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Flame-retardant bismaleimide resin and preparation method thereof

A bismaleimide and resin technology, applied in the field of biomass-based phosphoric ester flame retardant modified bismaleimide resin, flame retardant bismaleimide resin and its preparation, can solve the problem of High volatility, unsatisfactory compatibility, no technical solutions reported in the literature, etc., to achieve excellent flame retardant performance, easy industrial production, and low cost effects

Active Publication Date: 2017-03-22
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Phosphate esters are mostly viscous liquids, and they have the disadvantages of high volatility and unsatisfactory compatibility when added to resins as additive flame retardants.
So far, the technical scheme of modifying BMI based on biomass phosphate flame retardant has not been reported in the literature

Method used

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  • Flame-retardant bismaleimide resin and preparation method thereof
  • Flame-retardant bismaleimide resin and preparation method thereof
  • Flame-retardant bismaleimide resin and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0029] 1) Preparation of biomass-based phosphate esters

[0030] See attached figure 1 , it is the synthesis reaction formula of the phosphate ester based on biomass in the present invention, and the reaction is a phosphorylation reaction; in this embodiment, the specific method is: at 1±0.5°C, mix 36.0g sodium hydroxide with 10mL water Mix to obtain paste A, under stirring condition, add eugenol (147.8g) in dichloromethane (300mL) solution dropwise to paste A to prepare eugenol sodium suspension B. Then, at 0°C, a solution of phosphorus oxychloride (46.0 g) in dichloromethane (200 mL) was slowly added dropwise to the sodium eugenate suspension B, and the addition was completed after 2 hours, and the reaction was continued for 2 hours. Add 120g of 20% sodium hydroxide aqueous solution in reaction bottle after reaction finishes, to remove unreacted eugenol and the sodium chloride of generation. The organic layer was separated by extraction, washed with saturated brine until n...

Embodiment 2

[0038] 1) Preparation of biomass-based phosphate esters

[0039] Mix 42.0g sodium hydroxide with 13mL water at 1±0.5°C to obtain paste A, add eugenol (172.4g) in dichloromethane (400mL) dropwise to paste A under stirring condition Solution, prepared sodium eugenate suspending colloid B. Then, at 20°C, a solution of phosphorus oxychloride (46.0 g) in dichloromethane (250 mL) was slowly added dropwise to the sodium eugenate suspension B, and the addition was completed after 3 hours, and the reaction was continued for 3 hours. Add 200g of 10% sodium hydroxide aqueous solution in reaction bottle after reaction finishes, to remove unreacted eugenol and the sodium chloride of generation. The organic layer was separated by extraction, washed with saturated brine until neutral, and dried over anhydrous sodium sulfate. The solvent is rotary evaporated to obtain a light yellow liquid, which is the biomass-based phosphate flame retardant.

[0040] 2) Preparation of flame retardant bis...

Embodiment 3

[0043] 1) Preparation of biomass-based phosphate esters

[0044] Mix 48.0g of sodium hydroxide with 15mL of water in an ice-water bath at 0-5°C to obtain a paste A, and add eugenol (197.0g) in dichloromethane ( 500mL) solution to prepare sodium eugenate suspension B. Then, at 30°C, a solution of phosphorus oxychloride (46.0 g) in dichloromethane (300 mL) was slowly added dropwise to the sodium eugenate suspension B, and the dropwise addition was completed in 4 hours, and the reaction was continued for 4 hours. Add 300g of 5% sodium hydroxide aqueous solution in reaction bottle after reaction finishes, to remove unreacted eugenol and the sodium chloride of generation. The organic layer was separated by extraction, washed with saturated brine until neutral, and dried over anhydrous sodium sulfate. The solvent is rotary evaporated to obtain a light yellow liquid, which is the biomass-based phosphate flame retardant.

[0045] 2) Preparation of flame retardant bismaleimide resin...

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Abstract

The invention discloses flame-retardant bismaleimide resin and a preparation method thereof. The preparation method is characterized in that full-biomass eugenol is processed into eugenol salt suspensoid under the effect of strong base of alkali metal; a chloromethane solution of phosphorus oxychloride is dropped to the eugenol salt suspensoid to react, so as to obtain a biomass-based phosphate ester flame retardant; bismaleimide and 2,2'-diallyl bisphenol A are mixed with the obtained phosphate ester; the mixture is subjected to solidifying and after-treatment, so as to obtain the flame-retardant bismaleimide resin. Compared with petroleum-based bismaleimide resin, the flame-retardant bismaleimide resin prepared by the method is prepared through a biomass-based raw material, namely, eugenol; the raw material is green and reproducible; the flame-retardant bismaleimide resin remains the mechanical property and processing property of the petroleum-based eugenol resin and is outstanding in flame retardant property. The preparation method has the characteristics of being low in cost, and simple in production process; the preparation method has a wide application prospect in the fields such as the aerospace field, the electronic information field and the electrical insulation field.

Description

technical field [0001] The invention relates to a flame-retardant bismaleimide resin and a preparation method thereof, in particular to a biomass-based phosphate flame retardant-modified bismaleimide prepared by utilizing green renewable biomass resources. The invention relates to an amine resin, which belongs to the technical field of chemical engineering and polymer materials. Background technique [0002] Bismaleimide resin (BMI), as one of the representative high-performance thermosetting resins, has outstanding heat resistance, dielectric properties, heat and humidity resistance, and excellent mechanical properties, chemical resistance, radiation resistance, and Wear resistance and dimensional stability, so it has great application prospects in aerospace, electrical insulation, new energy and other fields. However, BMI has its own disadvantages such as high melting point, narrow processing window, and high brittleness of the cured product, which largely limits its appl...

Claims

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Application Information

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IPC IPC(8): C08G73/12
CPCC08G73/12
Inventor 顾嫒娟缪佳涛梁国正袁莉
Owner SUZHOU UNIV
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