Nano boron phosphate catalytic carbonization flame-retardant epoxy resin and preparation method thereof

Abstract

The invention discloses a nano boron phosphate catalytic carbonization flame-retardant epoxy resin and a preparation method thereof, belonging to the technical field of flame-retardant materials. The epoxy resin is mainly composed of an epoxy resin monomer, a curing agent and a catalytic carbonization flame retardant. The preparation method comprises the following steps: adding boric acid and phosphoric acid into a reactor, stirring at 110-120 DEG C for 25-35 minutes, and keeping the temperature for 4-5 hours to obtain a white solid 1; calcining the white solid 1 at 500-700 DEG C for 8-12 hours, washing for 3-5 times, and carrying out vacuum drying to obtain the solid acid nano boron phosphate; adding an ethanol dispersion solution of the solid acid nano boron phosphate into the epoxy resin monomer, uniformly dispersing by stirring, removing the ethanol in a vacuum, adding a curing agent, removing air, and curing to obtain the nano boron phosphate catalytic carbonization flame-retardant epoxy resin. The epoxy resin has the advantages of low flame retardant addition amount, high flame-retardant efficiency, low smoke generation amount and environment friendliness. The method has the advantages of simple preparation technique and low cost.

Description

technical field

[0001] The invention relates to a nano-boron phosphate catalyzed charcoal-forming flame-retardant epoxy resin and a preparation method thereof, and belongs to the technical field of flame-retardant materials. Background technique

[0002] Epoxy resin (EP) is an important class of thermosetting polymer materials, which are widely used in electronics, construction, aerospace, shipping and other fields due to their excellent mechanical properties, electrical properties and adhesive properties. base resin material. However, not only the flammability of EP limits its application (the oxygen index of pure epoxy resin is 26.8%, and the vertical burning test rating is UL94 without grade), but the traditional flame retardant tetrabromobisphenol A used for EP flame retardancy , has been included in the list of substances of concern due to the possible harm to the human body and the environment, and is undergoing risk assessment worldwide. Therefore, it is very necess...

Examples

Embodiment 1

[0037] A kind of nanometer boron phosphate is catalyzed into charcoal flame-retardant epoxy resin, taking described epoxy resin total mass (300g) as 100%, each component and its mass percentage are as follows:

[0038] E4484.5%,

[0039] m-PDA10.5%,

[0040] nano-BP 1.27 (the atomic molar ratio of boron and phosphorus is 1.27) 5.0%,

[0041] A preparation method of nano-boron phosphate catalyzed into charcoal and flame-retardant epoxy resin as described in this embodiment, the specific steps of the method are as follows:

[0042] (1) Add boric acid (1.25mol) and phosphoric acid (1mol) into a beaker, stir at 110°C for 25min, and keep warm for 4h to obtain white solid 1; put white solid 1 in a tube furnace, and adjust the heating rate to 5°C / min, heated up to 500°C, calcined for 8h, cooled with the furnace, washed 3 times, and dried in vacuum to obtain solid acid nano boron phosphate white powder with a particle size of about 40-60nm (such as figure 1 Shown), the actual ato...

Embodiment 2

[0048] A kind of nanometer boron phosphate is catalyzed into charcoal flame-retardant epoxy resin, taking described epoxy resin total mass (300g) as 100%, each component and its mass percentage are as follows:

[0049] E4484.5%,

[0050] m-PDA10.5%,

[0051] nano-BP 1.06 (the atomic molar ratio of boron and phosphorus is 1.06) 5.0%,

[0052] A preparation method of nano-boron phosphate catalyzed into charcoal and flame-retardant epoxy resin as described in this embodiment, the specific steps of the method are as follows:

[0053] (1) Add boric acid (1mol) and phosphoric acid (1mol) into a beaker, stir at 120°C for 35min, and keep warm for 5h to obtain a white solid 1; put the white solid 1 in a tube furnace, and adjust the heating rate to 8°C / min, heated up to 700°C, calcined for 12 hours, cooled with the furnace, washed 5 times, and dried in vacuum to obtain solid acid nano boron phosphate white powder with a particle size of about 60-80nm (such as figure 2 Shown), the ...

