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Halogen-free flame-retardant rosin-based epoxy resin and preparation method thereof

A rosin-based epoxy resin, flame retardant technology, applied in the direction of organic chemistry, etc., can solve the problem that the flame retardant of heterocyclic epoxy cannot meet the demand, etc., and achieve high strength, strong anti-ultraviolet performance, and high flame retardancy. Effect

Pending Publication Date: 2021-02-09
HUNAN TUOCHUANG POLYMERIC NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

With the increasing requirements in the electronic field, low-halogen or halogen-free flame-retardant epoxy resin needs to gradually increase, and heterocyclic epoxy cannot meet the demand in flame retardancy

Method used

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  • Halogen-free flame-retardant rosin-based epoxy resin and preparation method thereof
  • Halogen-free flame-retardant rosin-based epoxy resin and preparation method thereof
  • Halogen-free flame-retardant rosin-based epoxy resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A preparation method of halogen-free flame-retardant rosin-based epoxy resin, comprising the following steps:

[0024] (1) Put 1200 parts of maleabietic alcohol, 1200 parts of xylene solvent and 1.2 parts of calcium chloride into the reaction kettle, heat and stir to dissolve and stir evenly, add phosphorus oxychloride at 50°C and mix evenly, heat to 80°C And heat preservation reaction 4 hours;

[0025] (2) cooling down to room temperature, adding 40 parts of sodium hydroxide for neutralization;

[0026] (3) The reactant obtained in step (2) was filtered and added to the reactor together with 2500 parts of epichlorohydrin, stirred and heated to 80° C., added with 280 parts of sodium hydroxide, and reacted for 6.5 hours;

[0027] (4) The obtained product is filtered, washed with hot water at 70-80°C for 4 times to remove the halogen ions, dried, heated and reduced pressure to remove the solvent, and the halogen-free flame-retardant rosin-based epoxy resin is obtained. ...

Embodiment 2

[0029] A preparation method of halogen-free flame-retardant rosin-based epoxy resin, comprising the following steps:

[0030] (1) Put 1200 parts of maleabietic alcohol, 1200 parts of xylene solvent and 1.2 parts of calcium chloride into the reaction kettle, heat and stir to dissolve and stir evenly, add phosphorus oxychloride at 50°C and mix evenly, heat to 80°C And heat preservation reaction 4 hours;

[0031] (2) cooling down to room temperature, adding 40 parts of sodium hydroxide for neutralization;

[0032] (3) The reactant obtained in step (2) was filtered and added to the reactor together with 2500 parts of epichlorohydrin, stirred and heated to 80° C., added 3 parts of tetramethylammonium chloride, and reacted for 6.5 hours;

[0033] (4) The obtained product is filtered, washed with hot water at 70-80°C for 4 times to remove the halogen ions, dried, heated and reduced pressure to remove the solvent, and the halogen-free flame-retardant rosin-based epoxy resin is obtain...

Embodiment 3

[0035] A preparation method of halogen-free flame-retardant rosin-based epoxy resin, comprising the following steps:

[0036] (1) Put 1200 parts of maleabietic alcohol, 1200 parts of xylene solvent and 1.2 parts of calcium chloride into the reaction kettle, heat and stir to dissolve and stir evenly, add phosphorus oxychloride at 50°C and mix evenly, heat to 80°C And heat preservation reaction 4 hours;

[0037] (2) cooling down to room temperature, adding 40 parts of sodium hydroxide for neutralization;

[0038] (3) The reactant obtained in step (2) is filtered and added to the reaction kettle together with 2500 parts of epichlorohydrin, stirred and heated to 80° C., added with 1 part of boron trifluoride etherate complex, and reacted for 6.5 hours;

[0039] (4) The obtained product is filtered, washed with hot water at 70-80°C for 4 times to remove the halogen ions, dried, heated and reduced pressure to remove the solvent, and the halogen-free flame-retardant rosin-based epox...

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Abstract

The invention discloses a preparation method of halogen-free flame-retardant rosin-based epoxy resin, which comprises the following steps: adding maleic rosin alcohol prepared by reduction, a solventand a catalyst into a reaction kettle, conducting heating, stirring, dissolving and uniform stirring, adding a phosphide into the reaction kettle, and carrying out phosphating catalytic reaction; conducting cooling to room temperature for neutralization after the reaction is finished; then, subjecting the obtained intermediate product, epoxy chloropropane and an epoxidation catalyst to a heating reaction; and filtering an obtained product, conducting washing with water to remove halogen ions, and conducting drying and heating, and removing the solvent under reduced pressure. According to the halogen-free flame-retardant rosin-based epoxy resin, phenanthrene cyclic phosphide structures and high epoxy functionality exist in molecules, and a cured product of the halogen-free flame-retardant rosin-based epoxy resin has high ultraviolet resistance, high strength, high flame retardance, high chemical resistance and high electrical properties. The product has high epoxy functionality, the cured product can provide very high crosslinking density and good flame retardancy, corrosive gas is not generated, the flame retardant effect is lasting, and the toxicity is low.

Description

technical field [0001] The invention relates to the technical field of flame-retardant epoxy resins, in particular to a halogen-free flame-retardant rosin-based epoxy resin and a preparation method thereof. Background technique [0002] At present, flame retardant epoxy resins on the market are basically high-bromine types. With the increasing requirements in the electronic field, low-halogen or halogen-free flame-retardant epoxy resins need to gradually increase, and heterocyclic epoxy cannot meet the demand in terms of flame retardancy. my country is rich in rosin resources and is a natural renewable resource. In order to give full play to the characteristics and advantages of rosin itself, epoxidized deep processing of rosin can not only enrich the variety of epoxy resins, but also prepare high-performance epoxy resins with special properties. The invention provides a halogen-free flame-retardant rosin-based epoxy resin and a preparation method thereof. Contents of the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/32C07D303/30C07D301/28
CPCC08G59/3218C07D303/30C07D301/28
Inventor 雷冠军
Owner HUNAN TUOCHUANG POLYMERIC NEW MATERIAL CO LTD