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Halogen-free flame-retardant epoxy curing agent and preparation method thereof

An epoxy curing agent, solid technology, applied in the field of halogen-free flame retardant epoxy curing agent and its preparation, can solve the problems of increasing the risk of epoxy resin use, reducing the flame retardant efficiency, secondary damage, etc., and achieving good resistance. The effect of combustion effect, less side reaction and moderate reaction temperature

Active Publication Date: 2017-08-11
深圳威科射频技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Epoxy resin has brought great convenience in both national defense and civilian fields, but epoxy resin also has certain disadvantages, such as being combustible, which increases the risk of using epoxy resin to a certain extent
In the modification process of epoxy resin, the use of additive flame retardant can significantly improve the flame retardancy coefficient of epoxy resin, but the additive flame retardant will lead to migration or escape over time, so that the flame retardant efficiency decrease very much
Among the previous additive flame retardants, halogen-containing flame retardants are widely used due to their convenient preparation and low price. However, halogen-based flame retardants will release harmful substances such as dioxins during combustion, causing secondary damage.

Method used

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  • Halogen-free flame-retardant epoxy curing agent and preparation method thereof
  • Halogen-free flame-retardant epoxy curing agent and preparation method thereof
  • Halogen-free flame-retardant epoxy curing agent and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0027] 1) Preparation of HPM

[0028] Get 49g of maleic anhydride and place it in a three-necked flask, add 20ml of acetone solution. Add the ice-water mixture in the magnetic sub-stirrer, after the maleic anhydride gradually dissolves, add 54.5g of para-aminophenol (addition process, control the amount and time interval each time in small amounts for several times). A yellow suspension was obtained as the reaction proceeded. Filter under reduced pressure and dry in an oven. The product from the previous step was placed in a three-necked flask, added into a mixed solvent of toluene and DMF, and 86 g of p-toluenesulfonic acid was added as a catalyst. Adjust the temperature of the magnetic stirrer to 110°C and continue the reaction for 8h to obtain a red solution. Connected to a vacuum suction filtration device, suction filtration at 130°C for 30 minutes, after removing part of the solvent, the product was placed in deionized water, and left to cool to obtain a large amount o...

Embodiment 2

[0040] Embodiment 2: Determination of curing process without adding accelerator

[0041] The epoxy resin that gets 100g gained is placed in the beaker, and the oil bath temperature setting is 80 ℃. After the epoxy resin viscosity is very small, add the modified product prepared by 35g example 1). Stir well, pour into the mold with oxygen index, and put it in the oven. Pre-cure at 110°C for 1 hour, and cure at 130°C for 1 hour. At this time, check the solidification of the casting solution. Under these conditions, the compound system is still liquid, and the curing effect is very poor.

Embodiment 3

[0042] Embodiment 3: Determination of oxygen index of cured product without adding accelerator

[0043] The epoxy resin that gets 100g gained is placed in the beaker, and the oil bath temperature setting is 80 ℃. After the epoxy resin viscosity is very small, add the modified product prepared by 35g example 1). Stir well, pour into the mold with oxygen index, and put it in the oven. Pre-cure at 130°C for 1 hour, cure at 160°C for 2 hours, and post-cure at 180°C for 1 hour. At this time, the solidification of the casting solution was detected, and the solidification was good. The casting body spline of epoxy resin was obtained by demoulding. The cured product sample prepared in step 4 was tested according to the national standard GB / T2406 through the XZT-100A limiting oxygen index meter. The measured LOI is 28.1, which belongs to the flame retardant material. It shows that epoxy can still be cured at higher temperature without adding accelerator, and the addition of accele...

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Abstract

The invention relates to a halogen-free flame-retardant epoxy curing agent and a preparation method thereof. The preparation method comprises the following steps that 1, heating reaction is conducted on HPM, p-aminobenzoic acid and paraformaldehyde in the molar ratio of 1 to 1 to 2, and benzoxazine with carboxyl and maleimide structures is obtained; 2, the nucleophilic addition property of P-H bonds of DOPO is utilized, DPOP and benzoxazine with carboxyl and maleimide structures which is obtained in the step 1 are added, wherein the molar ratio is 2:1, the epoxy resin curing agent with a bimolecular DOPO structure is synthesized and obtained by the heating reaction. Compared with existing products, the epoxy curing agent and the preparation process thereof have the advantages of being simple in curing process, mild in reaction temperature, excellent in flame-retardant effect, difficult in burning in air, high in production rate, simple to operate, low in raw material price and wide in source.

Description

technical field [0001] The invention relates to a halogen-free flame-retardant epoxy curing agent and a preparation method thereof. Background technique [0002] As an important thermosetting resin, epoxy resin is an amorphous viscous liquid, which can be made into coatings, composite materials, casting materials, adhesives, molding materials and injection molding materials. Epoxy resin is plastic under heating conditions, epoxy resin has no obvious melting point, it is easy to soften when heated, gradually melts and becomes sticky, insoluble in water, and will not harden itself, so epoxy resin alone is almost There is no practical application value, but only the insoluble and infusible polymer that reacts with the curing agent to form a three-dimensional network structure under appropriate conditions has application value. The use of the curing agent is to chemically react with the epoxy resin, and the epoxy resin gradually solidifies to form a network-like three-dimension...

Claims

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Application Information

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IPC IPC(8): C08G59/50
CPCC08G59/504C08G59/5046C08G59/506
Inventor 曾黎明熊仁卿
Owner 深圳威科射频技术有限公司
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