Embodiment 3

[0059] A kind of nanometer boron phosphate is catalyzed into charcoal flame-retardant epoxy resin, taking described epoxy resin total mass (300g) as 100%, each component and its mass percentage are as follows:

[0060] E4484.5%,

[0061] m-PDA10.5%,

[0062] nano-BP 0.84 (the atomic molar ratio of boron and phosphorus is 0.84) 5.0%,

[0063] A preparation method of nano-boron phosphate catalyzed into charcoal and flame-retardant epoxy resin as described in this embodiment, the specific steps of the method are as follows:

[0064] (1) Add boric acid (0.8mol) and phosphoric acid (1mol) into a beaker, stir at 115°C for 30min, and keep warm for 4.5h to obtain a white solid 1; put the white solid 1 in a tube furnace, and adjust the heating rate to 7 °C / min, heat up to 600 °C, calcined for 10 h, cooled with the furnace, washed 4 times, and dried in vacuum to obtain solid acid nano boron phosphate white powder with a particle size of about 40-80 nm (such as image 3 Shown), the a...

technical field

[0001] The invention relates to a nano-boron phosphate catalyzed charcoal-forming flame-retardant epoxy resin and a preparation method thereof, and belongs to the technical field of flame-retardant materials. Background technique

[0002] Epoxy resin (EP) is an important class of thermosetting polymer materials, which are widely used in electronics, construction, aerospace, shipping and other fields due to their excellent mechanical properties, electrical properties and adhesive properties. base resin material. However, not only the flammability of EP limits its application (the oxygen index of pure epoxy resin is 26.8%, and the vertical burning test rating is UL94 without grade), but the traditional flame retardant tetrabromobisphenol A used for EP flame retardancy , has been included in the list of substances of concern due to the possible harm to the human body and the environment, and is undergoing risk assessment worldwide. Therefore, it is very necess...

Examples

Embodiment 1

[0037] A kind of nanometer boron phosphate is catalyzed into charcoal flame-retardant epoxy resin, taking described epoxy resin total mass (300g) as 100%, each component and its mass percentage are as follows:

[0038] E4484.5%,

[0039] m-PDA10.5%,

[0040] nano-BP 1.27 (the atomic molar ratio of boron and phosphorus is 1.27) 5.0%,

[0041] A preparation method of nano-boron phosphate catalyzed into charcoal and flame-retardant epoxy resin as described in this embodiment, the specific steps of the method are as follows:

[0042] (1) Add boric acid (1.25mol) and phosphoric acid (1mol) into a beaker, stir at 110°C for 25min, and keep warm for 4h to obtain white solid 1; put white solid 1 in a tube furnace, and adjust the heating rate to 5°C / min, heated up to 500°C, calcined for 8h, cooled with the furnace, washed 3 times, and dried in vacuum to obtain solid acid nano boron phosphate white powder with a particle size of about 40-60nm (such as figure 1 Shown), the actual ato...

Embodiment 2

[0048] A kind of nanometer boron phosphate is catalyzed into charcoal flame-retardant epoxy resin, taking described epoxy resin total mass (300g) as 100%, each component and its mass percentage are as follows:

[0049] E4484.5%,

[0050] m-PDA10.5%,

[0051] nano-BP 1.06 (the atomic molar ratio of boron and phosphorus is 1.06) 5.0%,

[0052] A preparation method of nano-boron phosphate catalyzed into charcoal and flame-retardant epoxy resin as described in this embodiment, the specific steps of the method are as follows:

[0053] (1) Add boric acid (1mol) and phosphoric acid (1mol) into a beaker, stir at 120°C for 35min, and keep warm for 5h to obtain a white solid 1; put the white solid 1 in a tube furnace, and adjust the heating rate to 8°C / min, heated up to 700°C, calcined for 12 hours, cooled with the furnace, washed 5 times, and dried in vacuum to obtain solid acid nano boron phosphate white powder with a particle size of about 60-80nm (such as figure 2 Shown), the ...

Embodiment 3

[0059] A kind of nanometer boron phosphate is catalyzed into charcoal flame-retardant epoxy resin, taking described epoxy resin total mass (300g) as 100%, each component and its mass percentage are as follows:

[0060] E4484.5%,

[0061] m-PDA10.5%,

[0062] nano-BP 0.84 (the atomic molar ratio of boron and phosphorus is 0.84) 5.0%,

[0063] A preparation method of nano-boron phosphate catalyzed into charcoal and flame-retardant epoxy resin as described in this embodiment, the specific steps of the method are as follows:

[0064] (1) Add boric acid (0.8mol) and phosphoric acid (1mol) into a beaker, stir at 115°C for 30min, and keep warm for 4.5h to obtain a white solid 1; put the white solid 1 in a tube furnace, and adjust the heating rate to 7 °C / min, heat up to 600 °C, calcined for 10 h, cooled with the furnace, washed 4 times, and dried in vacuum to obtain solid acid nano boron phosphate white powder with a particle size of about 40-80 nm (such as image 3 Shown), the a...

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