Epoxy resin fire retardant and preparation method thereof, as well as epoxy resin composition prepared from fire retardant

A technology of epoxy resin and flame retardant, which is applied in the field of epoxy resin composition, epoxy resin flame retardant and its preparation, can solve problems such as environmental pollution, reduction of material mechanical properties, migration and precipitation of flame retardant, and achieve Solve environmental pollution problems, good synergies, good environmental effects

Active Publication Date: 2018-03-06
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Halogen flame retardants will produce a large amount of toxic gases when they burn, which seriously pollute the environment and have been phased out. The thermal stability, compatibility with polymer matrix, permeability resistance and The processing performance is poor. The addition of nano-flame retardants to polymers will significantly reduce the mechanical properties of materials. The intumescent synergistic flame retardants represented by phosphorus-nitrogen have little improvement in the LOI of materials due to the lack of effective carbon sources.
[0004] US5277887 uses ammonium orthophosphate and phosphorus pentoxide as raw materials to prepare water-insoluble chain ammonium polyphosphate (APP) as a flame retardant for epoxy resins. The strong acid produced by the combustion and decomposition of the flame retardant promotes the development of the flame-retardant substrate. Dehydration into carbon, but due to the lack of synergistic flame retardant effect of the flame retardant system, the improvement of the material LOI is small
[0005] EP3531500 proposes to coat APP with melamine formaldehyde resin to form a microcapsule structure, and the flame retardant effect reaches UL-94VO level. Since the purpose of microencapsulation is mainly to reduce the water solubility of the flame retardant, there is no gap between the flame retardant and the matrix resin. The combination of chemical bonds makes the flame retardant easy to migrate and precipitate in the resin, which affects the performance of the material
[0006] CN105778152A provides a nitrogen-containing compound (3-amino-1,2,4-triazole) to modify carbon nanotubes, and introduce a compound with a high content of flame-retardant element N on the surface of carbon nanotubes.

Method used

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  • Epoxy resin fire retardant and preparation method thereof, as well as epoxy resin composition prepared from fire retardant
  • Epoxy resin fire retardant and preparation method thereof, as well as epoxy resin composition prepared from fire retardant
  • Epoxy resin fire retardant and preparation method thereof, as well as epoxy resin composition prepared from fire retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0082] (1) Preparation of flame retardant

[0083] ①Add 2g of single-walled carbon nanotubes to an Erlenmeyer flask filled with 45ml of mixed acid of 98wt% concentrated sulfuric acid and 68wt% concentrated nitric acid (volume ratio 1:3), ultrasonicate at 50°C for 3 hours, and then wash repeatedly with deionized water , drying in a vacuum oven at 80°C for 12h to constant weight to obtain acidified carbon nanotubes;

[0084] ② React the acidified carbon nanotubes obtained in (1) with a molar ratio of 1:5 and phosphorus trichloride at 125°C for 3 hours to obtain phosphite-modified carbon nanotubes.

[0085] ③ Mix 100 g of phosphite-modified carbon nanotubes obtained in (2) with 0.3 g of aluminum trichloride evenly, raise the temperature to 150 ° C, react for 5 h, and collect fractions with an absolute pressure of 0.1 MPa and a temperature of 177 ° C.

[0086] ④ Mix the distillate obtained in (3) with melamine at a molar ratio of 1:2.6, and react at 30°C for 4 hours; to obtain th...

Embodiment 2

[0097] (1) Preparation of flame retardant

[0098] ①Add 2g of single-walled carbon nanotubes to an Erlenmeyer flask filled with 45ml of mixed acid of 98wt% concentrated sulfuric acid and 68wt% concentrated nitric acid (volume ratio 1:2.5), ultrasonicate at 40°C for 3 hours, and then wash repeatedly with deionized water , dried in a vacuum oven at 85°C for 10h to constant weight to obtain acidified carbon nanotubes;

[0099] ② React the acidified carbon nanotubes obtained in (1) with a molar ratio of 1:3 and phosphorus trichloride at 140°C for 3.5 hours to obtain phosphite-modified carbon nanotubes.

