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Preparation method of high-flame retardant vinyl resin

A vinyl resin, high flame retardant technology, applied in the field of preparation of high flame retardant vinyl resin, can solve the problems of failing to meet the flame retardant requirements, increasing the load of the stirring motor, easy gelation, etc. The effect of increasing the service life and simple operation steps

Inactive Publication Date: 2019-07-19
华砻树脂股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Existing production of high flame retardant vinyl resins usually uses epoxy resin, tetrabromobisphenol A, styrene and other small materials for polymerization reaction. Tetrabromobisphenol A is a derivative of bisphenol A and is a white powder. Used as an additive for plastic products, it is one of the commonly used brominated flame retardants. The content of tetrabromobisphenol A directly affects the flame retardancy of vinyl resins. However, due to the large molecular weight of tetrabromobisphenol A, the viscosity is high when it melts , if the amount added is too large, it will easily lead to an increase in the viscosity of the material in the reactor, and the increase in viscosity will lead to uneven stirring of the material in the reactor, uneven local heating and easy gelation, and the quality of the product cannot be guaranteed; due to too high viscosity, It will increase the load of the stirring motor and easily cause the motor to burn out, but if the increased tetrabromobisphenol A content is small, the produced vinyl ester resin will have poor flame retardancy and fail to meet the flame-retardant requirements. Therefore, it is necessary to find a A method that can solve the above problems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A preparation method of high flame-retardant vinyl resin includes the following steps:

[0021] (1) The first step reaction: add epoxy resin, tetrabromobisphenol A and the first catalyst to the reaction kettle, stir and mix and then heat up to a step reaction temperature of 125°C, keep the constant temperature reaction for 30 minutes to reach the epoxy equivalent value 400 g / equivalent, reaching the end point of the first step reaction;

[0022] (2) Second step reaction: Cool the system that completed the first step reaction in step (1) to below 130°C, add 800 parts of styrene and 0.5 part of polymerization inhibitor, stir evenly, and wait until the temperature drops to the second step reaction temperature At 90°C, add methacrylic acid and stir evenly. When the auto-exotherm of the entire reaction system is stable, add a second catalyst to maintain the two-step reaction temperature and reach the end of the second-step reaction. The end point of the second-step reaction is ac...

Embodiment 2

[0026] A preparation method of high flame-retardant vinyl resin includes the following steps:

[0027] (1) The first step reaction: add epoxy resin, tetrabromobisphenol A and the first catalyst into the reaction kettle, stir and mix and then heat up to a step reaction temperature of 165°C, keep the constant temperature for 60 minutes to reach the epoxy equivalent value 500 g / equivalent, reaching the end point of the first step reaction;

[0028] (2) Second step reaction: Cool the system that completed the first step reaction in step (1) to below 130°C, add 900 parts of styrene and 1 part of polymerization inhibitor, stir evenly, and wait until the temperature drops to the second step reaction temperature At 115°C, add methacrylic acid and stir evenly. When the auto-exotherm of the entire reaction system is stable, add a second catalyst to maintain the two-step reaction temperature and reach the end of the second-step reaction. The end point of the second-step reaction is acid value...

Embodiment 3

[0032] A preparation method of high flame-retardant vinyl resin includes the following steps:

[0033] (1) The first step reaction: add epoxy resin, tetrabromobisphenol A and the first catalyst into the reaction kettle, stir and mix and then heat up to a one-step reaction temperature of 125°C, keep the constant temperature for 45 minutes to reach the epoxy equivalent value 450 g / equivalent, reaching the end point of the first step reaction;

[0034] (2) Second step reaction: Cool the system that completed the first step reaction in step (1) to below 130°C, add 850 parts of styrene and 0.8 part of polymerization inhibitor, stir evenly, and wait until the temperature drops to the second step reaction temperature At 105°C, add methacrylic acid and stir evenly. When the auto-exotherm of the entire reaction system is stable, add a second catalyst to maintain the two-step reaction temperature and reach the end of the second-step reaction. The end point of the second-step reaction is acid...

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Abstract

The invention discloses a preparation method of high-flame retardant vinyl resin. The preparation method comprises the following steps: first-step reaction: adding epoxy resin, tetrabromobisphenol A and a catalyst into a reaction kettle, stirring, mixing, then heating to a one-step reaction temperature and reaching a one-step reaction endpoint after the constant temperature reaction is maintainedto a certain amount of epoxy equivalent value; second-step reaction: adding a proper amount of styrene, uniformly stirring, adding methacrylic acids when the temperature is reduced to a two-step reaction temperature, uniformly stirring, then adding a catalyst to maintain the two-step reaction temperature reaction to reach a two-step reaction endpoint after the self-release heat of a whole reactionsystem is stable; adjusting and diluting: adding a proper amount of styrene to dilute, uniformly stirring and then reducing to a room temperature to obtain a finished product, namely the high-flame retardant vinyl resin. The invention provides the preparation method of the vinyl resin, which has the benefits that under the premise of ensuring the product quality, the viscosity of a reaction material at the second stage is reduced, the load of a stirring motor is reduced, and the use time is prolonged.

Description

Technical field [0001] The invention relates to the technical field of polymer materials, in particular to a method for preparing a highly flame-retardant vinyl resin. Background technique [0002] Vinyl ester resin is a special unsaturated polyester resin with a vinyl group at the end of the molecule and an epoxy resin structure in the middle skeleton. It is usually prepared by the ring-opening esterification reaction of epoxy resin and unsaturated monobasic acid. , Has the characteristics of epoxy and unsaturated polyester two thermosetting resins; vinyl ester resin retains the basic segments of epoxy resin, and has the good process performance of unsaturated polyester resin, which can be cured under suitable conditions , Showing some special excellent properties, such as excellent mechanical properties, heat resistance and chemical resistance. [0003] Existing production of high flame retardant vinyl resins usually use epoxy resin, tetrabromobisphenol A, styrene and other smal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/14C08G59/17
CPCC08G59/1433C08G59/1438C08G59/1466
Inventor 黄向群李小林吴汛燎
Owner 华砻树脂股份有限公司
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