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Benzoxazine intrinsic flame-retardant resin and preparation method thereof

A benzoxazine and intrinsic flame retardant technology, applied in the field of materials, can solve the problems of unknown flame retardant properties of resins, unreliable experimental results, etc., and achieve improved glass transition temperature and thermal stability, low limiting oxygen Index, the effect of saving oil resources

Pending Publication Date: 2020-06-05
淮北绿洲新材料有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, Zhang did not conduct a vertical burning test of benzoxazine resin in the paper, and the actual flame retardancy of the prepared resin is unknown.
However, Lin did not use the standard vertical burning test method in the paper, that is, two 10-second burning tests, but used two 3-second burning tests. Although the results showed that the resin was V-0 grade, because the standard method was not used to test results are not credible

Method used

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  • Benzoxazine intrinsic flame-retardant resin and preparation method thereof
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  • Benzoxazine intrinsic flame-retardant resin and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0043] Preparation of deoxybenzoin bisphenol:

[0044] Add deoxy-p-anizoin and pyridinium hydrochloride into the reaction vessel, wherein the molar ratio of deoxy-p-anizoin to pyridinium hydrochloride is 1:4, react at 200°C for 5 hours, and pour the reaction solution into glacial acetic acid after the reaction Recrystallize in an aqueous solution to obtain white crystals, and obtain deoxybenzoin bisphenol powder after drying.

[0045] Such as figure 1 Shown is the infrared spectrogram of the deoxybenzoin bisphenol prepared in this embodiment, 3453, 3344cm -1 Represents the characteristic absorption peak of phenol-OH, 1666cm -1 Represents the characteristic absorption peak of C=O, 3026cm -1 The position is the stretching vibration peak of C-H on the benzene ring, 2895cm -1 at -CH 2 stretching vibration peak. To sum up, it shows that the synthesized product of this example is deoxybenzoin bisphenol, and its molecular structure is shown in formula 3.

Embodiment 2

[0047] Preparation of intrinsic flame retardant benzoxazine monomer:

[0048] 5.70g (0.025mol) deoxybenzoin bisphenol, 4.85g (0.05mol) furfurylamine, 13.50g (0.45mol) paraformaldehyde prepared in Example 1 are added into the condensing tube, magnetic stirring, thermometer In a 250mL three-necked flask, the molar ratio of phenolic hydroxyl group, amino group and aldehyde functional group is 1:1:9, then add 75mL tetrahydrofuran solvent, mix well and heat to 65°C for 130h, after the reaction, pour the reaction solution into 100mL methanol Precipitate in the solution to obtain a milky white suspension, let it stand for 12 hours, remove the supernatant to obtain a brown precipitate, dry the brown precipitate at 60°C for 8 hours in vacuum, and finally grind the dried product to obtain a brown powder, which is intrinsic flame retardant type benzoxazine monomer.

[0049] Such as figure 2 Shown is the infrared spectrogram of the intrinsic flame retardant benzoxazine monomer prepared i...

Embodiment 3

[0051] Preparation of intrinsic flame retardant benzoxazine monomer:

[0052] 68.4g (0.3mol) deoxybenzoin bisphenol, 29.1g (0.3mol) furfurylamine, 36.0g (1.20mol) paraformaldehyde prepared in Example 1 are added to be equipped with condenser tube, magnetic sub-stirring, thermometer In a 250mL three-necked flask, the molar ratio of phenolic hydroxyl group, amino group and aldehyde functional group is 6:3:12, then add 75mL of toluene solvent, mix well, heat to 115°C for 8 hours, and pour the reaction solution into 100mL methanol after the reaction Precipitate in the solution to obtain a milky white suspension, let it stand for 12 hours, remove the supernatant to obtain a brown precipitate, dry the brown precipitate at 60°C for 8 hours in vacuum, and finally grind the dried product to obtain a brown powder, which is the intrinsic flame retardant type benzoxazine monomer.

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Abstract

The invention discloses benzoxazine intrinsic flame-retardant resin and a preparation method thereof, and the preparation method comprises the following steps: mixing deoxybenzoin bisphenol, furfurylamine and aldehyde compounds in an organic solvent, carrying out a reaction at 65-115 DEG C for 8-130 hours, and purifying a reaction product to obtain a benzoxazine monomer; and carrying out curing reaction on the obtained benzoxazine monomer at 80-280 DEG C for 1-48 hours to obtain the benzoxazine resin. Compared with the prior art, the intrinsic flame-retardant benzoxazine resin prepared by thepreparation method disclosed by the invention has a remarkably different chemical structure. The halogen-free flame-retardant thermoplastic elastomer has the advantages of higher flame retardancy, higher crosslinking density, higher glass-transition temperature (310-380 DEG C), higher carbon residue rate (45-62%), lower limit oxygen index (33.5-42.5) and lower heat release capacity, and the flameretardancy can reach Grade V-0 under standard tests.

Description

technical field [0001] The invention belongs to the technical field of materials, and in particular relates to an intrinsic flame-retardant benzoxazine monomer, a polymer and a preparation method thereof. Background technique [0002] Since entering the 21st century, protecting the environment, protecting nature, and protecting human health have become issues that human beings must face and improve. Polymer materials are widely used, but there is a fatal shortcoming that it is easy to decompose at high temperature, and it will continue to burn under the flame. Although halogen-based and phosphorus-based flame retardants can improve the flame retardancy of polymer materials, they will have adverse effects on the environment and human health. Therefore, the current polymer materials are developing in the direction of halogen-free, phosphorus-free, and intrinsically flame-retardant. Notably, intrinsically flame-retardant polymers do not require any kind of additives, enabling...

Claims

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Application Information

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IPC IPC(8): C08G73/02C07D413/14
CPCC08G73/0273C07D413/14
Inventor 曾鸣朱万林
Owner 淮北绿洲新材料有限责任公司
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