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A kind of preparation method of three (2-hydroxyethyl) isocyanuric acid acrylate mixture

A technology of isocyanuric acid acrylate and isocyanuric acid diacrylate, which is applied in the field of preparation of triisocyanuric acid acrylate mixture, can solve the problems of uncontrollable ratio and cumbersome preparation steps, and achieve low preparation cost and wide application Application prospects, the effect of simple preparation steps

Active Publication Date: 2016-11-09
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 cumbersome preparation steps of tris (2-hydroxyethyl) isocyanurate triacrylate in the prior art, it is impossible to control the three (2-hydroxyethyl) tris (2-hydroxyethyl) isocyanurate acrylate mixture. Regarding the ratio of isocyanurate diacrylate to tris(2-hydroxyethyl)isocyanurate triacrylate, the embodiment of the present invention provides a mixture of tris(2-hydroxyethyl)isocyanurate acrylate Preparation

Method used

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  • A kind of preparation method of three (2-hydroxyethyl) isocyanuric acid acrylate mixture
  • A kind of preparation method of three (2-hydroxyethyl) isocyanuric acid acrylate mixture
  • A kind of preparation method of three (2-hydroxyethyl) isocyanuric acid acrylate mixture

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Embodiment 1

[0028] The embodiment of the present invention provides a method for preparing a tris(2-hydroxyethyl)isocyanurate acrylate mixture, the method comprising:

[0029] Step 1: add three (2-hydroxyethyl) isocyanurate, acrylic acid, solvent, catalyst and the first polymerization inhibitor successively in the reactor, and described reactor is equipped with thermometer, water divider, serpentine Condenser tube, four-necked flask with stirring paddle, mix the above materials evenly by stirring to obtain a reaction system, and fill the water separator with solvent at the same time;

[0030] Step 2: Turn on the oil bath heating device, heat the four-necked flask, keep the temperature of the reaction system at 80-100°C, and at the same time feed air into the reaction system during the heating process, and heat the reaction system to reflux in the reactor for 4 ~ 8 hours, during which the reaction system carried out a chemical reaction in the reactor, and three (2-hydroxyethyl) isocyanurat...

Embodiment 2

[0067] The embodiment of the present invention provides a kind of preparation method of tris (2-hydroxyethyl) isocyanurate acrylate mixture, and described preparation method comprises:

[0068] Step 1: In a 500ml four-necked flask equipped with a thermometer, a water separator, a serpentine condenser, and a stirring paddle, 60.0g tris (2-hydroxyethyl) isocyanurate, 62.1g acrylic acid, and 33.0g toluene were successively , 40.3g ethyl acetate, 1.53g methanesulfonic acid, 1.53g HND-6 solid superacid, 0.3g copper sulfate pentahydrate, 0.01g p-hydroxyanisole were put into;

[0069]Among them, the mass ratio of tris(2-hydroxyethyl)isocyanurate to acrylic acid is 1:1.035, the solvent is toluene and ethyl acetate, the ratio of toluene to ethyl acetate is 1:1.22, and the solvent is 73.3g in total. And solvent is 60% of three (2-hydroxyethyl) isocyanurate and acrylic acid gross mass, and catalyzer is methanesulfonic acid and HND-6 solid superacid, and catalyzer is 3.06g altogether, and...

Embodiment 3

[0081] The embodiment of the present invention provides a kind of preparation method of tris (2-hydroxyethyl) isocyanurate acrylate mixture, and described preparation method comprises:

[0082] Step 1: In a 500ml four-necked flask equipped with a thermometer, a water separator, a serpentine condenser, and a stirring paddle, 60.0g tris (2-hydroxyethyl) isocyanurate, 41.4g acrylic acid, and 40.6g toluene were successively , 4.04g methanesulfonic acid, 0.05g copper sulfate pentahydrate, 0.01g cuprous chloride, 0.01g p-tert-butylcatechol;

[0083] Wherein the mass ratio of three (2-hydroxyethyl) isocyanurate and acrylic acid is 1:0.69, solvent is toluene, solvent is 40.6g, and solvent is three (2-hydroxyethyl) isocyanurate and 40% of the total mass of acrylic acid, the catalyst is methanesulfonic acid, the catalyst is 4.04g in total, and the catalyst is 4% of the total mass of three (2-hydroxyethyl) isocyanurate and acrylic acid, and the first polymerization inhibitor is Copper s...

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Abstract

The invention discloses a preparation method of a tri(2-ethoxy) isocyanurate acrylate mixture and belongs to the chemical engineering field. The method comprises the following steps: adding a reaction material into a reactor and uniformly mixing; heating a reaction system to 80-100 DEG C and maintaining for 4-8 hours, after reaction, cooling and washing, then standing for layering, and taking an upper organic phase; adding a polymerization inhibitor into the organic phase and decompressing and distilling to remove a solvent in the organic phase; and pressurizing and filtering the organic phase to obtain the tri(2-ethoxy) isocyanurate acrylate mixture. According to the preparation method disclosed by the invention, the reaction temperature is 80-100 DEG C, and impurities in the reaction system are removed by washing for 3-5 times; the solvent is separated from the reaction system by decompression and distillation, and pressurization and filtration are carried out to obtain a pure mixture. The mixture is simple in preparation step, relatively low in cost and can be industrially produced on a large scale; meanwhile, the proportion of tri(2-ethoxy) isocyanurate diacrylate and tri(2-ethoxy) isocyanurate triacrylate can be tracked, and the reaction is finished in any proportion to obtain mixtures with different chemical properties.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for preparing a tris(2-hydroxyethyl)isocyanurate acrylate mixture. Background technique [0002] UV curing technology is a new technology of energy saving and environmental protection, which is applied in the fields of coatings, inks, adhesives, electronics and composite materials. UV curing materials need to have excellent water resistance, chemical resistance, wear resistance, impact resistance, It has chemical properties such as heat resistance, and has the characteristics of high hardness, low shrinkage rate and good adhesion to weakly polar substrates. At present, tris (2-hydroxyethyl) isocyanurate acrylate is used as UV curing material. At the same time, three (2-hydroxyethyl) isocyanurate acrylate is also widely used in light-curing adhesives, adhesion promoters, plastic coatings, metal coatings, wood coatings, liquid photoresists, optical films , screen printing...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D251/34
CPCC07D251/34
Inventor 帅晶亮曹松
Owner ANQING FEIKAI NEW MATERIAL CO LTD
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