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Benzoxazine intermediate, and preparation method and application thereof

A technology of benzoxazine and intermediates, which is applied in the field of resin preparation, can solve the problems of short storage time, difficulty in realizing industrial production, and limited application, and achieve the goals of shortening gelation time, realizing industrial production, and extending storage time Effect

Active Publication Date: 2017-02-15
同宇新材料(广东)股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, in the preparation of benzoxazine intermediates, dihydric phenolic benzoxazines and diamine benzoxazines are mainly used. The benzoxazine intermediates prepared by such synthetic methods have unidentified structures in their structures. The ring-closed phenolic hydroxyl and amine groups have technical defects such as short storage time and insufficient Tg (glass transition temperature) during use, which affect their further applications
From the above technical background, it can be concluded that the benzoxazine intermediates in the prior art have the technical defects of short storage time and insufficient Tg, making it difficult to realize industrial production and limited application
[0004] Therefore, a benzoxazine intermediate and its preparation method and application have been developed, which are used to solve the technical defects of short storage time and insufficient Tg in the prior art, and realize its industrial production. Enlarging the scope of application has become a problem to be solved urgently by those skilled in the art

Method used

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  • Benzoxazine intermediate, and preparation method and application thereof
  • Benzoxazine intermediate, and preparation method and application thereof
  • Benzoxazine intermediate, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] This example is a specific example of preparing Product 1, and the structural formula of Product 1 is shown below.

[0028]

[0029] Under room temperature conditions, weigh and / or measure bisphenol F (1mol), 4,4'-diaminodiphenyl ether (0.2mol) aniline (1.6mol) and 333.3g of formaldehyde aqueous solution with a mass concentration of 36%, add Catalyst NaOH 0.025mol, dissolved in a mixed solution of toluene (1000ml) and ethanol (20ml).

[0030] In this embodiment, the catalyst is 10% NaOH aqueous solution, and the catalyst accounts for 0.5% of the total mass of the reaction system; in the phenolic chemicals, amine compounds and aldehyde compounds, the molar ratio of the functional group phenolic hydroxyl group, amine group and aldehyde group is 1:1:2.

[0031] After the reaction system was stirred, it was heated under reflux at 60-120° C. for 4 hours. After heating under reflux, after vacuum distillation, cooling, washing, purification and drying, the product 1 was o...

Embodiment 2

[0034] This example is a specific example for preparing product 2, and the structural formula of product 2 is shown below.

[0035]

[0036] At room temperature, weigh and / or weigh 2 mol of bisphenol A, 0.2 mol of 4,4'-diaminodiphenylmethane, 4 mol of aniline and 9.6 mol of paraformaldehyde, add 0.2 mol of catalyst, dissolve in 1000 ml of toluene and 10 ml of ethanol in the mixed solution.

[0037] In this embodiment, the catalyst is 25% ammonia solution, and the catalyst accounts for 1% of the total mass of the reaction system; in the phenolic chemicals, amine compounds and aldehyde compounds, the molar ratio of the functional group phenolic hydroxyl group, amine group and aldehyde group is 1:1.05:2.4.

[0038] After the reaction system was stirred, it was heated under reflux at 60-120° C. for 4 hours. After heating under reflux, product 2 was obtained after vacuum distillation, cooling, washing, purification and drying. Butanone was added for dilution to obtain a 70% r...

Embodiment 3

[0041] Examples are specific examples for preparing product 3, and the structural formula of product 3 is shown below.

[0042]

[0043] At room temperature, weigh and / or weigh 0.1 mol of bisphenol A, 0.09 mol of methylamine, 0.05 mol of 4,4'-diaminodiphenylmethane and 0.4 mol of paraformaldehyde, add 0.02 mol of catalyst, dissolve in toluene 100ml and 5ml of ethanol in a mixed solution.

[0044] In this embodiment, the catalyst is 25% ammonia solution, and the catalyst accounts for 1% of the total mass of the reaction system; in phenolic chemicals, amine compounds and aldehyde compounds, the molar ratio of the functional group phenolic hydroxyl group, amine group and aldehyde group It is 1.1:1:2.

[0045] After the reaction system was stirred, it was heated under reflux at 60-120° C. for 4 hours. After heating under reflux, product 3 was obtained after vacuum distillation, cooling, washing, purification and drying. Butanone was added for dilution to obtain a 70% resin s...

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PUM

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Abstract

The invention belongs to the field of resin preparation, and especially relates to a benzoxazine intermediate, and a preparation method and an application thereof. The invention provides a benzoxazine intermediate, a preparation method of the benzoxazine intermediate, and an application of the benzoxazine intermediate or a product prepared by the abovementioned preparation method in the preparation of high Tg and / or highly heatproof resin. The provided benzoxazine intermediate has a more stable chemical structure and can be stored for a longer time. The experiment results show that compared with the conventional products, the provided benzoxazine intermediate has a higher crosslinking density after being cured, and thus has higher Tg and longer storage time. The technical shortages of short storage time and insufficient Tg in the prior art are overcome, the industrial production can be realized, and the application range is enlarged.

Description

technical field [0001] The invention belongs to the field of resin preparation, in particular to a benzoxazine intermediate and its preparation method and application. Background technique [0002] Traditional copper-clad laminates for printed circuits mainly use brominated epoxy resin to achieve the flame-retardant function of the board. However, in recent years, carcinogens such as dioxin and dibenzofuran have been detected in the combustion products of electronic and electrical equipment wastes containing halogens such as bromine and chlorine, and highly toxic substances may be released during the combustion process of halogen-containing products hydrogen halide. On July 1, 2006, the EU's two environmental protection directives "Regarding Waste Electrical and Electronic Equipment" and "Restricting the Use of Certain Hazardous Substances in Electrical and Electronic Equipment" came into effect. The implementation of these two directives has made the development of haloge...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/06C07D265/16
Inventor 苏世国李圣京张驰章星
Owner 同宇新材料(广东)股份有限公司
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