[0100] ③ Mix 100 g of phosphite-modified carbon nanotubes obtained in (2) with 0.5 g of aluminum trichloride evenly, raise the temperature to 205° C., react for 5 hours, and collect fractions with an absolute pressure of 0.09 MPa and a temperature of 175° C.

[0101] ④ Mix the fraction obtained in (3) with o-phenylenediamine at a molar ratio of 1:3, and react at 35°C for 4 hours;...

Embodiment 3

[0112] (1) Preparation of flame retardant

[0113] ①Add 2g of single-walled carbon nanotubes to an Erlenmeyer flask containing 45ml of mixed acid of 98wt% concentrated sulfuric acid and 68wt% concentrated nitric acid (volume ratio 0.9:2.5), ultrasonicate at 70°C for 3 hours, and then wash repeatedly with deionized water , dried in a vacuum oven at 85°C for 10h to constant weight to obtain acidified carbon nanotubes;

[0114] ② React the acidified carbon nanotubes obtained in (1) with a molar ratio of 1.5:9.5 and phosphorus trichloride at 125° C. for 3.5 hours to obtain phosphite-modified carbon nanotubes.

[0115] ③ Mix 100 g of phosphite-modified carbon nanotubes obtained in (2) with 0.3 g of magnesium chloride, heat up to 150° C., react for 12 hours, and collect fractions with an absolute pressure of 0.09 MPa and a temperature of 175° C.

[0116] ④ Mix the fraction obtained in (3) with m-phenylenediamine in a molar ratio of 0.8:3, and react at 30°C for 5 hours; to obtain th...

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Abstract

The invention discloses an epoxy resin fire retardant and a preparation method thereof, as well as an epoxy resin composition prepared from the fire retardant. The fire retardant structurally comprises CNT (carbon nano tube)-nitrogen-phosphorus which is combined by chemical bonds. Not only can the fire retardant in a process of being heated and decomposing generate a large number of wormlike expansion carbon layers which are inlaid with one other so as to reduce thermal conductivity, but also can release phosphorus-containing strong acid and nitrogen-containing inert gas which can be respectively used for promoting an anti-flamed base material to dehydrate into carbon and reducing oxygen concentration. By a chemical reaction method, the fire retardant can be introduced into an epoxy cross-linking structure, because of the existence of the strong-polar chemical bonds, the fire retardant is prevented from migrating to the surface of a material, the epoxy resin composition is suitable forelectric and electrical engineering fields, the service life of the material is prolonged, and the safety of the material is improved.

Description

technical field [0001] The invention belongs to the field of epoxy resin, and in particular relates to an epoxy resin flame retardant, a preparation method thereof, and an epoxy resin composition prepared by using the flame retardant. Background technique [0002] Epoxy resin has excellent mechanical properties, electrical insulation, chemical corrosion resistance, heat resistance and adhesiveness after curing, and is widely used in many fields such as the automobile industry, electronics and electricity. Since epoxy resin is mainly composed of C, H, O and other elements, it has high flammability and continues to burn after leaving the fire, which is easy to cause fire. This shortcoming makes epoxy resin composite materials a great safety hazard. [0003] The limiting oxygen index (LOI) of unmodified epoxy resin is only about 19%. It can continue to burn in the air and belongs to flammable products. The flame retardancy of epoxy resin has become the focus of its application....

Claims

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Application Information

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IPC IPC(8): C08L63/00C08K7/24C08K9/02C08K9/04
CPCC08K7/24C08K9/02C08K9/04C08K2201/011C08L63/00
Inventor 周萌刘赵兴杜秀才冯百旋王慧骁初长坤曹善健
Owner WANHUA CHEM GRP CO LTD
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