Polyether amine benzoxazine prepolymer and method for preparing same

A benzoxazine and polyetheramine type technology, which is applied in the field of polyetheramine type benzoxazine prepolymer and its preparation, can solve the problem of difficult to use, brittle polybenzoxazine resin, not very high mechanical properties, etc. problem, to achieve the effect of low density, simple preparation process and excellent mechanical properties

Inactive Publication Date: 2015-12-02
CHINA UNIV OF GEOSCIENCES (WUHAN)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, polybenzoxazine resins also have some inherent disadvantages, such as most of the benzoxazine monomers are solid, and they are difficult to use as conveni

Method used

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  • Polyether amine benzoxazine prepolymer and method for preparing same
  • Polyether amine benzoxazine prepolymer and method for preparing same
  • Polyether amine benzoxazine prepolymer and method for preparing same

Examples

Experimental program
Comparison scheme
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Example Embodiment

[0021] Example 1

[0022] Preparation of polyetheramine benzoxazine prepolymer:

[0023] Add 5.04g (0.023mol) polyetheramine, 5.28g (0.023mol) bisphenol A, and 2.78g (0.092mol) paraformaldehyde into a 250mL three-necked flask equipped with a condenser, magnetic stirring, and thermometer. , The molar ratio of phenolic hydroxyl and amino functional groups is 2:1:1, then add 51mL of toluene / ethanol mixed solvent (toluene to ethanol volume ratio 2:1), mix well and heat to 80℃ to react for 9h. After the reaction, it will react. Pour the solution into 100mL methanol solution (concentration 50wt%) for precipitation to obtain a milky white suspension, stand for 12h, remove the supernatant to obtain a white precipitate, vacuum dry the white precipitate at 50℃ for 8h, and finally grind the dried product The brown-yellow powder obtained is the polyetheramine benzoxazine prepolymer.

[0024] The molecular structural formula of polyetheramine used in this embodiment is:

[0025]

[0026] Such as...

Example Embodiment

[0028] Example 2

[0029] Preparation of polyetheramine benzoxazine prepolymer:

[0030] Add 8.40g (0.023mol) polyetheramine, 5.28g (0.023mol) bisphenol A, 2.78g (0.092mol) formaldehyde into a three-necked flask equipped with condenser, magnetic stirring, thermometer, aldehyde group, phenolic hydroxyl group and The molar ratio of the amine functional group is 2:1:1, and then 51mL of chloroform is added as a solvent, and the mixture is evenly mixed and heated to 80°C for 10 hours. After the reaction is completed, the reaction solution is poured into 100mL of methanol solution (concentration 60wt%) for precipitation. Obtain a milky white suspension, stand for 24h, remove the supernatant to obtain a white precipitate, dry the white precipitate in vacuum at 60°C for 6h, and finally grind the dried product to obtain a brown-yellow powder, which is a polyetheramine benzoxone Oxazine prepolymer.

[0031] The molecular structural formula of polyetheramine used in this embodiment is:

[0032...

Example Embodiment

[0033] Example 3

[0034] Preparation of polyetheramine benzoxazine prepolymer:

[0035] Add 9.71g (0.023mol) polyetheramine, 5.28g (0.023mol) bisphenol A, 3.34g (0.11mol) formaldehyde into a three-necked flask equipped with condenser, magnetic stirring, thermometer, aldehyde group, phenolic hydroxyl group and The molar ratio of amine functional groups is 2.4:1:1, then add 51mL dimethylformamide as solvent, mix well and heat to 110℃ for 6h, after the reaction, pour the reaction solution into 100mL methanol solution (concentration 70wt%) Precipitate to obtain a milky white suspension, stand for 12h, remove the supernatant to obtain a white precipitate, dry the white precipitate in vacuum at 50℃ for 8h, and finally grind the dried product to obtain a brown-yellow powder, which is polyetheramine benzene And oxazine prepolymer.

[0036] The molecular structural formula of polyetheramine used in this embodiment is:

[0037]

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Abstract

The invention relates to a polyether amine benzoxazine prepolymer and a method for preparing the same. The method includes adding aldehyde compounds, bisphenol A and polyether amine compounds into a reaction container; adding organic solvents into the reaction container to dissolve the aldehyde compounds, the bisphenol A and the polyether amine compounds; enabling the aldehyde compounds, the bisphenol A and the polyether amine compounds to react to one another at the temperature of 80-110 DEG C for 6-10h to obtain reaction liquid; pouring the reaction liquid into methanol liquor after reaction is completed and precipitating the reaction liquid to obtain milk white suspension; allowing the milk white suspension to stand still, then removing supernatant to obtain white precipitate; drying the white precipitate and then grinding the white precipitate to obtain the polyether amine benzoxazine prepolymer. A molar ratio of aldehyde groups in the aldehyde compounds to phenolic hydroxyl in the bisphenol A to amino in the polyether amine compounds is 2-2.4:1-1.2:1-1.2. The polyether amine benzoxazine prepolymer and the method have the advantages that polyether amine benzoxazine resin ultimately obtained from the prepolymer by means of curing is excellent in heat resistance, mechanical property and dielectric property, and accordingly the polyether amine benzoxazine prepolymer can be widely applied to composite materials for copper-clad plates, laminated plates and the like.

Description

technical field [0001] The invention relates to the technical field of organic polymer materials, in particular to a polyetheramine type benzoxazine prepolymer and a preparation method thereof. Background technique [0002] Benzoxazines are six-membered heterocyclic compounds synthesized from phenolic compounds, amine compounds and aldehydes by Mannich reaction. Polybenzoxazine materials are a new class of thermosetting resins developed on the basis of traditional phenolic resins. While maintaining the excellent thermal properties, flame retardancy and electrical insulation of traditional phenolic resins, they overcome the traditional Phenolic resin has the disadvantage of releasing small molecules during processing and curing. The resulting product has low porosity and close to zero shrinkage in volume. The material has better high temperature thermal stability, flame retardancy, mechanical properties and chemical stability, etc., and absorbs water. Low resistance and no n...

Claims

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Application Information

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IPC IPC(8): C08G73/06C07D265/16
Inventor 曾鸣许清强徐庆玉冯子健
Owner CHINA UNIV OF GEOSCIENCES (WUHAN)
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