a method for preparing a pentaerythritol acrylate mixture, and the method for preparing the pentaerythritol acrylate mixture includes:

[0030] Step 1: Add pentaerythritol, acrylic acid, solvent, catalyst, first polymerization inhibitor and antioxidant to the reactor in sequence, and mix the above materials uniformly to obtain a reaction system, wherein the reactor is equipped with a thermometer, a water separator, a snake Four-necked flask with shaped condenser, stirring paddle and vent pipe;

[0031] Step 2: Turn on the heating device and heat the reactor to keep the temperature of the reaction system at 60-110°C and reflux the reaction system at a constant temperature. At the same time, a protective gas is introduced into the reaction system. The protective gas adopts a process The mixed gas of air and nitrogen keeps the flow of the mixed gas at 0.1~1000m3 / h. The mixed gas of process air and nitr...

Embodiment 2

[0121] Such as figure 1 As shown, the embodiment of the present invention provides a method for preparing a pentaerythritol acrylate mixture, and the method for preparing the pentaerythritol acrylate mixture includes:

[0122] Step 1: Add 60.0g pentaerythritol, 114.4g acrylic acid, 47.0g toluene, 82.3g cyclohexane, 1.85g formaldehyde into a four-necked flask equipped with thermometer, water trap, serpentine condenser, stirring blade and vent pipe. Sulfonic acid, 1.85g p-toluenesulfonic acid, 0.3g copper sulfate pentahydrate, 0.01g p-hydroxyanisole, 0.7g 2,6-di-tert-butyl-p-cresol and mixed uniformly to obtain a reaction system;

[0123] Among them: the mass ratio of pentaerythritol and acrylic acid is 1:1.9, the solvent is toluene and cyclohexane, the ratio of toluene and cyclohexane is 1:1.75, the total solvent is 129.3g, and the solvent is 41.9% of the total mass of the reaction system. The catalyst is methanesulfonic acid and p-toluenesulfonic acid. The total catalyst is 3.7g, ...

Embodiment 3

[0135] Such as figure 1 As shown, the embodiment of the present invention provides a method for preparing a pentaerythritol acrylate mixture, and the method for preparing the pentaerythritol acrylate mixture includes:

[0136] Step 1: Add 60.0g pentaerythritol, 130.7g acrylic acid, 76g benzene, 76g toluene, 2.86g methanesulfonic acid, into a four-necked flask equipped with a thermometer, a water trap, a serpentine condenser, a stirring blade, and a vent pipe. 2.86g solid super acid, 0.7g hydroquinone, 0.25g copper acetate, 1.28g 2,6-di-tert-butyl-p-cresol and mixed uniformly to obtain a reaction system;

[0137] Among them: the mass ratio of pentaerythritol and acrylic acid is 1:2.12, the solvent is benzene and toluene, the ratio of benzene to toluene is 1:1, the total solvent is 152g, and the solvent is 43.3% of the total mass of the reaction system, and the catalyst is methylsulfonate Acid and solid super acid, the total catalyst is 5.72g, and the catalyst is 3% of the total mas...

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Abstract

The invention discloses a preparation method of a pentaerythritol tetraacrylate mixture and belongs to the field of chemical engineering. The preparation method comprises following processes: (1) feeding reaction materials into a reactor and mixing the reaction materials uniformly; (2) heating the reaction system to perform constant-temperature reflux to obtain reaction products; (3) cooling the reaction products and washing the reaction products, allowing the reaction products to stand for being layered and obtaining an upper-layer organic phase; (4) adding a reducing agent to the organic phase for decoloration; (5) adding a polymerization inhibitor and removing solvents in the organic phase in a manner of reduced pressure distillation and molecular distillation; and (6) adding a diluent with mixing and performing pressurized filtration to obtain a finish product. The preparation method is free of generation of harmful gases, thereby avoiding air pollution. By means of the washing process, residual acrylic acid and other impurities in the reaction system are removed. By means of the reduced pressure distillation for separating the solvents and the reaction system and the molecular distillation for removing residual solid impurities, the pure finish product is obtained. By means of usage of an anti-oxidizing agent, feeding of a protective gas and the decoloration, yield of the finish product is increased and chroma of the finish product is reduced. By means of addition of the diluent, the finished product is enhanced in stability, is improved in application performances and is wider in application range.

Description

Technical field [0001] The invention relates to the field of chemical engineering, in particular to a method for preparing a pentaerythritol acrylate mixture. Background technique [0002] The pentaerythritol acrylate mixture is a kind of viscosity of 500±200cps, refractive index of 1.4603±0.01, density of 1.17-1.18 at 20°C, molecular weight of 352, and appearance of colorless or light yellow liquid. The pentaerythritol acrylate mixture has excellent properties such as high crosslink density, fast curing, scratch resistance, good flexibility, low volatility, chemical resistance, etc., and is widely used in coatings, inks, electronics, photopolymers and composite materials and other fields , Mainly used as diluent and adhesive. [0003] In the prior art, most of the reactions are carried out by reacting the reaction material, neutralizing the acid remaining in the reaction process, adding magnesium silicate to adsorb the salt generated during the reaction process, dehydrating, deso...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/54C07C67/08
CPCC07C67/08C07C67/48C07C67/58C07C67/62C07C69/54
Inventor 程为中谭鹏池萍邱晓生
Owner ANQING FEIKAI NEW MATERIAL CO LTD
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