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Halogen-free high-efficiency flame retardant, flame-retardant epoxy resin and preparation method thereof

A technology of epoxy resin and solid epoxy resin, which is applied in the field of composite materials, can solve the problems of harsh reaction conditions of flame retardant epoxy resin, too high addition of flame retardant, poor heat resistance of flame retardant epoxy resin, etc. Achieve excellent transparency, good plasticization, good flame retardant effect

Active Publication Date: 2021-01-05
AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The addition method is generally modified by directly adding a halogen-free powder flame retardant to the epoxy resin structure. The flame retardant and the epoxy resin are physically mixed, which will increase the flame retardancy of the epoxy resin to a greater extent. The viscosity of the epoxy resin reduces the process performance of the resin, the amount of flame retardant added should not be too high, and the improvement of flame retardant performance is limited
The modified polymerization method is to carry out modified polymerization of epoxy resin and reactive phosphorus-containing compounds. The reaction conditions for the preparation of flame-retardant epoxy resins by this method are harsh, the processing is difficult, and the phosphorus-containing substances are generally at the modified addition end. Non-main chain, resulting in poor heat resistance of flame retardant epoxy resin

Method used

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  • Halogen-free high-efficiency flame retardant, flame-retardant epoxy resin and preparation method thereof
  • Halogen-free high-efficiency flame retardant, flame-retardant epoxy resin and preparation method thereof
  • Halogen-free high-efficiency flame retardant, flame-retardant epoxy resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034]Flame retardant preparation:

[0035]In a reactor with a gas outlet, add 372g of dimethyl methylphosphonate, and at the same time add 6g of sodium carbonate as the catalyst, turn on the stirring, and start to heat up. When the temperature reaches 120°C, start to add tris(2) phosphoric acid to the reactor. -Chloroethyl) ester 285g. As the dripping progresses, there will be reaction gas methyl chloride generated. The reaction gas is condensed from the gas outlet of the reactor through the condenser and then enters the refrigerated compression unit for recovery. After the dripping is completed, continue to slowly increase the temperature to 160°C Continue the reaction and wait for almost no gas to be discharged, indicating that the reaction is basically complete, and a halogen-free high-efficiency flame retardant is obtained.

[0036]Epoxy resin formula:

[0037]

[0038]The preparation process is as follows:

[0039]In the first step, a certain amount of low-viscosity epoxy resin, halogen-free...

Embodiment 2

[0044]Flame retardant preparation:

[0045]In a reactor with a gas outlet, add 372g of dimethyl methylphosphonate, and at the same time add 6g of sodium hydroxide as a catalyst, turn on the stirring, and start to heat up. When the temperature reaches 120°C, start to add tris(phosphate) to the reactor. 300g of 2-chloroethyl) ester, as the dripping progresses, there will be reaction gas methyl chloride generated. The reaction gas is condensed from the gas outlet of the reactor through the condenser and then enters the refrigerated compression unit for recovery. After the dripping is completed, the temperature is slowly increased to 160 Continuing the reaction at ℃, and when there is basically no gas discharged, it indicates that the reaction is basically complete and a halogen-free high-efficiency flame retardant is obtained.

[0046]Epoxy resin formula:

[0047]

[0048]The preparation process is as follows:

[0049]In the first step, a certain amount of low-viscosity epoxy resin, halogen-free high...

Embodiment 3

[0054]Flame retardant preparation:

[0055]In a reactor with a gas outlet, 372g of dimethyl methylphosphonate was added, and 6g of sodium ethoxide as a catalyst was added at the same time. The stirring was turned on and the temperature started to rise. When the temperature reached 120°C, the reactor was started to drip tris(2) phosphate. -Chloroethyl ester 300g, as the dripping progresses, there will be reaction gas methyl chloride generated, the reaction gas is condensed from the gas outlet of the reactor through the condenser and then enters the refrigerating compression unit for recovery, after dripping, continue to slowly increase the temperature to 160°C Continue the reaction and wait for almost no gas to be discharged, indicating that the reaction is basically complete, and a halogen-free high-efficiency flame retardant is obtained.

[0056]Epoxy resin formula:

[0057]

[0058]The preparation process is as follows:

[0059]In the first step, a certain amount of low-viscosity epoxy resin, ha...

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Abstract

The invention provides a halogen-free high-efficiency flame retardant, flame-retardant epoxy resin and a preparation method thereof. The halogen-free high-efficiency flame retardant is synthesized bythe following method: adding dimethyl methylphosphonate, tris (2-chloroethyl) phosphate and a catalyst into a reaction device, heating to 100-180 DEG C, reacting for 2-10 hours under a stirring condition, and finishing the reaction when no gas is generated in the reaction system, thereby obtaining the product. The flame-retardant epoxy resin adopting the halogen-free high-efficiency flame retardant comprises low-viscosity epoxy resin, solid epoxy resin, the halogen-free high-efficiency flame retardant, a toughening agent, a curing agent and an accelerant. The halogen-free high-efficiency flameretardant prepared by the invention is high in phosphorus content and large in molecular weight, and the flame-retardant epoxy resin using the halogen-free high-efficiency flame retardant is good inflame-retardant effect and not easy to separate out.

Description

Technical field[0001]The invention relates to a preparation method of a halogen-free high-efficiency flame retardant, and also relates to a flame-retardant epoxy resin using the halogen-free high-efficiency flame retardant and a preparation method thereof, belonging to the technical field of composite materials.Background technique[0002]Epoxy resins generally use phenolic compounds to react with epichlorohydrin to obtain a resin whose end groups are epoxy groups. With the development of the electronic and electrical industry, epoxy resin has been widely used in electronic circuit substrates and power insulation boards because of its good heat resistance, dimensional stability, modulus and rigidity, and excellent adhesion to metals.[0003]Due to fire protection requirements, electronic circuit substrates and power insulation boards have strict flame retardant requirements. The epoxy resin has the possibility of burning under high temperature ignition conditions. Traditional printed ci...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/5333C08L63/00C08L75/04C07F9/40
CPCC08K5/5333C08L63/00C08L75/04C07F9/4006C07F9/4075C08L2201/02C08L2201/22C08L2205/03C08L2205/025C08L2201/10
Inventor 董大为欧秋仁陈哲明周子群李阳
Owner AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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