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Epoxy resin reaction-type microcapsule fire retardant and preparation method thereof

A technology of epoxy resin and flame retardant, which is applied in the field of epoxy resin reactive microcapsule flame retardant and its preparation, which can solve the problems of adverse effects on physical and mechanical properties of materials, insignificant matrix compatibility, etc., and achieve improved stability Sexuality and physical and mechanical properties, improve performance and use stability, improve the effect of surface polarity

Inactive Publication Date: 2013-08-07
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the problems of dispersibility and compatibility in the process of adding flame retardants, these microcapsule flame retardants have improved dispersibility, but the compatibility with the matrix has not been significantly improved, and the physical and mechanical properties of the material have not been significantly improved. performance is adversely affected

Method used

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  • Epoxy resin reaction-type microcapsule fire retardant and preparation method thereof
  • Epoxy resin reaction-type microcapsule fire retardant and preparation method thereof
  • Epoxy resin reaction-type microcapsule fire retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] In a reactor equipped with a stirring and condensing device, disperse 20g of ammonium polyphosphate (Type II, Hangzhou Jieersi Flame Retardant Chemical Co., Ltd., the same below) in 80ml of absolute ethanol to obtain a mixed solution, and weigh 0.65g of iso Triglycidyl cyanurate (epoxy value 0.97, Shanghai Fangruida Chemical Co., Ltd., epoxy group content 6.31×10 -3 mol) was dissolved in 10ml chloroform to obtain triglycidyl isocyanurate solution, and 3.90g epoxy resin (E-44) (epoxy value 0.44, Jiangsu Wuxi Resin Factory, epoxy group content was 0.017mol) was dissolved The epoxy resin solution was obtained in 20ml of absolute ethanol, and when the mixture was heated to 50°C, these two solutions were added to the reaction kettle in turn, kept stirring at 50°C for 30min, and then heated to 65°C, at 2 drops / s Add the curing agent solution obtained by dissolving 2.37g of modified alicyclic amine curing agent 1618 (the equivalent of active hydrogen is 113, Guangdong Xiubo Ch...

Embodiment 2

[0032] In a reactor with a stirring and condensing device, disperse 20g ammonium polyphosphate in 40ml absolute ethanol to obtain a mixed solution, weigh 0.60g triglycidyl isocyanurate (manufacturer is the same as Example 1, epoxy group The content is 5.82×10 -3mol), it was dissolved in 5ml of chloroform to obtain a triglycidyl isocyanurate solution, when the mixture was heated to 30°C, the triglycidyl isocyanurate solution was added to the reaction kettle, and the mixture was stirred and reacted at 30°C for 10 minutes. Then be warming up to 40 DEG C, drop 0.41g modified alicyclic amine curing agent 1618 (manufacturer is the same as embodiment 1, active hydrogen content is 3.63 * 10 -3 mol) was dissolved in 10ml of absolute ethanol to obtain a solidifying agent solution, kept at 40°C for 2 hours, then heated to 78°C, kept for 12 hours, cooled to room temperature, filtered with suction, and washed with distilled water and absolute ethanol respectively. ℃ vacuum drying for 8 ho...

Embodiment 3

[0034] In a reactor with a stirring and condensing device, disperse 20g ammonium polyphosphate in 60ml dehydrated alcohol to obtain a mixed solution, weigh 0.62g triglycidyl isocyanurate (manufacturer is the same as Example 1, epoxy group The content is 6.01×10 -3 mol), it is dissolved in 10ml chloroform to obtain triglycidyl isocyanurate solution, and takes by weighing 3.72g epoxy resin (E-44) (manufacturer is the same as embodiment 1, epoxy group content is 0.016mol) dissolving Obtain an epoxy resin solution in 20ml of absolute ethanol, and when the mixed solution is heated to 40°C, these two solutions are added to the reaction kettle in turn, kept stirring at 40°C for 20min, and then heated to 50°C, with 2 drops / Add dropwise the curing agent solution obtained by dissolving 2.32g of modified alicyclic amine curing agent 1618 (the manufacturer is the same as in Example 1, with an active hydrogen content of 0.021mol) in 20ml of absolute ethanol at a speed of s, and keep the r...

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Abstract

The invention belongs to the field of polymer flame retardation and discloses an epoxy resin reaction-type microcapsule fire retardant and a preparation method thereof. The epoxy resin reaction-type microcapsule fire retardant is characterized in that at least one phosphorus-containing fire retardant is utilized as a capsule core; a product of a reaction of at least one curing agent, an epoxy resin and triglycidyl isocyanurate is utilized as a capsule material; a mass ratio of the capsule material to the capsule core is (0.05 to 0.4): 1; and a mass ratio of the epoxy resin to the triglycidyl isocyanurate is (0 to 6): 1. The preparation method provided by the invention comprises the following steps of dispersing the at least one phosphorus-containing fire retardant in at least one solvent,heating, adding a triglycidyl isocyanurate solution and an epoxy resin solution into the heated solution, stirring for a reaction for 10 to 30 minutes, dropwisely adding a curing agent solution into the reaction system, carrying out a reaction process for 1 to 2 hours, heating to a temperature of 70 to 78 DEG C, carrying out a reaction process for 2 to 12 hours, cooling, filtering, washing and drying to obtain the epoxy resin reaction-type microcapsule fire retardant. The epoxy resin reaction-type microcapsule fire retardant has uniform granularity, good liquidity, low water-solubility and good polymer compatibility. Through utilization of the epoxy resin reaction-type microcapsule fire retardant, good flame resistance, good water tolerance and good mechanical properties are obtained.

Description

technical field [0001] The invention belongs to the field of flame retardant polymers, in particular to an epoxy resin reactive microcapsule flame retardant and a preparation method thereof. Background technique [0002] Epoxy resin is widely used in various industrial fields due to its excellent performance, but its application in areas with high flame retardancy requirements is greatly limited due to its flammability. With the development of flame retardant technology and people's emphasis on environmental protection and personal safety, epoxy resin flame retardant is undergoing a transformation from a halogen-based flame retardant system to a halogen-free flame retardant system. Among them, phosphorus-based flame retardants have become a research hotspot to replace halogen-based flame retardants, and have gradually moved from the laboratory to the market. Phosphorus-based flame retardants include inorganic phosphorus-based and organic phosphorus-based flame retardants, a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K9/10C08K3/32C08L63/00C08K13/06
Inventor 沈敏敏张延奎吴昆魏续瑞
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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