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Trifluoromethanesulfonic acid metal salt/benzoxazine resin composition and preparation method thereof

A trifluoromethanesulfonic acid and resin composition technology, applied in the field of trifluoromethanesulfonic acid metal salt/benzoxazine resin composition and its preparation, can solve the problems of loss of material performance, high curing temperature, high brittleness, etc. , to achieve the effect of improving heat resistance, reducing the curing peak temperature greatly, and adding less

Active Publication Date: 2019-07-30
NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, benzoxazine also has some defects: (1) high brittleness; (2) high curing temperature; (3) heat resistance needs to be further improved
At present, research at home and abroad is mainly focused on reducing the curing temperature, and the blending / copolymerization method is often accompanied by the loss of material properties

Method used

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  • Trifluoromethanesulfonic acid metal salt/benzoxazine resin composition and preparation method thereof
  • Trifluoromethanesulfonic acid metal salt/benzoxazine resin composition and preparation method thereof
  • Trifluoromethanesulfonic acid metal salt/benzoxazine resin composition and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment 1 Based on aluminum trifluoromethanesulfonate catalyzed as catalyst curing benzoxazine resin method

[0027] Aluminum trifluoromethanesulfonate and benzoxazine resin are mixed in a ratio of 40mmol / mol (the mass percentage content of aluminum trifluoromethanesulfonate is 3.96wt%), it is dissolved in toluene solvent, trifluoromethanesulfonic acid The mass percent concentration of aluminum and benzoxazine resin in the mixed solution is adjusted to be 50wt%. Stir at room temperature until completely dissolved, then dry in a vacuum oven at 80°C to constant weight, and grind the mixture in a mortar to make it evenly mixed. The homogeneously mixed samples were transferred to molds. Put the mold into a forced air drying oven, and use a stepwise heating program (120°C / 1h, 150°C / 1h, 180°C / 2h, 210°C / 1h) to cure to obtain benzoxazine resin (BOZ-Al).

Embodiment 2

[0028] Embodiment 2 is based on ytterbium trifluoromethanesulfonate and catalyzes the method for curing benzoxazine resins as a catalyst

[0029] Mix ytterbium trifluoromethanesulfonate and benzoxazine resin in a ratio of 50mmol / mol (the mass percent content of ytterbium trifluoromethanesulfonate is 6.31wt%), dissolve it in chloroform solvent, trifluoromethanesulfonic acid The mass percent concentration of aluminum and benzoxazine resin in the mixed solution is adjusted to be 60wt%. Stir at room temperature until completely dissolved, then dry in a vacuum oven at 50°C to constant weight, and grind the mixture in a mortar to make it evenly mixed. The homogeneously mixed samples were transferred to molds. Put the mold into a forced air drying oven, and use a stepwise temperature rise program (120°C / 1h, 150°C / 1h, 180°C / 2h, 210°C / 1h) to cure to obtain benzoxazine resin (BOZ-Yb).

Embodiment 3

[0030] Embodiment 3 is based on lanthanum trifluoromethanesulfonate and catalyzes the method for curing benzoxazine resin as a catalyst

[0031] Lanthanum trifluoromethanesulfonate is mixed with benzoxazine resin in a ratio of 30mmol / mol (the mass percentage content of lanthanum trifluoromethanesulfonate is 3.68wt%), it is dissolved in dioxane solvent, trifluoromethanesulfonate The mass percent concentration of aluminum methanesulfonate and benzoxazine resin in the mixed solution is adjusted to be 40wt%. Stir at room temperature until completely dissolved, then dry in a vacuum oven at 70°C to constant weight, and grind the mixture in a mortar to make it evenly mixed. The homogeneously mixed samples were transferred to molds. Put the mold into a forced air drying oven, and use a stepwise heating program (120°C / 1h, 150°C / 1h, 180°C / 2h, 210°C / 1h) to cure to obtain benzoxazine resin (BOZ-La).

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Abstract

The invention provides a metal trifluoromethane sulfonate / benzoxazine resin composition and a preparation method thereof. The preparation method includes: weighing raw materials according to the proportion, dissolving the raw materials into a solvent, stirring until all the raw materials are dissolved, drying in a vacuum drying oven until constant weight is achieved, and grinding the mixture to achieve even mixing; transferring the evenly mixed sample to a die, placing the die into an air dry oven, and using a curing method adopting stepped temperature rising to obtain benzoxazine resin. The preparation method has the advantages that metal trifluoromethane sulfonate serving as the catalyst can effectively lower the curing temperature of the benzoxazine resin and increase the original heat resistance of the benzoxazine resin; the method is simple to operate and good in stability, and the prepared benzoxazine resin is high in carbon yield and suitable for being used to prepare high-performance and high-temperature-resistant flame-retardant materials.

Description

technical field [0001] The invention relates to a thermosetting resin and the technical field of curing thereof, in particular to a metal trifluoromethanesulfonate / benzoxazine resin composition and a preparation method thereof. Background technique [0002] The benzoxazine resin is prepared by reacting phenolic compounds, primary amine compounds and formaldehyde to form monomers, and then cross-linking and curing under the action of heating and / or catalysts. Compared with traditional thermosetting resins, benzoxazine resins have unique advantages: (1) little volume change during curing; (2) low water absorption; (3) high carbon residue rate; (4) curing process (5) No by-products are generated during the curing process; (6) The flexibility of molecular design is high. However, benzoxazine also has some defects: (1) high brittleness; (2) high curing temperature; (3) heat resistance needs to be further improved. At present, research at home and abroad is mainly focused on red...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G14/06C08L61/34
CPCC08G14/06C08L61/34C08L2201/08
Inventor 闫红强胡佳楠方征平程捷
Owner NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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