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Method for preparing modified epoxy acrylate

A technology of epoxy acrylate and hydroxy acrylate, applied in the field of preparing modified epoxy acrylate, can solve the problems of adverse effects of acrylic substrate and cured film, difficult temperature control, etc., and achieve the effect of increasing molecular weight and reducing Tg

Active Publication Date: 2013-03-27
江苏三木化工股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The existing epoxy acrylate is mainly formed by ring-opening esterification of epoxy resin and acrylic acid. During the synthesis process, the molar ratio of epoxy resin to acrylic acid is required to be extremely accurate. At the same time, the reaction is a strong exothermic reaction. Temperature is difficult to control; a small amount of acrylic acid residues can adversely affect both the substrate and the cured film

Method used

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  • Method for preparing modified epoxy acrylate
  • Method for preparing modified epoxy acrylate
  • Method for preparing modified epoxy acrylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Synthesis of intermediates: Add 98 kg of maleic anhydride, 116 kg of hydroxyethyl acrylate, 0.3 kg of hypophosphorous acid and 0.5 kg of p-hydroxyanisole into the reactor in sequence, stir evenly, and heat up to 90°C for 2.5 Hours, check the acid value to the theoretical value (212mgKOH / g), discharge (denoted as A), and stand by;

[0035] (2) Organic acid chain extension: Put 464 kg of epoxy resin 828, 15 kg of adipic acid and 1 kg of triethylamine into the reaction kettle according to the formula, stir evenly, slowly raise the temperature to 90°C for 3 hours, and check the acidity. After the value is less than or equal to 1 mgKOH / g, turn on the cooling water and reduce the temperature to 50°C;

[0036] (3) Esterification reaction at elevated temperature: Add material A, 2 kg of triethylamine, 0.8 kg of p-hydroxyanisole, 2 kg of 2,5-dimethylhydroquinone, and 0.2 kg of hypophosphorous acid in sequence according to the formula In the reaction kettle; heat up, when th...

Embodiment 2

[0041] (1) Synthesis of intermediates: Add 98 kg maleic anhydride, 116 kg hydroxyethyl methacrylate, 0.3 kg hypophosphorous acid and 0.5 kg p-hydroxyanisole into the reaction kettle in sequence, stir evenly, and heat up to 80°C React for 3 hours, check the acid value to (212mgKOH / g), discharge (recorded as A), and set aside;

[0042] (2) Organic acid chain extension: Put 464 kg of epoxy resin 828, 15 kg of adipic acid and 1 kg of triethylamine into the reaction kettle according to the formula, stir evenly, slowly raise the temperature to 95°C for 3 hours, and check the acid After the value is less than or equal to 1 mgKOH / g, turn on the cooling water and reduce the temperature to 60°C;

[0043] (3) Esterification reaction at elevated temperature: Add material A, 2 kg of triethylamine, 0.8 kg of p-hydroxyanisole, 2 kg of 2,5-dimethylhydroquinone, and 0.2 kg of hypophosphorous acid in sequence according to the formula In the reaction kettle; heat up, when the temperature reache...

Embodiment 3

[0048] (1) Synthesis of intermediates: Add 139 kg of phthalic anhydride, 106 kg of hydroxyethyl acrylate, 0.3 kg of hypophosphorous acid and 0.5 kg of p-hydroxyanisole into the reactor in sequence, stir evenly, and heat up to 110°C for 2.5 hours , after checking the acid value to the theoretical value (212 mgKOH / g), discharge the material (denoted as A) and wait for use;

[0049] (2) Organic acid chain extension: Put 414 kg of epoxy resin 828, 14 kg of sebacic acid and 1 kg of triphenylphosphine into the reaction kettle according to the formula, stir evenly, slowly raise the temperature to 105°C for 2 hours, and check After the acid value is ≤1 mgKOH / g, turn on the cooling water and reduce the temperature to 65°C;

[0050] (3) Esterification reaction at elevated temperature: Add material A, 2 kg of triphenylphosphine, 0.5 kg of p-hydroxyanisole, 2 kg of 2,5-dimethylhydroquinone, and 0.2 kg of hypophosphorous acid in sequence according to the formula Put it into the reaction ket...

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Abstract

The invention discloses a method for preparing modified epoxy acrylate. The method comprises the following steps of: (1) synthesizing an intermediate: adding anhydride, hydroxyl acrylate monomers, an anti-oxidant 1 and a polymerization inhibitor 1 in turn into a reaction kettle in turn, uniformly stirring, heating to the temperature of between 80 and 120DEG C, reacting for 2 to 3 hours, and discharging a material (marked as A) for later use; (2) expanding chain of organic acid: adding epoxy resin, organic diacid and a catalyst 1 into the reaction kettle in a formula ratio, uniformly stirring, slowly heating to the temperature of between 90 and 120DEG C, reacting for 2 to 3 hours, and after the acid value is less than or equal to 1mgKOH / g, starting cooling water to cool to the temperature of between 50 and 70DEG C; (3) heating for esterification: adding the material A, a catalyst 2, a polymerization inhibitor 2 and an anti-oxidant 2 into the reaction kettle in a formula ratio in turn, heating and keeping temperature; (4) cooling and diluting; and (5) performing central control inspection. The molecular weight can be properly increased, flexible groups can be increased, and the glass-transition temperature of the product is reduced.

Description

technical field [0001] The invention relates to the technical field of UV resins, in particular to a method for preparing modified epoxy acrylate. Background technique [0002] The development of communication resins is closely related to the communication industry and provides the basis for the development of the communication industry. Internationally, communication resins are monopolized by a few multinational companies. At present, the production of products is mainly concentrated in more than ten companies such as BASF and Bayer in Germany, Sartomer and Cytec in the United States, and their production capacity accounts for about 90% of the world's total production capacity. The production and application research of domestic communication resins lags behind western developed countries. The production scale is small, the technology is backward, the purity is low, the viscosity is high, and the product quality is poor. It has been unable to meet the market demand for many...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/14C08G59/16C09D163/10
Inventor 薛中群惠正权罗侃仝伟葛文成马希海曹磊
Owner 江苏三木化工股份有限公司
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