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Preparation method of reactive acrylate crosslinking agent

A technology of acrylates and crosslinking agents, which is applied in the field of preparation of reactive acrylates crosslinking agents, can solve problems such as high acid value and high viscosity, and achieve the effects of high product purity, convenient operation and clear structure

Inactive Publication Date: 2020-06-05
ZHEJIANG HUANGMA NEW MATERIALS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this type of reactive acrylate crosslinking agent uses epoxy resin with high viscosity in the preparation process, which makes it have the disadvantages of high viscosity and high acid value.

Method used

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  • Preparation method of reactive acrylate crosslinking agent
  • Preparation method of reactive acrylate crosslinking agent

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preparation example Construction

[0020] A preparation method of reactive acrylate crosslinking agent, comprising the following steps:

[0021] S1: Put phthalic anhydride compounds and acrylate compounds into a reaction vessel with mechanical stirring, the molar ratio of the two is 1:1-1.5, in order to inhibit the polymerization of acrylate compounds, it is necessary to add the first polymerization inhibitor, which The mass percentage of the total mass of the reaction raw materials (namely acid anhydride and acrylate compound) is 0.01-0.5%. After the three are mixed, the reaction is carried out at a temperature of 80-120° C. for 4-12 hours to obtain an intermediate product.

[0022] S2: Add the second polymerization inhibitor and catalyzer in described reaction vessel, the mol ratio of described intermediate product and epoxy monomer is 1:1-10, and the quality of described second polymerization inhibitor accounts for reaction raw material ( That is, the percentage of the total mass of the intermediate product ...

Embodiment 1

[0032] A preparation method of reactive acrylate crosslinking agent, comprising the following steps:

[0033] S1: Put 296g of phthalic anhydride, 232g of hydroxyethyl acrylate, and 0.1g of the first polymerization inhibitor hydroquinone into a three-necked round-bottomed flask with mechanical stirring, start stirring, and heat up to 80°C. Stir for 12h to obtain about 524g of intermediate product;

[0034] S2: Take 264g of the intermediate and put it into the glass reactor, then put in 0.06g of the catalyst triethylamine and 0.06g of the second polymerization inhibitor hydroquinone, start stirring; raise the temperature of the glass reactor to 30°C, and start slowly dripping Add 44g of ethylene oxide, and keep the reaction temperature at 30-35°C in order to prevent the polymerization reaction of the raw materials at too high a temperature; after the ethylene oxide is added dropwise, continue to keep warm for 1 hour; then vacuumize until the glass reactor is vacuumed The temper...

Embodiment 2

[0036] A preparation method of reactive acrylate crosslinking agent, comprising the following steps:

[0037] S1: Put 296g of phthalic anhydride and 260g of hydroxypropyl acrylate into a three-neck round bottom flask with mechanical stirring, add 2.8g of the first polymerization inhibitor hydroquinone, start stirring, raise the temperature to 100°C, and stir 6h, obtain intermediate product 556g;

[0038] S2: Take 278g of the intermediate and put it into a 2.5L glass reactor, then put in 7.2g of the catalyst triethylenediamine and 3.6g of the second polymerization inhibitor p-hydroxyanisole, start stirring; raise the temperature of the glass reactor to 50 ℃, began to slowly drop 440g of ethylene oxide, in order to prevent the polymerization reaction of raw materials from excessive temperature, the reaction temperature was kept at 50-55 ℃; after the ethylene oxide was added dropwise, continue to keep warm for 5h; Then vacuumize until the vacuum degree in the glass reactor is 30...

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Abstract

The invention provides a preparation method of a reactive acrylate crosslinking agent. The preparation method comprises the following steps: adding acid anhydride, an acrylate compound and a first polymerization inhibitor into a reaction vessel, mixing, reacting at 80-120 DEG C to obtain an intermediate product; adding a catalyst and a second polymerization inhibitor into the intermediate product;heating to a reaction temperature, dropwise adding an epoxy monomer, carrying out a reaction at 30-80 DEG C, continuously carrying out a curing reaction for 1-5 h after the epoxy monomer is completely added, cooling to a temperature of 30-50 DEG C, degassing, removing the unreacted epoxy monomer, and discharging to obtain a reaction type acrylate crosslinking agent. Compared with an existing acrylate crosslinking agent, the provided acrylate crosslinking agent has the advantages that the viscosity and the acid value are obviously reduced, and moreover, the preparation process is simple and easy to operate.

Description

technical field [0001] The invention relates to the related technical field of crosslinking agents containing benzene rings, acrylate groups and alkoxy group structures, in particular to a preparation method of reactive acrylate crosslinking agents. Background technique [0002] Acrylate cross-linking agents are widely used in the field of polymer synthesis, and are suitable for various polymerization methods, such as solution polymerization, emulsion polymerization, and suspension polymerization, to prepare polymers with cross-linked structures, especially reactive acrylate cross-linking The agent has a high photocuring rate, excellent aging resistance and water resistance, and has a wide range of applications. However, this type of reactive acrylate crosslinking agent uses a relatively high-viscosity epoxy resin in the preparation process, which has disadvantages such as high viscosity and high acid value. The invention improves the synthesis process of acrylate, and prep...

Claims

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Application Information

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IPC IPC(8): C08G65/26C07C67/08C07C69/80C07C67/26
CPCC08G65/2615C07C67/08C07C67/26C07C69/80
Inventor 万庆梅王马济世余渊荣高雷刘志湘
Owner ZHEJIANG HUANGMA NEW MATERIALS TECH CO LTD
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