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A kind of bio-based phosphaphenanthrene flame retardant curing agent and preparation method thereof

A phosphaphenanthrene, bio-based technology, applied in the field of bio-based phosphaphenanthrene flame retardant curing agent, can solve the problem of low yield and achieve the effects of good thermal stability and excellent flame retardant performance

Active Publication Date: 2021-10-19
BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, its yield is not high, reaching a maximum of 68.8%.

Method used

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  • A kind of bio-based phosphaphenanthrene flame retardant curing agent and preparation method thereof
  • A kind of bio-based phosphaphenanthrene flame retardant curing agent and preparation method thereof
  • A kind of bio-based phosphaphenanthrene flame retardant curing agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Sequentially weigh 10.8g (0.1mol) of p-phenylenediamine and 19.2g (0.2mol) of furfural, add 500ml of propanol to a 1000ml three-necked flask, and then add the weighed raw materials in turn. Introduce nitrogen into the three-necked flask for 5 minutes, and stir After completely dissolving, after reacting for 7 hours under the condition of 40°C oil bath, a Schiff base type intermediate was obtained; adding 43.2g (0.2mol) of DOPO, heating up to 70°C under the condition of oil bath, reflux reaction for 10h, after the reaction, The solvent was removed to dryness. Finally, the bio-based phosphaphenanthrene flame retardant curing agent FPD was dried in a vacuum oven at 80 °C, and the yield was 98.4%.

Embodiment 2

[0025] Sequentially weigh 10.8g (0.1mol) of p-phenylenediamine and 28.8g (0.3mol) of furfural, add 500ml of ethanol to a 1000ml three-necked flask, then add the weighed raw materials in turn, inject helium gas into the three-necked flask for 5 minutes, and stir After completely dissolving and reacting at 25°C for 8 hours, a Schiff base-type intermediate was obtained; add 64.8g (0.3mol) of DOPO, heat up to 75°C under oil bath conditions, and reflux for 12h. After the reaction, the solvent Remove dryness. Finally, the bio-based phosphaphenanthrene flame retardant curing agent FPD was dried in a vacuum oven at 100 °C, and the yield was 99.5%.

Embodiment 3

[0027] Sequentially weigh 10.8g (0.1mol) of p-phenylenediamine and 24.0g (0.25mol) of furfural, add 500ml of tetrahydrofuran into a 1000ml three-necked flask, add the weighed raw materials in turn, pass argon gas into the three-necked flask for 5 minutes, and stir After completely dissolving, react at 45°C for 9h to obtain a Schiff base-type intermediate; add 49.7g (0.23mol) of DOPO, heat the oil bath to 60°C, reflux for 14h, and remove the solvent after the reaction dry. Finally, the bio-based phosphaphenanthrene flame retardant curing agent FPD was dried in a vacuum oven at 70 °C, and the yield was 99.2%.

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PUM

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Abstract

The invention discloses a bio-based phosphaphenanthrene flame-retardant curing agent (FPD for short) and a preparation method thereof. The preparation method of the flame-retardant curing agent is as follows: Amino group undergoes condensation reaction to obtain Schiff base intermediate (F‑Schiff base); The H bond and the C=N in the Schiff base intermediate F-Schiff base undergo an addition reaction to prepare a bio-based phosphaphenanthrene flame retardant curing agent FPD. The flame retardant curing agent has the following advantages: the raw material of FPD comes from natural Biomass materials are non-toxic, non-polluting, green and environmentally friendly, and have the effects of flame retardancy and curing. They do not contain halogens, contain acid sources, carbon sources, and gas sources. According to the thermogravimetric test, in a nitrogen atmosphere, the mass retention rate of FPD at 700°C is 40.5%, which can endow the epoxy resin material with excellent flame retardancy and good thermal stability, and the yield is as high as 98%.

Description

technical field [0001] The invention relates to a bio-based phosphaphenanthrene flame retardant curing agent, which is a phosphaphenanthrene flame retardant curing agent containing biomass raw materials prepared by a chemical synthesis method, and belongs to the technical field of preparing flame retardant materials by a chemical synthesis method. Background technique [0002] At present, with the wide application of polymer materials, people pay more attention to the flame retardancy of materials. In the field of flame retardants, halogenated flame retardants have high-efficiency flame-retardant properties, but they will release dioxin or dibenzofuran during their combustion. In order to prevent the release of such flame retardants when they function Toxic and harmful substances, the "Stockholmont Convention", the EU's ROHS directive and REACH regulations, and my country's "Waste Household Electrical Appliances and Electronic Products Pollution Prevention and Control Technol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6574C08G59/50
CPCC07F9/657172C08G59/504
Inventor 钱立军姚忠樱邱勇陈雅君许博
Owner BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY