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Silicon-containing benzoxazine resin capable of being cured at low temperature and preparation method thereof

A technology of benzoxazine and resin, which is applied in the field of preparation of hybrid benzoxazine resin, can solve the problems of unfavorable molding processing and harsh production equipment, and achieve the effect of convenient adjustment

Active Publication Date: 2020-05-15
SHAANXI TIANCE NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the curing temperature of the silicon-containing benzoxazine resin prepared by the above method is >220°C, which is not conducive to molding and processing, and puts forward more stringent requirements for production equipment.

Method used

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  • Silicon-containing benzoxazine resin capable of being cured at low temperature and preparation method thereof
  • Silicon-containing benzoxazine resin capable of being cured at low temperature and preparation method thereof
  • Silicon-containing benzoxazine resin capable of being cured at low temperature and preparation method thereof

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preparation example Construction

[0025] The preparation method of the silicon-containing benzoxazine resin of the present invention is specifically realized according to the following method.

[0026]

[0027] Dissolve benzoxazine resin and nitrogen silane resin in a solvent according to a certain ratio, and then undergo a hydrosilylation reaction in the presence of a catalyst. After the reaction is completed, remove the solvent from the system at a low temperature under vacuum conditions. A silicon-containing benzoxazine resin is obtained.

[0028] Among them, at least one of R1 and R5 is an unsaturated functional group in the benzoxazine resin structure, and the unsaturated functional group can be a functional group containing unsaturated bonds such as allyl, propargyl or norbornene; R2 and R3 are independently is methyl, phenyl or amino; R4 is phenyl or silicon. R6 is the hydrogenated group of R1; R7 is the hydrogenated group of R5.

[0029] Specifically, the benzoxazine resin is prepared by reacting ...

Embodiment 1

[0037] Select the formula (3) bifunctional benzoxazine resin Bala prepared by bisphenol A, allylamine and paraformaldehyde as the benzoxazine resin containing unsaturated functional groups, trimethylchlorosilane, methyltrichlorosilane The nitrogen silane of the formula (4) prepared by ammonolysis with methylhydrogen dichlorosilane and ammonia is an organic silicon resin. Dissolve the two resins in petroleum ether according to a certain molar ratio, add chloroplatinic acid (the molar ratio of chloroplatinic acid to silicon-hydrogen bond is 2%) and react at 120°C for 2h, then spin evaporate at 80°C for 1h to remove the solvent , the silicon-containing benzoxazine resin BL can be obtained. According to the different molar ratios of silicon-hydrogen bonds and allyl groups, silicon-containing benzoxazine resins with different curing activities and different thermal stability can be obtained, as shown in Table 1.

[0038]

[0039]

[0040] Table 1 Example 1 DSC activity corres...

Embodiment 2

[0046] The formula (5) bifunctional benzoxazine resin BPala prepared by biphenol, allylamine and paraformaldehyde is selected as the benzoxazine resin containing unsaturated functional groups, methyltrichlorosilane and methylhydrogendi The nitrogen silane of the formula (6) prepared by chlorosilane and ammonia ammonolysis method is a silicone resin, dissolved in the solvent tetrahydrofuran, adding nickel acetylacetonate (the amount of nickel acetylacetonate is 2% mol of the silicon-hydrogen bond) and reacting at 60 ° C for 5 hours , and then at 60°C for 1 hour to remove the solvent, the silicon-containing benzoxazine resin BPL can be obtained. According to the different molar ratios of silicon-hydrogen bonds and allyl groups, silicon-containing benzoxazines with different curing activities and different thermal stability can be obtained. Oxazine resins, see Table 2.

[0047]

[0048]

[0049] Table 2 Example 2 The DSC activity corresponding to the hybrid resin and the ca...

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Abstract

The invention provides silicon-containing benzoxazine resin capable of being cured at a low temperature and a preparation method thereof. The silicon-containing benzoxazine resin prepared by the method has a primary amine group with higher activity, and can catalyze the curing of the benzoxazine resin, so that the benzoxazine resin has low curing temperature, the curing activity of the benzoxazineresin is tested by DSC, and the result shows that the method can obviously reduce the curing temperature of benzoxazine.

Description

technical field [0001] The invention belongs to the field of resin preparation, and in particular relates to a preparation method of a hybrid benzoxazine resin containing silicon element and capable of curing at low temperature. Background technique [0002] Benzoxazine resin is a new type of phenolic resin, and no small molecules are released during the curing process of the resin. Compared with traditional phenolic, epoxy and other resins, this resin has no volume shrinkage during curing. Moreover, by adjusting the molecular structure, a series of benzoxazine resins with different properties can be obtained. flammability. Conventional halogen flame retardants and phosphorus-based flame retardants are harmful to the environment and the human body. Therefore, new silicon-based flame retardants have been developed in recent years. CN 102134254B discloses a method for synthesizing silicon-containing benzoxazine resins using silane coupling agents containing primary amines. ...

Claims

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Application Information

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IPC IPC(8): C08G77/388C08G14/06
CPCC08G77/388C08G14/06
Inventor 杨泽诚艾涛张鸿翔江汛刘建国华栋
Owner SHAANXI TIANCE NEW MATERIAL TECH
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