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Preparation method for maleimide-containing biphenol type benzoxazine

A technology of maleimide biphenol type and benzoxazine, which is applied in the field of preparation of benzoxazine intermediates and can solve the problem of maleimide biphenol type benzoxazine that has not yet been seen. Intermediates and their resin synthesis and curing properties

Inactive Publication Date: 2014-01-01
SICHUAN VOCATIONAL & TECHN COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In summary, scholars at home and abroad have done a lot of research on the preparation of benzoxazine intermediates and resins, but there is no research on maleimide biphenol type benzoxazine intermediates and resins. Any reports and patents on the study of synthesis and its curing properties

Method used

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  • Preparation method for maleimide-containing biphenol type benzoxazine
  • Preparation method for maleimide-containing biphenol type benzoxazine
  • Preparation method for maleimide-containing biphenol type benzoxazine

Examples

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Embodiment 1

[0028] In this embodiment, the preparation method of the benzoxazine intermediate containing maleimide biphenyl diphenol type structure, its process steps are as follows:

[0029] (1) Synthesis reaction 1

[0030] Add 14g of formaldehyde aqueous solution, 17g of APMI, 800mL of ethyl acetate, and 100mL of water into a 1000mL round-bottomed flask in sequence, and react at room temperature for about 10h, then pour the reaction solution into a beaker filled with 1000mL of water to precipitate, vacuum filter, Washed with tap water, put into an oven and dried at 60° C. for 4 hours to obtain TMIPT as light yellow solid powder with a yield of about 96%.

[0031] (2) Synthesis reaction 2

[0032] Add 3.0g of paraformaldehyde, 19.5g of TMIPT, 12.0g of biphenol, and 1000mL of 1,4-dioxane into a 1500mL round-bottomed flask in turn, raise the temperature to 110°C and reflux for 27h to obtain a khaki-yellow precipitate. The reaction solution, the obtained reaction solution is poured into ...

Embodiment 2

[0034] In this embodiment, the preparation method of the benzoxazine intermediate containing maleimide biphenyl diphenol type structure, its process steps are as follows:

[0035] (1) Synthesis reaction 1

[0036] Add 21g of formaldehyde aqueous solution, 25.5g of APMI, 1200mL of ethyl acetate, and 150mL of water into a 1500mL round-bottomed flask in sequence, and react at room temperature for about 13h, then pour the reaction solution into a beaker filled with 2000mL of water to precipitate, vacuum pump filtered, washed with tap water, and dried in an oven at 60° C. for 6 h to obtain TMIPT as a light yellow solid powder with a yield of about 92%.

[0037] (2) Synthesis reaction 2

[0038] Add 4.5g of paraformaldehyde, 29.5g of TMIPT, 18.0g of biphenol, and 1200mL of 1,4-dioxane into a 1500mL round-bottomed flask in turn, raise the temperature to 110°C and reflux for 30h to obtain a khaki-yellow precipitate. The reaction solution, the resulting reaction solution was poured i...

Embodiment 3

[0040] In this embodiment, the preparation method of the benzoxazine intermediate containing maleimide biphenyl diphenol type structure, its process steps are as follows:

[0041] (1) Synthesis reaction 1

[0042] Add 22.4g of formaldehyde aqueous solution, 27.2g of APMI, 1280mL of ethyl acetate, and 160mL of water into a 1500mL round-bottomed flask in sequence, and react at room temperature for about 14 hours, then pour the reaction solution into a beaker filled with 1500mL of water to precipitate, vacuum Suction filtration, washing with tap water, drying in an oven at 60° C. for 4 hours to obtain TMIPT as light yellow solid powder with a yield of about 94%.

[0043] (2) Synthesis reaction 2

[0044] Add 4.8g of paraformaldehyde, 31.2g of TMIPT, 19.2g of biphenol, and 1300mL of 1,4-dioxane into a 1500mL round-bottomed flask in turn, raise the temperature to 110°C and reflux for 32h to obtain a khaki-yellow precipitate. The reaction solution, the resulting reaction solution ...

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Abstract

A preparation method for a benzoxazine intermediate adopting a maleimide-containing biphenol type structure comprises the following steps: (1) synthetic reaction 1: firstly, adding an aldehyde compound and a solvent into a reaction vessel at the indoor temperature and under normal pressure to be uniformly mixed, then adding an amine compound into the vessel while stirring, reacting for at least 10 hours under the normal pressure and at the temperature of 0-100 DEG C, after the reaction is completed, pouring the reaction liquid into a washing liquid to be washed, filtering and collecting a solid substance, and drying the solid substance at the temperature of 30-100 DEG C, so as to obtain an intermediate containing a triazine structure; (2) synthetic reaction 2: sequentially adding the obtained solid substance (triazine) as well as the aldehyde compound, biphenol, and 1, 4-dioxane intt the reaction vessel to be uniformly mixed, heating up to the temperature of 110 DEG C and carrying out a backflow reaction for 30 hours to obtain a reaction liquid containing earthy yellow precipitation, pouring the reaction liquid into deionized water, fully stirring, precipitating, leaching, washing for multiple times by using the deionized water and ethyl alcohol, and then drying in a dryer, so as to obtain the earthy yellow powder solid target product.

Description

Technical field: [0001] The invention belongs to the field of preparation of intermediates of benzoxazine monomers, in particular to a preparation method of intermediates of benzoxazines containing maleimide biphenyl diphenol structure. Background technique: [0002] Benzoxazine is a new type of phenolic resin modified product. It is a class of intermediates containing heterocyclic structures synthesized from phenolic compounds, amine compounds and aldehyde compounds. Under the action of heating and catalysts, ring-opening polymerization occurs to form a nitrogen-containing network similar to phenolic resins. That is, benzoxazine resin. The structural formula of the benzoxazine monomer is as follows: [0003] [0004] The advantage of benzoxazine resin is that it not only has the heat resistance and flame retardancy of ordinary thermosetting phenolic resin or thermoplastic phenolic resin, but also has no small molecules released during the molding and curing process of ...

Claims

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Application Information

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IPC IPC(8): C07D413/14
CPCC07D413/14
Inventor 陶果何展云曾琪张凯徐友辉陈自然
Owner SICHUAN VOCATIONAL & TECHN COLLEGE
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